CN104852070B - A kind of solid-oxide fuel battery electrolyte and its preparation method and application - Google Patents
A kind of solid-oxide fuel battery electrolyte and its preparation method and application Download PDFInfo
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- CN104852070B CN104852070B CN201510295050.1A CN201510295050A CN104852070B CN 104852070 B CN104852070 B CN 104852070B CN 201510295050 A CN201510295050 A CN 201510295050A CN 104852070 B CN104852070 B CN 104852070B
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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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- 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
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- 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
The invention discloses a kind of solid-oxide fuel battery electrolyte and its preparation method and application, Ce is first prepared using nitrate micro-gel flooding0.8Gd0.2O1.9, then 50%Ce is prepared using solid phase paddling process0.8Gd0.2O1.9‑10.4%Li2CO3‑10.4%Na2CO316.7%CdO 12.5%MgO electrolyte, its relative density reaches 100%, in air atmosphere 500 DEG C when ionic conductivity be 0.0175S/cm, ionic conductivity reaches 0.0243S/cm at 600 DEG C, for in intermediate temperature solid oxide fuel cell, output power density increases, and SOFC is had more preferable chemical property.
Description
Technical field
The invention belongs to solid-oxide fuel battery electrolyte preparation field, and in particular to a kind of solid oxide fuel
Cell electrolyte and its preparation method and application.
Background technology
The whole world expands day by day to the demand of the energy, and gradually payes attention to the problem of environmental degradation, and traditional energy system is by nothing
Method adapts to society to efficient, cleaning, the requirement of safe, economic energy system, and the development of the energy will face huge challenge, because
This fuel cell will turn into 21st century important energy source device.SOFC（SOFC）It is anti-by electrochemistry
Answering process makes the chemical energy in fossil class A fuel A be converted into electric energy, due to without burning and mechanical process, being greatly enhanced
Energy conversion efficiency, it is to avoid or reduce the generation of the pollutants such as NOx, SOx, CO, CO2 and dust；The work temperature of SOFC
At 500 DEG C ~ 1000 DEG C, its byproduct is the heat and vapor of high-quality to degree, in the case of heat-CCHP, capacity usage ratio
Up to 80% or so, it is a kind of energy resource system of clean and effective.
The operating temperature of traditional SOFC is high（900~1000℃）, hot operation accelerates reacting to each other between part and expands
Dissipate, the increase of cell performance decay speed, so performance necessarily to materials such as electrode material and connectors proposes requirement higher,
So as to increase battery system expense, the commercialized development of SOFC is greatly limit.Therefore, for SOFC commercialized developments it is necessary to
SOFC operating temperatures are reduced, low temperature SOFC has turned into inexorable trend in exploitation.In SOFC systems, electrolyte is the core of battery
The heart, the performance of electrolyte directly decides the operating temperature and performance of SOFC batteries.During traditional electrolyte cannot be applied to
Cryogenic conditions, therefore must just seek the electrolyte with high conductivity under middle low temperature.
The content of the invention
It is an object of the invention to provide a kind of solid-oxide fuel battery electrolyte and its preparation method and application, system
The relative density of electrolyte reach 100%, in air atmosphere 500 DEG C when ionic conductivity be 0.0175S/cm, 600
DEG C when ionic conductivity reach 0.0243S/cm, in intermediate temperature solid oxide fuel cell, output power density increase,
Make SOFC that there is more preferable chemical property.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of component of solid-oxide fuel battery electrolyte presses mole percent：50%Ce0.8Gd0.2O1.9-10.4%
Li2CO3-10.4%Na2CO3-16.7%CdO-12.5%MgO。
Preparation method：Ce is first prepared using nitrate micro-gel flooding0.8Gd0.2O1.9, then prepared using solid phase paddling process
50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3-16.7%CdO-12.5%MgO。
Comprise the following steps that：
1）Ce0.8Gd0.2O1.9Preparation
A) Ce is pressed0.8Gd0.2O1.9Stoichiometric proportion weighs Ce (NO3)3·6H2O and Gd2O3, and by metal cation and lemon
