CN108736051A - A kind of preparation method of the electrolytic thin-membrane barrier layer of intermediate temperature SOFC - Google Patents
A kind of preparation method of the electrolytic thin-membrane barrier layer of intermediate temperature SOFC Download PDFInfo
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- CN108736051A CN108736051A CN201810262013.4A CN201810262013A CN108736051A CN 108736051 A CN108736051 A CN 108736051A CN 201810262013 A CN201810262013 A CN 201810262013A CN 108736051 A CN108736051 A CN 108736051A
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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
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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
- H01M8/1253—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 zirconium oxide
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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
- H01M2008/1293—Fuel cells with solid oxide electrolytes
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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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- 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
- H01M2300/0094—Composites in the form of layered products, e.g. coatings
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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
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Abstract
The invention discloses a kind of preparation methods of the electrolytic thin-membrane barrier layer of intermediate temperature SOFC, include the following steps：S1：Anode powder NiO and starch are taken, pore creating material is made in mixed grinding in the agate mortar, keeps its surfacing smooth；S2：Zirconium powder is added in mold, the Anode blank that thickness is 1.2-1.5mm is pressed into；S3：Then the Anode blank suppressed is pre-sintered 5-7h；S4：GDC powder is made by EDTA- citric acid combustion synthesis methods, appropriate dispersant and acetone ball milling 3h or more is added in GDC powder；S5：Organic bond is added, ball milling 12h obtains the gelatinous thick liquid of milky, acetone evaporated into tasteless；S6：Start spin coater and carries out coating；S7：The supporter for coating film is transferred in high temperature furnace and is sintered.
Description
Technical field
The present invention relates to solid oxide fuel cell manufacturing technology field more particularly to a kind of electrolyte of intermediate temperature SOFC
The preparation method of thin-film barrier layers.
Background technology
Solid oxide fuel cell SOFC (Solid Oxide Fuel Cell) has energy conversion efficiency high (primary
Generating efficiency 50%~60%), advantage at low cost, long-time stability are good, especially can directly use it is various containing carbons fire
Material, such as using fossil fuel as gases such as the natural gas (CH4) of representative, coal gas (underground gasified gas, coke-stove gas, coal bed gas)
Fuel can also be widened further to the reproducible biomass fuel such as biogas and biogas, be derived from a wealth of sources, it is easy to it is existing
There is energy resources supply system compatibility.So solid oxide fuel cell is high based on being realized in existing energy supply system
Imitate the very promising new energy technology of power generation.
Realize that the key of SOFC industrialization is to reduce the cost of battery, and the effective ways for reducing cost are to reduce battery
Operating temperature.The selection of the electrolyte and electrode material of SOFC is very crucial, and the electrochemical properties of one side material itself determine
The performance of battery, between another aspect electrolyte and electrode the microstructure and atomic arrangement at interface all consumingly affect boundary
The electrochemical properties in face, and then influence the performance of battery.Due in SOFC assembling process high-temperature process and at the operation duration phase
In hot environment, traditional sofc cathode LSM, LSMC, LSC, LSCF etc. can change with electrolyte YSZ on interface
Reaction is learned, zirconic acid lanthanum La2Zr2O7 and strontium zirconate SrZrO3 is generated.Due to the ionic conductivity ratio YSZ of La2ZrO7, SrZr03
Low several orders of magnitude, this has just seriously affected the overall performance of SOFC, and interfacial reaction is also performance degradation in SOFC operational process
The main reason for, therefore the research tool of interfacial reaction has very important significance.Since YSZ is the electrolyte for comparing sizing,
So under the premise of ensureing that battery has ideal output performance, can usually be solved the problems, such as by following three approach：
(1) optimize cathode material, the method for such as adulterating LSM can play interfacial reaction certain inhibiting effect；(2)
Novel electrolyte is developed, the conductivity higher than traditional yttria-stabilized zirconia (YSZ) electrolyte is obtained；(3) exist
Increasing by one layer of GDC barrier material between cathode and electrolyte YSZ, YSZ be made | GDC thin-film electrolytes avoid interfacial reaction.
It is the focus and emphasis of low temperature research in current SOFC in terms of three above.
In traditional YSZ electrolyte-supporting types SOFC, supporters of the YSZ as entire battery is made respectively on its two sides
Standby anode and cathode is to form single battery.If reducing electrolyte thickness, YSZ thin-film electrolytes are made, due to the machinery of film
Limited strength, cannot function as the supporter of entire battery, thus need anode or cathode as supporter.At present research compared with
More is using anode as supporter, and it is a key during entire anode support type SOFC makes to prepare thin dense electrolyte film
Link.If electrolytic thin-membrane gas leakage can reduce the open-circuit voltage of battery, the output performance of battery is seriously affected, therefore, exploitation is high
The electrolyte thin membrane preparation method of cost performance is always the hot spot of the direction that SOFC research worker makes great efforts and current research.
