CN108232259A - A kind of preparation method of medium temperature solid fuel cell electrolyte - Google Patents
A kind of preparation method of medium temperature solid fuel cell electrolyte Download PDFInfo
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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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The present invention relates to a kind of preparation methods of medium temperature solid fuel cell electrolyte, belong to field of new energy technologies.The present invention has higher oxygen ionic conductivity at relatively low temperature using doped cerium oxide electrolyte, and it is being sintered with there is preferable chemical compatibility and mechanical matching with high performance cathodes material under operating temperature, and pass through doping cerium, the rare earth elements such as gadolinium form the electrolyte of battery, greatly improve its oxygen vacancy concentration, so as to improve its ionic conductivity, and relatively low synthesis temperature reduces the crystalline size of material, improve the sintering character and sintered density of material, so that the oxygen ion conduction of electrolyte is protected, pass through composite titanium dioxide and strontium oxide strontia again, reduce the average grain size of electrolyte, so that the particle homogenization of electrolyte, it can more be densified on the whole, improve ionic conductivity, and then improve the output power of the monocell of electrolyte-supported.
Description
Technical field
The present invention relates to a kind of preparation methods of medium temperature solid fuel cell electrolyte, belong to new energy technology neck
Domain.
Background technology
Solid fuel cell（SOFC）As a kind of pure, stable, efficient energy conversion device, become and effectively solve energy
One of important technical of source crisis and problem of environmental pollution.Electrolyte of the Solid oxygen ion conductor as SOFC,
The properties such as operating temperature, stability, energy conversion efficiency have an important influence on the application of SOFC.Solid electrolyte material
Basic demand is：Must have ionic conductivity height, electronic conductivity is low；Stability in fuel and oxidizing atmosphere is good；With
It is not chemically reacted between adjacent constituent element；It is fine and close and with adjacent constituent element matched coefficients of thermal expansion.At present, applied to SOFC's
Electrolyte is mainly fluorite structure, perovskite structure and novel apatite structure material.
The SOFC of early development usually works under 800~1000 DEG C of hot conditions, this can lead to the types of fuel cells
Problems are encountered in exploitation, manufacture and application.Such as the selection of material of high temperature limiting, reduce battery life：
The group element material of SOFC is used to prepare under the premise of the electric property that must have enough protrusions, it is necessary to have outstanding chemistry
The working environment of high temperature is adapted to thermal stability；High operating temperature often brings battery work some accidental to ask
Topic, the performance that but will clearly result in SOFC gradually decay, and reduce the service life of battery.These are greatly limited
The development of SOFC.When the operation temperature of SOFC is reduced in 500~800 DEG C of mesophilic range, battery can be not only significantly improved
Thermodynamic efficiency, the cost of manufacture of battery is greatly lowered, but also high-temperature stability, elevated-temperature seal difficulty etc. can be solved
Problem simplifies the material requirements of battery design, slows down reacting to each other between battery component, avoids the degeneration of battery material, extends
The service life of battery.
The research of intermediate temperature SOFC still in the starting stage, is concentrated mainly in the exploitation of critical material at present.Wherein, solid-state
Electrolyte is the most crucial constituent element of battery, performance, including ionic conductivity, structure, chemical stability, coefficient of thermal expansion, cause
Densification temperature etc. not only directly affects the operating temperature and energy conversion efficiency of battery, also limits matched electrode
The selection of material and corresponding technology of preparing.But the electrolyte sintering character and sintered density used at present is poor, conductive
Rate is low, therefore, is badly in need of researching and developing a kind of electrolyte haveing excellent performance.
Invention content
The technical problems to be solved by the invention：For the electrolyte sintering character and sintered density used at present
Difference, the problem of conductivity is low, provide a kind of preparation method of medium temperature solid fuel cell electrolyte.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Gadolinium oxide, samarium oxide is taken to add in mass fraction to be uniformly mixed in 20% salpeter solution, adds in cerium nitrate hexahydrate stirring
It is completely dissolved to solid, adds citric acid, ethylenediamine tetra-acetic acid, sodium hydroxide solution is added dropwise after being uniformly mixed is to pH
8~9,15~20h is stood, obtains reaction solution；
（2）Reaction solution is transferred in the water heating kettle with Teflon liner and carries out hydro-thermal reaction, diafiltration is crossed after being cooled to room temperature
Drying is washed, obtains presoma；
（3）Presoma is placed in Muffle furnace and is lighted, self-propagating combustion reaction occurs, again at 700~800 DEG C after burning
3~5h of lower heat preservation calcining obtains electrolyte just powder；
（4）Powder at the beginning of electrolyte is fitted into ball mill, titanium dioxide, strontium oxide strontia, absolute ethyl alcohol are added, with 300~500r/
Min 5~8h of ball milling, obtain mixed-powder；
（5）It is mixed-powder is tabletted and be sintered, obtain medium temperature solid fuel cell electrolyte.