The mol ratio of acid ion is 1.5:1 weighs citric acid；
B) with the dilute nitric acid dissolution Gd that concentration is 10-15wt.%2O3；
C) by Ce (NO3)3·6H2O and citric acid dissolve in distilled water respectively；
D) two kinds of solution of step c) are poured into the gadolinium nitrate solution of step b) respectively, is added dropwise over ammoniacal liquor, adjust pH
Be worth is 7；
E) mixed solution for obtaining step d) is heated to 45 DEG C while stirring, and constant temperature is continuously stirred, and in whipping process
In by the way that ammoniacal liquor is added dropwise, the pH value of solution is maintained at 7, until formed gel；
F) gel is heated, until self-propagating combustion occurs forms fluffy oxide powder；
G) powder is heated to 790-810 DEG C, is incubated 2.9-3.1 hours, natural cooling is obtained Ce0.8Gd0.2O1.9Powder；
2）The preparation of electrolyte
A) according to 50%Ce0.82Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3Moles the hundred of -16.7%CdO-12.5%MgO
Point content weighs Ce respectively0.82Gd0.2O1.9Powder, Li2CO3、Na2CO3、Cd(NO3)2·4H2O and Mg (NO3)2·6H2O, will
Li2CO3、Na2CO3、Cd(NO3)2·4H2O and Mg (NO3)2·6H2O grinds 3h using solid phase paddling process, adds
Ce0.82Gd0.2O1.9Powder, continues to stir mixing 2h, by 790-810 DEG C of sintering 4h of mixed-powder, obtains 50%Ce0.82Gd0.2O1.9-
10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO powder；
B) by 50%Ce0.82Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO powder exists
Disc-shaped is made under the pressure of 300MPa, then 690-710 DEG C is heated to 3 DEG C per minute of firing rate, 1.4-1.6 is small for insulation
When, obtain 50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO electrolyte disks.
Step d) and e) in ammoniacal liquor concentration be 15-20wt.%.
Obtained 50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO electrolyte should
For 500-800 DEG C of intermediate temperature solid oxide fuel cell.
Remarkable advantage of the invention is：The relative density of obtained electrolyte reaches 100%, and in air atmosphere 500
DEG C when ionic conductivity be 0.0175S/cm, ionic conductivity reaches 0.0243S/cm at 600 DEG C, for middle low-temperature solid oxidation
In thing fuel cell, output power density increase makes SOFC have more preferable chemical property.
Specific embodiment
A kind of component of solid-oxide fuel battery electrolyte presses mole percent：50%Ce0.8Gd0.2O1.9-10.4%
Li2CO3-10.4%Na2CO3-16.7%CdO-12.5%MgO。
Preparation method：Ce is first prepared using nitrate micro-gel flooding0.8Gd0.2O1.9, then prepared using solid phase paddling process
50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3-16.7%CdO-12.5%MgO。
Comprise the following steps that：
1）Ce0.8Gd0.2O1.9Preparation
A) Ce is pressed0.8Gd0.2O1.9Stoichiometric proportion weighs Ce (NO3)3·6H2O and Gd2O3, and by metal cation and lemon
The mol ratio of acid ion is 1.5:1 weighs citric acid；
B) with the dilute nitric acid dissolution Gd that concentration is 10-15wt.%2O3；
C) by Ce (NO3)3·6H2O and citric acid dissolve in distilled water respectively；
D) two kinds of solution of step c) are poured into the gadolinium nitrate solution of step b) respectively, is added dropwise over ammoniacal liquor, adjust pH
Be worth is 7；
E) mixed solution for obtaining step d) is heated to 45 DEG C while stirring, and constant temperature is continuously stirred, and in whipping process
In by the way that ammoniacal liquor is added dropwise, the pH value of solution is maintained at 7, until formed gel；
F) gel is heated, until self-propagating combustion occurs forms fluffy oxide powder；
G) powder is heated to 790-810 DEG C, is incubated 2.9-3.1 hours, natural cooling is obtained Ce0.8Gd0.2O1.9Powder；
2）The preparation of electrolyte
A) according to 50%Ce0.82Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3Moles the hundred of -16.7%CdO-12.5%MgO
Point content weighs Ce respectively0.82Gd0.2O1.9Powder, Li2CO3、Na2CO3、Cd(NO3)2·4H2O and Mg (NO3)2·6H2O, will
Li2CO3、Na2CO3、Cd(NO3)2·4H2O and Mg (NO3)2·6H2O grinds 3h using solid phase paddling process, adds
Ce0.82Gd0.2O1.9Powder, continues to stir mixing 2h, by 790-810 DEG C of sintering 4h of mixed-powder, obtains 50%Ce0.82Gd0.2O1.9-
10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO powder；
B) by 50%Ce0.82Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO powder exists
Disc-shaped is made under the pressure of 300MPa, then 690-710 DEG C is heated to 3 DEG C per minute of firing rate, 1.4-1.6 is small for insulation
When, obtain 50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO electrolyte disks.
