CN106935889B - A kind of intermediate temperature solid oxide fuel cell electrolyte of oxygen ion conduction - Google Patents
A kind of intermediate temperature solid oxide fuel cell electrolyte of oxygen ion conduction Download PDFInfo
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- CN106935889B CN106935889B CN201710308716.1A CN201710308716A CN106935889B CN 106935889 B CN106935889 B CN 106935889B CN 201710308716 A CN201710308716 A CN 201710308716A CN 106935889 B CN106935889 B CN 106935889B
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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
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
- H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
- H01M8/126—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides the electrolyte containing cerium oxide
-
- 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
- H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
- H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
- H01M8/1266—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides the electrolyte containing bismuth oxide
-
- 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
-
- 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
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
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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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to the preparation fields of solid electrolyte, and in particular to a kind of intermediate temperature solid oxide fuel cell electrolyte of oxygen ion conduction.The present invention prepares a kind of intermediate temperature solid oxide fuel cell electrolyte, electrolyte Ce using nitrate micro-gel flooding0.87La0.11Ni0.02O2‑α‑Bi1.55La0.45O3Composite electrolyte, wherein 0 α≤0.075 <.Its relative density reaches 98% or more；The electrolyte in air atmosphere 700 DEG C when ionic conductivity reach 1.88 × 10‑2S/cm。
Description
Technical field
The invention belongs to the preparation fields of solid electrolyte, and in particular to a kind of middle temperature solid-oxide of oxygen ion conduction
Fuel-cell electrolyte.
Background technique
With the development of global industry and increasing rapidly for population, tellurian resource will be increasingly shorter.And it is traditional
Generation mode is to pass through burning conversion by the chemical energy in the fossil energies such as petroleum, natural gas to push away for thermal energy, then by thermal energy mostly
Dynamic mechanical equipment generates mechanical energy, is ultimately converted to electric energy.This energy conversion is not only limited by Carnot cycle, can also be produced
Harmful substances and the noises such as raw a large amount of dust, carbon dioxide, nitrogen oxides and sulfide.Therefore seek a kind of energy conversion efficiency
High and environmental-friendly new energy technology is the key that presently relevant energy sector makes great efforts to develop.Solid oxide fuel cell
It (SOFC) is a kind of device directly by the chemical energy Efficient Conversion being stored in fuel and oxidant for electric energy, due to not firing
Burning and mechanical process, greatly improve energy conversion efficiency, avoid or reduce the generation of pollutant, and its byproduct is
The heat and vapor of high-quality, can be used to heat-electricity supply, be a kind of important energy source devices.
The operating temperature of traditional SOFC is worked at such high temperatures generally all at 1000 DEG C so that SOFC presence is permitted
More problems: electrode densifies, metallic interconnection materials require high and battery hermetization bad etc., considerably increases SOFC's with this
Cost limits its business development.In order to which its operating temperature must be just reduced to middle low temperature by SOFC commercialized development, and it is electrolysed
Matter can be obtained as the part of core the most in SOFC if electrolyte can have high conductivity under medium and low temperature
The ideal SOFC of medium temperature is obtained, so Novel electrolytic material must be developed.Electrolyte of the invention is in medium temperature operating condition
High conductivity can be obtained, down to meet the electrolyte that can be used in intermediate temperature SOFC required at present.
Summary of the invention
It is novel using nitrate micro-gel flooding in order to improve the performance of intermediate temperature solid oxide fuel cell electrolyte
Ce0.87La0.11Ni0.02O2-α(CLNO)-Bi1.55La0.45O3(LSB) composite electrolyte, relative density reach 98% or more；?
Conductivity is 1.88 × 10 when air atmosphere is 700 DEG C lower-2S/cm。
Preparation method:
1.Ce0.87La0.11Ni0.02O2-α(0 < α≤0.075) (CLNO) the preparation method comprises the following steps:
1) according to stoichiometric ratio precise raw material Ce (NO3)3·6H2O、La(NO3)3·nH2O、Ni(NO3)3·
6H2O, complexing agent citric acid are weighed by [n (CA): n (metal cation)=1.5:1]；
2) Ce (NO3)3·6H2O、La(NO3)3·nH2O、Ni(NO3)3·6H2O and citric acid use deionized water molten respectively
Solution, it is uniform to mix the above solution & stir；
3) it is 7 that ammonium hydroxide (ammonia concn 15wt%-20wt%), which is added dropwise, and adjusts pH value.