Due to the conductivity and its thickness exponent function relation of electrolyte, as thickness increases, conductivity is with exponential relationship
Decline, its electrical property of extreme influence, therefore the thickness of general electrolyte is 10~30 μm, so the preparation process of barrier layer is necessary
Ensure that the thickness of film is very low.In addition to the requirement of electrolyte thickness, the gas for requiring to also have electrolyte most important to electrolyte
Close property, electrolyte are a thin layers between anode and cathode, are to be spaced the oxidation of battery and reduction reaction only
A thin layer will lead to the decaying and destruction of battery quickly if the gas on electrolyte both sides is mutually collaborated.
Therefore, the prior art has much room for improvement.
Invention content
In order to solve the above technical problem, the present invention provides a kind of preparation sides of the electrolytic thin-membrane barrier layer of intermediate temperature SOFC
Method, using slurry spin coating technique, electrolyte thin film thickness obtained is thin, consistency is high, it can be achieved that industrialized production.
The specific technical solution of the present invention is：
A kind of preparation method of the electrolytic thin-membrane barrier layer of intermediate temperature SOFC, wherein include the following steps：
S1：Anode powder NiO and starch are taken, pore creating material is made in mixed grinding in the agate mortar, takes pore creating material in stainless
In steel mold, powder is paved, applies pressure, keeps its surfacing smooth；
S2：Zirconium powder is added in mold, paves Zirconium powder, and thickness is depressed in the pressure of 350MPa
For the Anode blank of 1.2-1.5mm；
S3：Then the Anode blank suppressed is pre-sintered 5-7h, the supporter as spin coating GDC electrolytic thin-membranes；
S4：GDC powder is made by EDTA- citric acid combustion synthesis methods, appropriate dispersant and acetone is added in GDC powder
Ball milling 3h or more opens the reunion in GDC powder to reduce the grain size of powder, improves the uniformity of GDC powder；
S5：According to GDC powder: organic bond=1：2 mass ratio weighs addition organic bond, and ball milling 12h is obtained
The gelatinous thick liquid of milky, constant temperature preserves after taking-up, acetone is evaporated into tasteless；
S6：The anode-supported piece of pre-sintering is placed on the turntable of spin coater, viscous fluid is added dropwise toward support chip center
Body starts spin coater progress coating after opening vacuum pump operation 30s, and 500 DEG C of annealing heat preservation 30min are applied again after being painted with the first tunic
Next layer repeats 3~4 layers of spin coating to ensure the thickness of film；
S7：The supporter for coating film is transferred in high temperature furnace and is sintered, sintering step is:Heating rate control is 3
DEG C/min, 300 DEG C of heat preservation 10min, 800 DEG C keep the temperature 10min, keep the temperature 5h at 1350 DEG C, are then down to room with the rate of 3 DEG C/min
Temperature.
The preparation method of the electrolytic thin-membrane barrier layer of a kind of intermediate temperature SOFC, wherein be pre-sintered in the step S3
Mode is：Heating rate control is 3 DEG C/min；300 DEG C of heat preservation 10min；800 DEG C of heat preservation 10min；5h is kept the temperature at 1350 DEG C；So
Room temperature is down to the rate of 3 DEG C/min afterwards.
The preparation method of the electrolytic thin-membrane barrier layer of a kind of intermediate temperature SOFC, wherein organic in the step S5
Adhesive contains the terpinol of 6% ethyl cellulose.
A kind of preparation method of the electrolytic thin-membrane barrier layer of intermediate temperature SOFC, wherein spin coater in the step S6
Setting operation parameter be：V1=800r/min at a slow speed, t1=10s；Quick v2=3500r/min, t2=30s.
The preparation method of the electrolytic thin-membrane barrier layer of a kind of intermediate temperature SOFC, wherein be pre-sintered in the step S6
Mode：Heating rate is 3 DEG C/min；300 DEG C of heat preservation 10min；500 DEG C of heat preservation 30min；Then it is down to the rate of 3 DEG C/min
Room temperature.
Advantageous effect：The present invention provides a kind of preparation method of the electrolytic thin-membrane barrier layer of intermediate temperature SOFC, in anode branch
The pre-sintering temperature of support body is 1350 DEG C, the content of GDC is 50% in spin coating slurry, the item that the spin coating number of plies of electrolyte is 4 layers
Under part, the preferable GDC barrier layers electrolytic thin-membrane of compactness has successfully been made.