Step（1）The gadolinium oxide, samarium oxide, cerium nitrate hexahydrate, citric acid, ethylenediamine tetra-acetic acid parts by weight be 1.8
~2.7 parts of gadolinium oxides, 1.7~2.6 parts of samarium oxides, 34.7~52.1 parts of cerium nitrate hexahydrates, 9.6~14.4 parts of citric acids, 2.9~
4.4 parts of ethylenediamine tetra-acetic acids.
Step（2）The hydrothermal reaction process is carries out hydro-thermal reaction, the hydro-thermal reaction time 10 at 120~180 DEG C
~12h.
Step（4）The amount of titanium is the 2.96~6.67% of gadolinium oxide quality.
Step（4）The strontium oxide strontia dosage is the 3.70~8.33% of gadolinium oxide quality.
Step（5）The tabletted process is is pressed into a diameter of 12~15mm, thickness under 220~250MPa pressure
Disk for 1~2mm.
Step（5）The sintering process is that 8~10h is sintered at 1300~1450 DEG C.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention has higher oxygen ionic conductivity at relatively low temperature using doped cerium oxide electrolyte, and
It is being sintered with there is preferable chemical compatibility and mechanical matching, and pass through with high performance cathodes material under operating temperature
The electrolyte that the rare earth elements such as cerium, gadolinium form battery is adulterated, its oxygen vacancy concentration is greatly improved, is led so as to improve its ion
Electrically, and relatively low synthesis temperature reduces the crystalline size of material, improves the sintering character and sintered density of material, makes
The oxygen ion conduction for obtaining electrolyte is protected；
（2）The present invention increases the relative density of electrolyte, and then increase ceramics by composite titanium dioxide and strontium oxide strontia
Crystal phase reduces the generation of gas phase, and then improves the Vickers hardness of electrolyte, and can to clean Si miscellaneous for composite titanium dioxide
Matter, combined oxidation strontium can promote to clean, and can reduce the average grain size of electrolyte so that the particle of electrolyte is uniform
Change, can more be densified on the whole, improve ionic conductivity, and then improve the output work of the monocell of electrolyte-supported
Rate.
Specific embodiment
1.8~2.7g gadolinium oxides are taken, 1.7~2.6g samarium oxides, it is 20% salpeter solution to add in 100~150g mass fractions
In, 34.7~52.1g cerium nitrate hexahydrates are added in after stirring 15~20min with 300~400r/min, it is complete to solid to continue stirring
Dissolving, adds 9.6~14.4g citric acids, mass fraction is added dropwise after being uniformly mixed in 2.9~4.4g ethylenediamine tetra-acetic acids
It is 8~9 for 5% sodium hydroxide solution to pH, stands 15~20h, obtain reaction solution, reaction solution is transferred to Teflon liner
Water heating kettle in, carry out hydro-thermal reaction at 120~180 DEG C, the hydro-thermal reaction time is 10~12h, is filtered after being cooled to room temperature
Filter residue, be washed with deionized again 2~3 times, then be placed in drying box after washing filter residue 2~3 times with absolute ethyl alcohol, 120
It is dried at~150 DEG C to constant weight, obtains presoma, presoma is placed in Muffle furnace and lights generation self-propagating combustion reaction, combustion
3~5h is calcined in heat preservation at 700~800 DEG C again after burning, obtains electrolyte just powder, powder at the beginning of electrolyte is fitted into ball mill,
Add 0.08~0.12g titanium dioxide, 0.10~0.15g strontium oxide strontias, 20~30mL absolute ethyl alcohols, with 300~500r/min
5~8h of ball milling, obtains mixed-powder, mixed-powder is pressed into a diameter of 12~15mm under 220~250MPa pressure, thickness is
The disk of 1~2mm, and 8~10h is sintered at 1300~1450 DEG C, obtain medium temperature solid fuel cell electrolyte.