4) it step 3) is obtained mixed solution is put into blender to be heated to 45 DEG C, be continuously stirred at 45 DEG C, and stirring
By adding ammonium hydroxide during mixing, the pH value of solution is set to be maintained at 7, until forming gel；
5) gel immigration evaporating dish is placed on electric furnace and is heated, until self-propagating combustion, which occurs, forms fluffy oxide
Powder；
6) organic matter is removed within 30 ± 5 minutes in 600 DEG C of ± 10 DEG C of calcinings, then calcine 3 ± 0.1 hours at 800 DEG C ± 10 DEG C,
Form Ce0.87La0.11Ni0.02O2-αPowder.
2.Bi1.55La0.45O3(LSB) the preparation method comprises the following steps:
1) according to stoichiometric ratio precise raw material Bi2O3,La2O3。
2) by Bi2O3And La2O3Mixing and ball milling is for 24 hours；
3) mixture after ball milling is calcined 24 ± 0.1 hours at 800 DEG C ± 10 DEG C, obtains final product.
3. weighing two kinds of powder by CLNO:LSB mass ratio 95:5, ball milling 3h allows it uniformly to mix, prepares 95%
LCNO-5%LSB powder.
4. manufactured CLNO-LSB powder is put into mold, under the pressure of 300MPa, disk is made, by circle with every
The heating speed of 3 DEG C of minute is heated to 1200 DEG C ± 10 DEG C and keeps the temperature 4 ± 0.1 hours, electrolyte disk required for obtaining.
Remarkable advantage of the invention is:
(1) by CeO2Codope, increase oxygen vacancy concentration, and oxonium ion is exactly based on Lacking oxygen and expands in lattice
It dissipates, to improve conductivity.
(2) cell electrolyte produced by the present invention is with higher in medium temperature (600 DEG C -800 DEG C) range using temperature
Conductivity, higher power density.
(3) Bi in electrolyte1.55La0.45O3Have the function of reducing sintering temperature, so that sintering temperature is low, it is more energy saving.
(4) electrolyte produced by the present invention is suitable for intermediate temperature solid oxide fuel cell.
Detailed description of the invention
The relationship of ionic conductivity and test temperature of Fig. 1 electrolyte CLNO-LSB after 1200 DEG C are sintered 4h.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
Ce0.87La0.11Ni0.02O2-α(CLNO) preparation method
1.Ce0.87La0.11Ni0.02O1.9Preparation method
1) according to stoichiometric ratio precise raw material Ce (NO3)3·6H2O, La (NO3)3·nH2O, Ni (NO3)3·
6H2O, complexing agent citric acid are weighed according to [n (CA): n (metal cation)=1.5:1].
2) Ce (NO3)3·6H2O,La(NO3)3·nH2O, Ni (NO3)3·6H2O and citric acid use deionized water molten respectively
Solution；
3) it is uniform to mix the above solution & stir
4) it step 3) is obtained mixed solution is put into blender to be heated to 45 DEG C, be continuously stirred at 45 DEG C, and stirring
By adding ammonium hydroxide during mixing, the pH value of solution is set to be maintained at 7, until forming gel；
5) gel immigration evaporating dish is placed on electric furnace and is heated, until self-propagating combustion, which occurs, forms fluffy oxidate powder
End；
6) organic matter is removed within 30 ± 5 minutes in 600 DEG C of ± 10 DEG C of calcinings, then calcine 3 ± 0.1 hours at 800 DEG C ± 10 DEG C,
Form Ce0.87La0.11Ni0.02O2-αPowder.
2.Bi1.55La0.45O3(LSB) the preparation method comprises the following steps:
1) according to stoichiometric ratio precise raw material Bi2O3And La2O3。
2) by Bi2O3And La2O3Mixing and ball milling is for 24 hours；
3) mixture after ball milling is calcined 24 ± 0.1 hours at 800 DEG C ± 10 DEG C, obtains final product.