Step d) and e) in ammoniacal liquor concentration be 15-20wt.%.
Obtained 50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO electrolyte should
For 500-800 DEG C of intermediate temperature solid oxide fuel cell.
Embodiment 1
A kind of component of solid-oxide fuel battery electrolyte presses mole percent：50%Ce0.8Gd0.2O1.9-10.4%
Li2CO3-10.4%Na2CO3-16.7%CdO-12.5%MgO。
Preparation method：Ce is first prepared using nitrate micro-gel flooding0.8Gd0.2O1.9, then prepared using solid phase paddling process
50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3-16.7%CdO-12.5%MgO。
Comprise the following steps that：
1）Ce0.8Gd0.2O1.9Preparation
A) Ce is pressed0.8Gd0.2O1.9Stoichiometric proportion weighs Ce (NO3)3·6H2O and Gd2O3, and by metal cation and lemon
The mol ratio of acid ion is 1.5:1 weighs citric acid；
B) with the dilute nitric acid dissolution Gd that concentration is 10-15wt.%2O3；
C) by Ce (NO3)3·6H2O and citric acid dissolve in distilled water respectively；
D) two kinds of solution of step c) are poured into the gadolinium nitrate solution of step b) respectively, is added dropwise over ammoniacal liquor, adjust pH
Be worth is 7；
E) mixed solution for obtaining step d) is heated to 45 DEG C while stirring, and constant temperature is continuously stirred, and in whipping process
In by the way that ammoniacal liquor is added dropwise, the pH value of solution is maintained at 7, until formed gel；
F) gel is heated, until self-propagating combustion occurs forms fluffy oxide powder；
G) powder is heated to 800 DEG C, is incubated 3 hours, natural cooling is obtained Ce0.8Gd0.2O1.9Powder；
2）The preparation of electrolyte
A) according to 50%Ce0.82Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3Moles the hundred of -16.7%CdO-12.5%MgO
Point content weighs Ce respectively0.82Gd0.2O1.9Powder, Li2CO3、Na2CO3、Cd(NO3)2·4H2O and Mg (NO3)2·6H2O, will
Li2CO3、Na2CO3、Cd(NO3)2·4H2O and Mg (NO3)2·6H2O grinds 3h using solid phase paddling process, adds
Ce0.82Gd0.2O1.9Powder, continues to stir mixing 2h, by 800 DEG C of sintering 4h of mixed-powder, obtains 50%Ce0.82Gd0.2O1.9-
10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO powder；
B) by 50%Ce0.82Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO powder exists
Disc-shaped is made under the pressure of 300MPa, then 700 DEG C are heated to 3 DEG C per minute of firing rate, be incubated 1.5 hours, obtained
50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO electrolyte disks.
Step d) and e) in ammoniacal liquor concentration be 15-20wt.%.
The method of testing of electrical conductivity：
The conductance for alternating current of electrolyte is determined using two-terminal method.By obtained 50%Ce0.82Gd0.2O1.9-10.4%Li2CO3-
10.4%Na2CO3Silver paste is coated on -16.7%CdO-12.5%MgO electrolyte disks two sides, and silver is obtained after being then calcined 2h in 450 DEG C
Electrode.The silver electrode at two ends is connected with alternating current impedance instrument with filamentary silver.The alternating current impedance instrument for using is limited for Shanghai Chen Hua instrument
Company's model CHI660E electrochemical workstations, using current potential 10mV, determine frequency range 1kHZ-20MHZ, determine alternating current
The temperature led is 500-600 DEG C, is determined in air atmosphere.Electrical conductivity is calculated using equation below：
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。
Ionic conductivity is 0.0175S/cm at 500 DEG C, and ionic conductivity reaches 0.0243S/cm at 600 DEG C.
Obtained electrolyte disk is used in intermediate temperature solid oxide fuel cell, output power density increase, makes solid
Oxide body fuel cell has more preferable chemical property.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with
Modification, should all belong to covering scope of the invention.