Example 1
1.8g gadolinium oxides are taken, 1.7g samarium oxides add in 100g mass fractions in 20% salpeter solution, to be stirred with 300r/min
34.7g cerium nitrate hexahydrates are added in after 15min, continues stirring and is completely dissolved to solid, add 9.6g citric acids, 2.9g ethylenediamines
Tetraacethyl, it is 8 that mass fraction is added dropwise after being uniformly mixed, which is 5% sodium hydroxide solution to pH, stands 15h, obtains reaction solution, will
Reaction solution is transferred in the water heating kettle with Teflon liner, carries out hydro-thermal reaction at 120 DEG C, the hydro-thermal reaction time 10h,
Filter residue is filtered to obtain after being cooled to room temperature, is washed with deionized again 2 times, then be placed in drying after washing filter residue 2 times with absolute ethyl alcohol
It in case, is dried at 120 DEG C to constant weight, obtains presoma, presoma is placed in Muffle furnace and lights generation self-propagating combustion and is anti-
Should, 3h is calcined in heat preservation at 700 DEG C again after burning, obtains electrolyte just powder, powder at the beginning of electrolyte is fitted into ball mill, then is added
Enter 0.08g titanium dioxide, 0.10g strontium oxide strontias, 20mL absolute ethyl alcohols with 300r/min ball milling 5h, obtain mixed-powder, by mixed powder
End is pressed into a diameter of 12mm under 220MPa pressure, and thickness is the disk of 1mm, and is sintered 8h at 1300 DEG C, obtain it is described in
Warm solid fuel cell electrolyte.
Example 2
2.3g gadolinium oxides are taken, 2.2g samarium oxides add in 125g mass fractions in 20% salpeter solution, to be stirred with 350r/min
43.7g cerium nitrate hexahydrates are added in after 17min, continues stirring and is completely dissolved to solid, add 12g citric acids, 3.6g ethylenediamines
Tetraacethyl, it is 8.5 that mass fraction is added dropwise after being uniformly mixed, which is 5% sodium hydroxide solution to pH, stands 17h, obtains reaction solution,
Reaction solution is transferred in the water heating kettle with Teflon liner, hydro-thermal reaction is carried out at 150 DEG C, the hydro-thermal reaction time is
11h filters to obtain filter residue after being cooled to room temperature, be washed with deionized again 3 times, then be placed in after washing filter residue 2 times with absolute ethyl alcohol
It in drying box, is dried at 135 DEG C to constant weight, obtains presoma, presoma is placed in Muffle furnace and lights generation self- propagating combustion
Reaction is burnt, 4h is calcined in heat preservation at 750 DEG C again after burning, obtains electrolyte just powder, powder at the beginning of electrolyte is fitted into ball mill,
0.10g titanium dioxide, 0.13g strontium oxide strontias are added, 25mL absolute ethyl alcohols with 400r/min ball milling 7h, obtain mixed-powder, will be mixed
It closes powder and a diameter of 14mm is pressed under 235MPa pressure, thickness is the disk of 1mm, and is sintered 9h at 1375 DEG C, obtains institute
State medium temperature solid fuel cell electrolyte.
Example 3
2.7g gadolinium oxides are taken, 2.6g samarium oxides add in 150g mass fractions in 20% salpeter solution, to be stirred with 400r/min
52.1g cerium nitrate hexahydrates are added in after 20min, continues stirring and is completely dissolved to solid, add 14.4g citric acids, 4.4g second two
Amine tetraacethyl, it is 9 that mass fraction is added dropwise after being uniformly mixed, which is 5% sodium hydroxide solution to pH, stands 20h, obtains reaction solution,
Reaction solution is transferred in the water heating kettle with Teflon liner, hydro-thermal reaction is carried out at 180 DEG C, the hydro-thermal reaction time is
12h filters to obtain filter residue after being cooled to room temperature, be washed with deionized again 3 times, then be placed in after washing filter residue 3 times with absolute ethyl alcohol
It in drying box, is dried at 150 DEG C to constant weight, obtains presoma, presoma is placed in Muffle furnace and lights generation self- propagating combustion
Reaction is burnt, 5h is calcined in heat preservation at 800 DEG C again after burning, obtains electrolyte just powder, powder at the beginning of electrolyte is fitted into ball mill,
0.12g titanium dioxide, 0.15g strontium oxide strontias are added, 30mL absolute ethyl alcohols with 500r/min ball milling 8h, obtain mixed-powder, will be mixed
It closes powder and a diameter of 15mm is pressed under 250MPa pressure, thickness is the disk of 2mm, and is sintered 10h at 1450 DEG C, obtains institute
State medium temperature solid fuel cell electrolyte.