3. weighing two kinds of powder by CLNO:LSB mass ratio 95:5, ball milling 3h allows it uniformly to mix, prepares 95%LCNO-
5%LSB powder.
It is specific:
The preparation of 100 grams of CLNO-LSB:
1) 1 mole of Ce is prepared0.87La0.11Ni0.02O1.9
Weigh 0.87 mole of Ce (NO3)3·6H2O:0.87*434.22=377.77 gram
Weigh 0.11 mole of La (NO3)3·nH2O:0.11*324.92=35.74 gram
Weigh 0.02 mole of Ni (NO3)3·6H2O:0.02*290.79=5.82 gram
Weigh 1.5 moles of citric acid: 1.5*210.14=315.21 gram
By Ce (NO3)3·6H2O,La(NO3)3·nH2O,Ni(NO3)3·6H2O and citric acid use deionized water molten respectively
Solution；It is uniform to mix the above solution & stir；It is put into water-bath and is heated to 45 DEG C, continuously stirred at 45 DEG C, and stirred
By adding ammonium hydroxide in journey, the pH value of solution is set to be maintained at 7, until forming gel；Gel immigration evaporating dish is placed on electric furnace and is added
Heat, until self-propagating combustion, which occurs, forms fluffy oxide powder.
Powder is removed into organic matter in 600 DEG C of calcining 30min, is then calcined 3 hours at 800 DEG C, forms CLNO powder.
2) 1 mole of Bi is prepared1.55La0.45O3
Weigh 1.55 moles of Bi2O3: 1.55*465.96=722.24 gram
Weigh 0.45 mole of La2O3: 0.45*325.81=146.61 gram
The Bi that will be weighed up2O3And La2O3Add alcohol mixing and ball milling for 24 hours, it is 12 hours dry, it calcines for 24 hours, obtains at 800 DEG C
Final product Bi1.55La0.45O3；
3) 100 grams of 95wt%Ce0.87La0.11Ni0.02O1.9-5wt%Bi1.55La0.45O3Preparation
Weigh 95 grams of Ce0.8Gd0.2O1.9
Weigh 5 grams of Bi1.55La0.45O3
By above-mentioned latter two powder mixing and ball milling 3h, keeps its grinding sufficiently and uniform, obtain 95%CLNO-5%LSB powder
End.
Embodiment 2
The preparation of disk: the CLNO-LSB powder that embodiment 1 is prepared into is put into mold, under the pressure of 300MPa,
The disk that diameter is 13mm ± 0.1mm, thickness 0.5mm ± 0.1mm is made, disk is heated with 3 DEG C of heating speed per minute
4 ± 0.1 hours are kept the temperature to 1200 DEG C ± 10 DEG C, electrolyte disk required for obtaining.
The test method of conductivity:
The conductance for alternating current of electrolyte is measured using two-terminal method.By the institute after being sintered 4 ± 0.1 hours at 1200 DEG C ± 10 DEG C
Silver paste is coated on the CLNO-LSB electrolyte disk two sides obtained, and silver electrode is then made after 450 DEG C of roasting 2h.With filamentary silver by both ends
Silver electrode connect with alternating current impedance instrument.The alternating current impedance instrument used is Shanghai Chen Hua Instrument Ltd. model CHI660E
Electrochemical workstation measures frequency range 1kHz-20MHz using current potential 10mV, and the temperature for measuring conductance for alternating current is 700 DEG C,
It measures in air atmosphere, is measured in air atmosphere.Conductivity is calculated using following formula:
In formula, σ is electrolytic conductivity, S/cm；
H is electrolyte sheet thickness, unit cm；
R is bath resistance, unit Ω；
S is electrolyte sheet cross-sectional area, unit cm2。
Claims (2)
1. a kind of intermediate temperature solid oxide fuel cell electrolyte preparation method of oxygen ion conduction, it is characterised in that: described
Electrolyte is Ce0.87La0.11Ni0.02O2-α-Bi1.55La0.45O3Composite electrolyte, wherein 0 α≤0.075 <；The battery electrolysis
The specific preparation step of matter are as follows:
One, Ce0.87La0.11Ni0.02O2-αThe preparation method comprises the following steps:
