CN107611461A - A kind of preparation method of SOFC - Google Patents
A kind of preparation method of SOFC Download PDFInfo
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- CN107611461A CN107611461A CN201710922797.4A CN201710922797A CN107611461A CN 107611461 A CN107611461 A CN 107611461A CN 201710922797 A CN201710922797 A CN 201710922797A CN 107611461 A CN107611461 A CN 107611461A
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- 8ysz
- anode
- electrolyte
- sofc
- cell
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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
Abstract
The invention discloses a kind of preparation method of SOFC, solid fuel cell is made up of anode, negative electrode and electrolyte, and its Anodic is the compound porous structure that NiO, 8YSZ and graphite mixture form, and electrolyte is fine and close 8Y ZrO2（8YSZ）After the compression molding of low pressure, it is compressing to apply 200 400MPa pressure at 100 150 DEG C for ion conductive layer, anode layer and dielectric substrate, is then burnt altogether at a temperature of 1,150 1350 DEG C of C and forms half-cell, then passes through screen-printing deposition negative electrode and form monocell.The present invention can effectively improve the compact density of 8YSZ electrolyte, and then reduce co-fired temperature on the premise of 8YSZ electrolyte consistency is ensured, improve the chemical property of monocell.
Description
Technical field
The invention belongs to SOFC technical field, and in particular to a kind of SOFC
Preparation method.
Background technology
SOFC (SOFC) is to use solid oxide electrolyte as barrier film, will by electrochemical reaction
The chemical energy of fuel is converted directly into a kind of generation technology of electric energy.In all fuel cells, solid oxide fuel electricity
Pond is that what is had found be converted into the maximally effective device of electric energy by fuel chemical energy.SOFC application is quite extensive, almost
Cover all conventional electric power markets, including house with, commercially use, industrial/live generator, and government utility generates electricity
Factory etc., or even compact power, portable power source, electricity consumption from far-off regions and high quality power supply etc. are applied also for, wherein to stand
Commercial power source, industrial heat chp system and the Miniature Power Unit market prospects of type are more good.
The good SOFC anode materials of now widely used performance comparision are mainly Ni/8YSZ（The oxidation of stabilized with yttrium oxide
Zirconium）Cermet.Because SOFC anodes need to provide the transport channel of fuel gas, therefore anode construction should be porosity and looseness；And
And the Ni particles easy agglomeration, and abnormal growth at high temperature in anode, this can reduce SOFC three phase boundary length, institute
So that the sintering temperature of anode should be reduced.But anode and 8YSZ electrolyte are in and burnt altogether, the sintering temperature for reducing anode will certainly
The consistency of electrolyte is influenceed, so as to influence the ionic conduction of electrolyte.In order to ensure the consistency of electrolyte, usual anode and
The co-fired temperature of electrolyte need to reach 1400oMore than C.Therefore, if can be reduced on the premise of 8YSZ electrolyte consistency is ensured
Co-fired temperature, with regard to anode performance can be effectively improved, while save a large amount of energy consumptions.
The content of the invention
In order to solve the deficiencies in the prior art, it is an object of the invention to provide a kind of system of SOFC
Preparation Method, it is desirable to provide a kind of new half-cell green compact forming method, effectively improve the compact density of 8YSZ electrolyte, Jin Er
Ensure to reduce co-fired temperature on the premise of 8YSZ electrolyte consistency, improve the chemical property of monocell.
In order to realize above-mentioned technical purpose, the technical scheme is that：
A kind of preparation method of SOFC, it comprises the following steps：
1）In mass ratio 4:6:1 to weigh NiO, 8YSZ and graphite be anode material, and using ethanol as abrasive media, anode material is mixed
Anode powder is made in drying after merging is fully ground 24 hours；
2）Weigh a certain amount of anode powder and be put into mould and flatten, the anode layer as half-cell；
3）A certain amount of 8YSZ nano-powders are weighed, add its weight 10-30% deionized water, are fully ground in mortar
Even obtained electrolyte raw material, is then equably covered in step 2 by electrolyte raw material）Half-cell anode layer in described mould
Top；
4）It is compressing to apply 200-400Mpa pressure at a temperature of 100 DEG C -150 DEG C, pressurize 20-40 minutes, obtains half-cell
Green compact；
5）Above-mentioned half-cell green compact are placed in Muffle furnace, 3.5-4 hours are sintered at a temperature of 1150-1350 DEG C, it is then natural
Room temperature is cooled to, obtains half-cell；
6）Above-mentioned half-cell is coated into negative electrode with the mode of silk-screen printing, is placed in Muffle furnace sintering 2- in 1050-1100 DEG C
2.5h obtains monocell, i.e., described SOFC.