Medium temperature solid fuel cell electrolyte prepared by the present invention and the cell electrolyte of Shanghai company production
Material is detected, specific testing result such as following table table 1：
1 medium temperature solid fuel cell electrolyte performance characterization of table
The medium temperature solid fuel cell electrolyte that as shown in Table 1 prepared by the present invention, conductivity is high, the power density of battery
Greatly, grain size is smaller and uniform.
Claims (7)
1. a kind of preparation method of medium temperature solid fuel cell electrolyte, which is characterized in that specifically preparation process is：
（1）Gadolinium oxide, samarium oxide is taken to add in mass fraction to be uniformly mixed in 20% salpeter solution, adds in cerium nitrate hexahydrate stirring
It is completely dissolved to solid, adds citric acid, ethylenediamine tetra-acetic acid, sodium hydroxide solution is added dropwise after being uniformly mixed is to pH
8~9,15~20h is stood, obtains reaction solution；
（2）Reaction solution is transferred in the water heating kettle with Teflon liner and carries out hydro-thermal reaction, diafiltration is crossed after being cooled to room temperature
Drying is washed, obtains presoma；
（3）Presoma is placed in Muffle furnace and is lighted, self-propagating combustion reaction occurs, again at 700~800 DEG C after burning
3~5h of lower heat preservation calcining obtains electrolyte just powder；
（4）Powder at the beginning of electrolyte is fitted into ball mill, titanium dioxide, strontium oxide strontia, absolute ethyl alcohol are added, with 300~500r/
Min 5~8h of ball milling, obtain mixed-powder；
（5）It is mixed-powder is tabletted and be sintered, obtain medium temperature solid fuel cell electrolyte.
A kind of 2. preparation method of medium temperature solid fuel cell electrolyte as described in claim 1, which is characterized in that step
Suddenly（1）The gadolinium oxide, samarium oxide, cerium nitrate hexahydrate, citric acid, ethylenediamine tetra-acetic acid parts by weight for 1.8~2.7 parts oxidation
Gadolinium, 1.7~2.6 parts of samarium oxides, 34.7~52.1 parts of cerium nitrate hexahydrates, 9.6~14.4 parts of citric acids, 2.9~4.4 parts of ethylenediamines
Tetraacethyl.
A kind of 3. preparation method of medium temperature solid fuel cell electrolyte as described in claim 1, which is characterized in that step
Suddenly（2）The hydrothermal reaction process is 10~12h to carry out hydro-thermal reaction, the hydro-thermal reaction time at 120~180 DEG C.
A kind of 4. preparation method of medium temperature solid fuel cell electrolyte as described in claim 1, which is characterized in that step
Suddenly（4）The amount of titanium is the 2.96~6.67% of gadolinium oxide quality.
A kind of 5. preparation method of medium temperature solid fuel cell electrolyte as described in claim 1, which is characterized in that step
Suddenly（4）The strontium oxide strontia dosage is the 3.70~8.33% of gadolinium oxide quality.
A kind of 6. preparation method of medium temperature solid fuel cell electrolyte as described in claim 1, which is characterized in that step
Suddenly（5）The tabletted process is 1~2mm's to be pressed into a diameter of 12~15mm, thickness under 220~250MPa pressure
Disk.
A kind of 7. preparation method of medium temperature solid fuel cell electrolyte as described in claim 1, which is characterized in that step
Suddenly（5）The sintering process is that 8~10h is sintered at 1300~1450 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109638325A (en) * | 2018-12-18 | 2019-04-16 | 福州大学 | A kind of intermediate temperature solid oxide fuel cell electrolyte of strontium doping |
| CN112759392A (en) * | 2020-12-25 | 2021-05-07 | 合肥学院 | Multi-component co-doped cerium oxide-based solid electrolyte material and preparation method thereof |
-
2017
- 2017-12-30 CN CN201711491523.0A patent/CN108232259B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109638325A (en) * | 2018-12-18 | 2019-04-16 | 福州大学 | A kind of intermediate temperature solid oxide fuel cell electrolyte of strontium doping |
| CN109638325B (en) * | 2018-12-18 | 2022-03-15 | 福州大学 | Strontium-doped medium-temperature solid oxide fuel cell electrolyte |
| CN112759392A (en) * | 2020-12-25 | 2021-05-07 | 合肥学院 | Multi-component co-doped cerium oxide-based solid electrolyte material and preparation method thereof |
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