1) according to stoichiometric ratio precise raw material Ce (NO3)3·6H2O、La(NO3)3·nH2O、Ni(NO3)3·6H2O, and
It is that 1:1.5 weighs citric acid by the molar ratio of metal cation and citric acid；
2) Ce (NO3)3·6H2O、La(NO3)3·nH2O、Ni(NO3)3·6H2O and citric acid use deionized water dissolving respectively, mix
It is uniform to close the above solution & stir；
3) it is 7 that ammonium hydroxide is added dropwise into step (2) mixed liquor and adjusts pH value；
4) mixed solution for obtaining step 3), which is put into blender, is heated to 45 DEG C, continuously stirs at 45 DEG C, and stirring
In the process by adding ammonium hydroxide, the pH value of solution is set to be maintained at 7, until forming gel；
5) gel immigration evaporating dish is placed on electric furnace and is heated, until self-propagating combustion, which occurs, forms fluffy oxide powder；
6) powder obtained by step (5) is removed into organic matter in 30 ± 5 minutes in 600 DEG C of ± 10 DEG C of calcinings, is then forged at 800 DEG C ± 10 DEG C
It burns 3 ± 0.1 hours, forms Ce0.87La0.11Ni0.02O2-αPowder；
Two, Bi1.55La0.45O3The preparation method comprises the following steps:
1) according to stoichiometric ratio precise raw material Bi2O3And La2O3；
2) by Bi2O3And La2O3Mixing and ball milling is for 24 hours；
3) mixture after ball milling is calcined 24 ± 0.1 hours at 800 DEG C ± 10 DEG C, obtains final product；
Three, Ce is pressed0.87La0.11Ni0.02O2-αAnd Bi1.55La0.45O395:5 in mass ratio weighs two kinds of powder, and ball milling 3h makes it equal
Even mixing prepares Ce0.87La0.11Ni0.02O2-α-Bi1.55La0.45O3Powder；
Four, by manufactured Ce0.87La0.11Ni0.02O2-α-Bi1.55La0.45O3Powder is put into mold, under the pressure of 300MPa,
Disk is made, disk is heated to 1200 DEG C ± 10 DEG C with 3 DEG C of heating speed per minute and keeps the temperature 4 ± 0.1 hours, needed for obtaining
The electrolyte disk wanted.
2. the intermediate temperature solid oxide fuel cell electrolyte preparation method of oxygen ion conduction according to claim 1,
It is characterized by: the ammonia concn is 15wt%-20wt%.
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| CN108682884B (en) * | 2018-04-27 | 2021-05-25 | 山东理工大学 | Oxygen ion type composite electrolyte of intermediate-temperature solid oxide fuel cell and preparation method thereof |
| CN114709457B (en) * | 2022-03-10 | 2023-08-18 | 福州大学 | Double-doped medium-temperature solid oxide fuel cell electrolyte and preparation method thereof |
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| CN101662033A (en) * | 2008-08-25 | 2010-03-03 | 中国科学院物理研究所 | Solid oxide fuel cell and preparation method thereof |
| CN105633439A (en) * | 2016-01-08 | 2016-06-01 | 福州大学 | Electrolyte for intermediate-temperature solid oxide fuel cell and preparation method of electrolyte |
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| RU2236069C1 (en) * | 2003-06-10 | 2004-09-10 | Мятиев Ата Атаевич | Bismuth oxide based electrode-electrolyte couple, its production method, and organogel |
| JP4748465B2 (en) * | 2009-05-28 | 2011-08-17 | Ｔｏｔｏ株式会社 | Fuel cell device |
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| CN101662033A (en) * | 2008-08-25 | 2010-03-03 | 中国科学院物理研究所 | Solid oxide fuel cell and preparation method thereof |
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| CN105633439A (en) * | 2016-01-08 | 2016-06-01 | 福州大学 | Electrolyte for intermediate-temperature solid oxide fuel cell and preparation method of electrolyte |
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