Claims (3)
1. a kind of preparation method of solid-oxide fuel battery electrolyte, it is characterised in that：Component presses mole percent：
50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3-16.7%CdO-12.5%MgO；
The preparation method of described solid-oxide fuel battery electrolyte, comprises the following steps that：
1）Ce0.8Gd0.2O1.9Preparation
A) Ce is pressed0.8Gd0.2O1.9Stoichiometric proportion weighs Ce (NO3)3·6H2O and Gd2O3, and by metal cation and citrate
The mol ratio of ion is 1.5:1 weighs citric acid；
B) with the dilute nitric acid dissolution Gd that concentration is 10-15wt.%2O3；
C) by Ce (NO3)3·6H2O and citric acid dissolve in distilled water respectively；
D) two kinds of solution of step c) are poured into the gadolinium nitrate solution of step b) respectively, is added dropwise over ammoniacal liquor, regulation pH value is
7；
E) mixed solution for obtaining step d) is heated to 45 DEG C while stirring, and constant temperature is continuously stirred, and leads in whipping process
Dropwise addition ammoniacal liquor is crossed, the pH value of solution is maintained at 7, until forming gel；
F) gel is heated, until self-propagating combustion occurs forms fluffy oxide powder；
G) powder is heated to 790-810 DEG C, is incubated 2.9-3.1 hours, natural cooling is obtained Ce0.8Gd0.2O1.9Powder；
2）The preparation of electrolyte
A) according to 50%Ce0.82Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3The Mole percent of -16.7%CdO-12.5%MgO contains
Amount weighs Ce respectively0.82Gd0.2O1.9Powder, Li2CO3、Na2CO3、Cd(NO3)2·4H2O and Mg (NO3)2·6H2O, by Li2CO3、
Na2CO3、Cd(NO3)2·4H2O and Mg (NO3)2·6H2O grinds 3h using solid phase paddling process, adds Ce0.82Gd0.2O1.9Powder
End, continues to stir mixing 2h, by 790-810 DEG C of sintering 4h of mixed-powder, obtains 50%Ce0.82Gd0.2O1.9-10.4%Li2CO3-
10.4%Na2CO3- 16.7%CdO-12.5%MgO powder；
B) by 50%Ce0.82Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO powder is 300Mpa's
Disc-shaped is made under pressure, then 690-710 DEG C is heated to 3 DEG C per minute of firing rate, be incubated 1.4-1.6 hours, obtained
50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO electrolyte disks.
2. method according to claim 1, it is characterised in that：Step d) and e) in ammoniacal liquor concentration be 15-20wt.%.
3. a kind of application of solid-oxide fuel battery electrolyte prepared by the method for claim 1, its feature exists
In：50%Ce0.8Gd0.2O1.9-10.4%Li2CO3-10.4%Na2CO3- 16.7%CdO-12.5%MgO electrolyte is applied to 500-800
DEG C intermediate temperature solid oxide fuel cell.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105655618B (en) * | 2016-01-08 | 2018-01-12 | 福州大学 | One kind melts mixed type intermediate temperature solid oxide fuel cell electrolyte admittedly |
| CN106328972A (en) * | 2016-08-29 | 2017-01-11 | 董晓 | Preparation method of mid-low temperature solid oxide fuel cell cathode material |
| CN106207238A (en) * | 2016-09-30 | 2016-12-07 | 福州大学 | A kind of molten salts compound intermediate temperature solid oxide fuel cell electrolyte |
| CN110444796B (en) * | 2019-09-10 | 2022-05-17 | 东北大学 | Method for improving electrolyte conductivity of solid oxide fuel cell |
| CN112759392B (en) * | 2020-12-25 | 2022-11-01 | 合肥学院 | Multi-component co-doped cerium oxide-based solid electrolyte material and preparation method thereof |
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| CN1269613A (en) * | 2000-02-16 | 2000-10-11 | 刘向荣 | Composite ceramic material for middle-temperature oxide fuel cell |
| CN1697223A (en) * | 2005-06-17 | 2005-11-16 | 清华大学 | Electrolyte composed of zinc doped cerium oxide and inorganic salt in use for fuel cell of solid oxide in low temperature |
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| CN1269613A (en) * | 2000-02-16 | 2000-10-11 | 刘向荣 | Composite ceramic material for middle-temperature oxide fuel cell |
| CN1697223A (en) * | 2005-06-17 | 2005-11-16 | 清华大学 | Electrolyte composed of zinc doped cerium oxide and inorganic salt in use for fuel cell of solid oxide in low temperature |
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