Further, the step 2）The anode powder weighed and step 3）The mass ratio of the 8YSZ nano-powders weighed is
0.25-0.3∶0.02。
Preferably, the step 2）The anode powder weighed and step 3）The mass ratio of the 8YSZ nano-powders weighed is 0.3:
0.02。
The step 2）, anode powder application 50MPa pressure is flattened.
The step 3）, the particle diameter of 8YSZ nano-powders is 20nm.
The step 6）, cathode material is 7 in mass ratio by LSCF and 8YSZ:3 compositions.
The step 6）Obtained SOFC, the thickness of its anode is 500-800 μm, the thickness of negative electrode
For 50-80 μm, the thickness of electrolyte is 20-30 μm.
The present invention uses above technical scheme, and solid fuel cell is made up of anode, negative electrode and electrolyte, and its Anodic is
NiO, 8YSZ and graphite mixture composition compound porous structure, electrolyte is fine and close 8Y-ZrO2（8YSZ）Ion conductive layer, sun
Pole layer and dielectric substrate are after the compression molding of low pressure, and application 200-400MPa pressure is compressing at 100-150 DEG C, then
Burnt altogether at a temperature of 1150-1350 DEG C and form half-cell, then monocell is formed by screen-printing deposition negative electrode.
Research finds that green density has significant effect to the sintering characteristic and electric property of 8YSZ electrolyte, therefore carries
The green density of high 8YSZ electrolyte, there is very big facilitation to preparing high-performance SOFC batteries.The present invention by
A certain proportion of deionized water is added in 8YSZ nano-powders, in design temperature and forming under the pressure, compact density can be obtained
Very high 8YSZ dielectric substrate green compact.Compared with prior art, beneficial effects of the present invention are：
（1）8YSZ green densities are obtained by the inventive method and reach more than 70%, its consistency after sinter at 1200 DEG C and
Consistency is suitable at 1400 DEG C of tradition.After being sintered with the anode that electrolyte burns altogether at 1200 DEG C, crystallite dimension substantially reduces, and
Without agglomeration phenomenon.
（2）The raising of dielectric substrate green density makes anode/electrolyte co-fired temperature scope widen significantly, improves production
The flexibility ratio of technique.
（3）Conventional anode/electrolyte co-fired temperature is 1400oC, after being improved by the inventive method, it can drop significantly
Required energy consumption is sintered in low production process, improves product competitiveness.
Brief description of the drawings
The present invention is further elaborated with reference to the accompanying drawings and detailed description：
Fig. 1 is that the 8YSZ electrolyte that embodiment 2 obtains sinters the scanning electron microscope (SEM) photograph after 1200 DEG C；
Fig. 2 is the scanning electron microscope (SEM) photograph after 1200 DEG C of the anode sintering that embodiment 2 obtains.
Embodiment
A kind of preparation method of SOFC, it comprises the following steps：
1）In mass ratio 4:6:1 to weigh NiO, 8YSZ and graphite be anode material, and using ethanol as abrasive media, anode material is mixed
Anode powder is made in drying after merging is fully ground 24 hours；
2）Weigh a certain amount of anode powder to be put into mould, the pressure for applying 50MPa is flattened, the anode as half-cell
Layer；
3）The 8YSZ nano-powders that a certain amount of particle diameter is 20nm are weighed, its weight 10-30% deionized water are added, in mortar
In be fully ground uniformly obtained electrolyte raw material, electrolyte raw material is equably then covered in step 2）In described mould
Above half-cell anode layer；
Wherein, step 2）The anode powder weighed and step 3）The mass ratio of the 8YSZ nano-powders weighed is 0.25-0.3: 0.02.
4）It is compressing to apply 200-400Mpa pressure at a temperature of 100 DEG C -150 DEG C, pressurize 20-40 minutes, obtains half
Battery green compact；
5）Above-mentioned half-cell green compact are placed in Muffle furnace, 3.5-4 hours are sintered at a temperature of 1150-1350 DEG C, it is then natural
Room temperature is cooled to, obtains half-cell；
6）Above-mentioned half-cell is coated into negative electrode with the mode of silk-screen printing, cathode material is 7 in mass ratio by LSCF and 8YSZ:3
Composition, it is placed in Muffle furnace obtaining monocell in 1050-1100 DEG C of sintering 2-2.5h, i.e., described solid oxide fuel electricity
Pond.
The SOFC that the present invention obtains, the thickness of its anode is 500-800 μm, and the thickness of negative electrode is
50-80 μm, the thickness of electrolyte is 20-30 μm.
Embodiment 1
A kind of preparation method of SOFC, comprises the following steps：
1）In mass ratio 4:6:1 to weigh NiO, 8YSZ and graphite be anode material, and using ethanol as abrasive media, anode material is mixed
Anode powder is made in drying after merging is fully ground 24 hours；
2）The anode powder for weighing 0.3g is put into mould with the pressing of 50MPa pressure, the anode layer as half-cell；
3）Weigh 0.02g 8YSZ nano-powders（Particle diameter 20nm）, the deionized water of its weight 10% is added, it is abundant in mortar
Grinding uniformly obtains electrolyte raw material, and the electrolyte raw material after grinding is equably then covered in into step 2）Mould Anodic layer
Top, at 100 DEG C apply 200Mpa pressure it is compressing, pressurize 20 minutes, obtain half-cell green compact；
At the same time, 0.25g 8YSZ powders, the deionized water of its weight 10% is added, is molded to obtain with same temperature and pressure
8YSZ electrolyte green compact；With electronic balance precise green body quality, with slide measure and micrometer measure respectively its diameter and
Thickness, its density then is calculated with the ratio between quality volume（That is electrolyte green density）For 71.2%；
4）Above-mentioned half-cell green compact and 8YSZ electrolyte green compact are placed in Muffle furnace, 4h is sintered at 1150 DEG C, it is then natural
It is cooled to room temperature, you can obtain half-cell and 8YSZ electrolyte, wherein 8YSZ electrolyte consistency reaches 97.1%；
5）Half-cell after sintering is coated into negative electrode with the mode of silk-screen printing, cathode material is in mass ratio by LSCF and 8YSZ
7:3 compositions, it is placed in 1100 DEG C of sintering 2h in Muffle furnace and obtains monocell, at 800 DEG C, power density reaches 0.501A/
cm2。
Embodiment 2
A kind of preparation method of SOFC, comprises the following steps：
1）In mass ratio 4:6:1 to weigh NiO, 8YSZ and graphite be anode material, and using ethanol as abrasive media, anode material is mixed
Anode powder is made in drying after merging is fully ground 24 hours；
2）The anode powder for weighing 0.3g is put into mould with the pressing of 50MPa pressure, the anode layer as half-cell；
3）Weigh 0.02g 3YSZ nano-powders（Particle diameter 20nm）, the water of its weight 20% is added, is fully ground in mortar
It is even to obtain electrolyte raw material, the electrolyte raw material after grinding is equably then covered in step 2）Mould Anodic layer it is upper
Side, application 400Mpa pressure is compressing at 150 DEG C, pressurize 40 minutes, obtains half-cell green compact；
At the same time, 0.25g 8YSZ powders are taken, add the deionized water of its weight 20%, are molded with same temperature and pressure
Obtain 8YSZ electrolyte green compact；With electronic balance precise green body quality, it is straight that its is measured respectively with slide measure and micrometer
Footpath and thickness, its density then is calculated with the ratio between quality volume（That is electrolyte green density）For 74.5%；
4）Above-mentioned half-cell green compact and 8YSZ electrolyte green compact are placed in Muffle furnace, 4h is sintered at 1200 DEG C, it is then natural
It is cooled to room temperature, you can obtain half-cell and 8YSZ electrolyte, wherein 8YSZ electrolyte consistency reaches 98.7%；
5）Half-cell after sintering is coated into negative electrode with the mode of silk-screen printing, cathode material is in mass ratio by LSCF and 8YSZ
7:3 compositions, it is placed in Muffle furnace obtaining monocell in 1100 DEG C of sintering 2h.At 800 DEG C, power density reaches 0.579A/
cm2。
Fig. 1 is that the present embodiment 8YSZ electrolyte sinters the scanning electron microscope (SEM) photograph after 1200 DEG C, and 200 DEG C are reduced in sintering temperature
In the case of, the consistency after 8YSZ sintering is higher, reaches the level under 1400 DEG C of sintering of tradition；
Fig. 2 is the scanning electron microscope (SEM) photograph after 1200 DEG C of the present embodiment anode sintering, in the case where sintering temperature reduces by 200 DEG C, sun
The agglomeration of pole crystal grain, the ill effect of abnormal growth are greatly improved.
Embodiment 3
A kind of preparation method of SOFC, comprises the following steps：
1）In mass ratio 4:6:1 to weigh NiO, 8YSZ and graphite be anode material, and using ethanol as abrasive media, anode material is mixed
Anode powder is made in drying after merging is fully ground 24 hours；
2）The anode powder for weighing 0.3g is put into mould with the pressing of 50MPa pressure, the anode layer as half-cell；
3）Weigh 0.02g 3YSZ nano-powders（Particle diameter 20nm）, the water of its weight 30% is added, is fully ground in mortar
It is even to obtain electrolyte raw material, the electrolyte raw material after grinding is equably then covered in step 2）Mould Anodic bottom it is upper
Side, application 300Mpa pressure is compressing at 120 DEG C, pressurize 30 minutes, obtains half-cell green compact；
At the same time, 0.25g 8YSZ powders are taken, add the deionized water of its weight 30%, are molded with same temperature and pressure
Obtain 8YSZ electrolyte green compact；With electronic balance precise green body quality, it is straight that its is measured respectively with slide measure and micrometer
Footpath and thickness, its density then is calculated with the ratio between quality volume（That is electrolyte green density）For 73.2%；
4）Above-mentioned half-cell green compact and 8YSZ electrolyte green compact are placed in Muffle furnace, 3.5h is sintered at 1350 DEG C, then certainly
So it is cooled to room temperature, you can obtain half-cell and 8YSZ electrolyte.Wherein 8YSZ electrolyte consistency reaches 98.5%；
5）Half-cell after sintering is coated into negative electrode with the mode of silk-screen printing, cathode material is in mass ratio by LSCF and 8YSZ
7:3 compositions, it is placed in 1050 DEG C of sintering 2.5h in Muffle furnace and obtains monocell.At 800 DEG C, power density reaches 0.561A/
cm2。
Claims (7)
- A kind of 1. preparation method of SOFC, it is characterised in that：It comprises the following steps：1）In mass ratio 4:6:1 to weigh NiO, 8YSZ and graphite be anode material, and using ethanol as abrasive media, anode material is mixed Anode powder is made in drying after merging is fully ground；2）Weigh a certain amount of anode powder and be put into mould and flatten, the anode layer as half-cell；3）A certain amount of 8YSZ nano-powders are weighed, add its weight 10-30% deionized water, are fully ground in mortar Even obtained electrolyte raw material, is then equably covered in step 2 by electrolyte raw material）Half-cell anode layer in described mould Top；4）It is compressing to apply 200-400Mpa pressure at a temperature of 100 DEG C -150 DEG C, pressurize 20-40 minutes, obtains half-cell Green compact；5）Above-mentioned half-cell green compact are placed in Muffle furnace, 3.5-4 hours are sintered at a temperature of 1150-1350 DEG C, it is then natural Room temperature is cooled to, obtains half-cell；6）Above-mentioned half-cell is coated into negative electrode with the mode of silk-screen printing, is placed in Muffle furnace sintering 2- in 1050-1100 DEG C 2.5h obtains monocell, i.e., described SOFC.
- A kind of 2. preparation method of SOFC according to claim 1, it is characterised in that：The step 2）The anode powder weighed and step 3）The mass ratio of the 8YSZ nano-powders weighed is 0.25-0.3: 0.02.
- A kind of 3. preparation method of SOFC according to claim 2, it is characterised in that：The step 2）The anode powder weighed and step 3）The mass ratio of the 8YSZ nano-powders weighed is 0.3: 0.02.
- A kind of 4. preparation method of SOFC according to claim 1, it is characterised in that：The step 2）, anode powder application 50MPa pressure is flattened.
- A kind of 5. preparation method of SOFC according to claim 1, it is characterised in that：The step 3）, the particle diameter of 8YSZ nano-powders is 20nm.
- A kind of 6. preparation method of SOFC according to claim 1, it is characterised in that：The step 6）, cathode material is 7 in mass ratio by LSCF and 8YSZ:3 compositions.
- A kind of 7. preparation method of SOFC according to claim 1, it is characterised in that：The step 6）Obtained SOFC, the thickness of its anode is 500-800 μm, and the thickness of negative electrode is 50-80 μm, electrolyte Thickness be 20-30 μm.
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Cited By (3)
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| CN110137551A (en) * | 2019-05-17 | 2019-08-16 | 福州大学 | A kind of SOFC and preparation method thereof of three pole cofiring |
| CN114188579A (en) * | 2022-01-04 | 2022-03-15 | 徐州华清京昆能源有限公司 | High-strength heat-resistant circulating fuel cell |
| CN114335586A (en) * | 2022-01-04 | 2022-04-12 | 苏州华清京昆新能源科技有限公司 | Method for improving flatness of product after sintering of semi-cell isolation layer |
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| CN114335586A (en) * | 2022-01-04 | 2022-04-12 | 苏州华清京昆新能源科技有限公司 | Method for improving flatness of product after sintering of semi-cell isolation layer |
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Application publication date: 20180119 |