Description of the drawings
Fig. 1 is battery cross-section diagram made from embodiment 1；
Fig. 2 is cell I-V made from embodiment 1 and I-P curve graphs；
Fig. 3 is battery cross-section diagram made from embodiment 2；
Fig. 4 is cell I-V made from embodiment 2 and I-P curve graphs.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1
S1：It takes a certain amount of anode powder NiO that suitable starch is added and makees pore creating material, in the agate mortar mixed grinding 1h
Afterwards, it takes appropriate mixed-powder in the stainless steel mould of a diameter of 15mm, paves powder, give pressure appropriate, make its surface
Flat smooth；
S2：Continue appropriate YSZ powders being added in mold, by adjusting bolt, paves YSZ powders, and in 350MPa
Pressure depress to thickness be 1.2mm Anode blank；
S3：Then the Anode blank suppressed is obtained into anode support in lower pre-sintering 5h；
S4：Appropriate GDC powder is mixed with KD1, proper amount of acetone solvent ball milling 3h is added, to reduce powder reunion, improves powder
Last uniformity；
S5：The GDC that above-mentioned ball milling is crossed is added in the appropriate organic bond terpinol of 6% ethyl cellulose (contain), into
The ball milling of row 12h obtains GDC slurries；
S6：By on the electrolyte YSZ of above-mentioned slurry for rotary coating to anode support, parameter is set as：V1=800r/ at a slow speed
Min, t1=10s；Quick v2=3 500r/min, t2=30s.Then 500 DEG C of annealing keeps the temperature 30min；
S7：Spin coating 3 times is repeated, finally 1350 DEG C of annealing 5h in high temperature furnace；
Fig. 1 is the section SEM of anode-supported monocell obtained, as we can see from the figure the GDC resistances after 2 spin coatings
Spacer structure densification is smooth, and thickness is about 5 μm；Fig. 2 is I-V, I-P curve of monocell, and the open-circuit voltage at 800 DEG C is
1.08V, maximum power density 550Wcm-2.
Embodiment 2
S1：It takes a certain amount of anode powder NiO that suitable starch is added and makees pore creating material, in the agate mortar mixed grinding 1h
Afterwards, it takes appropriate mixed-powder in the stainless steel mould of a diameter of 15mm, paves powder, give pressure appropriate, make its surface
Flat smooth；
S2：Continue appropriate YSZ powders being added in mold, by adjusting bolt, paves YSZ powders, and in 350MPa
Pressure depress to thickness be 1.2mm Anode blank；
S3：Then the Anode blank suppressed is obtained into anode support in lower pre-sintering 5h；
S4：Appropriate GDC powder is mixed with KD1, proper amount of acetone solvent ball milling 3h is added, to reduce powder reunion, improves powder
Last uniformity；
S5：The GDC that above-mentioned ball milling is crossed is added in the appropriate organic bond terpinol of 6% ethyl cellulose (contain), into
The ball milling of row 12h obtains GDC slurries；
S6：By on the electrolyte YSZ of above-mentioned slurry for rotary coating to anode support, parameter is set as：V1=800r/ at a slow speed
Min, t1=10s；Quick v2=3 500r/min, t2=30s.Then 500 DEG C of annealing keeps the temperature 30min；
S7：Spin coating 4 times is repeated, finally 1350 DEG C of annealing 5h in high temperature furnace；
Fig. 3 is the section SEM of anode-supported monocell obtained, as we can see from the figure the GDC resistances after 4 spin coatings
Spacer structure densification is smooth, and thickness is about 5 μm；Fig. 4 is I-V, I-P curve of monocell, and the open-circuit voltage at 800 DEG C is
1.06V, maximum power density 620Wcm-2.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention, every according to the present invention
Technical spirit still falls within the technology of the present invention side to any simple modification, change and equivalent transformation made by above example
The protection domain of case.
Claims (5)
1. a kind of preparation method of the electrolytic thin-membrane barrier layer of intermediate temperature SOFC, which is characterized in that include the following steps：
S1：Anode powder NiO and starch are taken, pore creating material is made in mixed grinding in the agate mortar, takes pore creating material in stainless steel mold
In tool, powder is paved, applies pressure, keeps its surfacing smooth；
S2：Zirconium powder is added in mold, paves Zirconium powder, and depress to thickness in the pressure of 350MPa and be
1.2-1.5mm Anode blank；
S3：Then the Anode blank suppressed is pre-sintered 5-7h, the supporter as spin coating GDC electrolytic thin-membranes；
S4：GDC powder is made by EDTA- citric acid combustion synthesis methods, appropriate dispersant and acetone ball milling is added in GDC powder
3h or more opens the reunion in GDC powder to reduce the grain size of powder, improves the uniformity of GDC powder；
S5：According to GDC powder: organic bond=1：2 mass ratio weighs addition organic bond, and ball milling 12h obtains milky white
The gelatinous thick liquid of color, constant temperature preserves after taking-up, acetone is evaporated into tasteless；
S6：The anode-supported piece of pre-sintering is placed on the turntable of spin coater, thick liquid is added dropwise toward support chip center, beats
Open and start spin coater after vacuum pump operation 30s and carry out coating, be painted with 500 DEG C of annealing heat preservation 30min after the first tunic apply again it is next
Layer repeats 3~4 layers of spin coating to ensure the thickness of film；
S7：The supporter for coating film is transferred in high temperature furnace and is sintered, sintering step is:Heating rate control for 3 DEG C/
Min, 300 DEG C of heat preservation 10min, 800 DEG C keep the temperature 10min, keep the temperature 5h at 1350 DEG C, are then down to room temperature with the rate of 3 DEG C/min.
2. the preparation method of the electrolytic thin-membrane barrier layer of a kind of intermediate temperature SOFC according to claim 1, which is characterized in that institute
Stating pre-sintering mode in step S3 is：Heating rate control is 3 DEG C/min；300 DEG C of heat preservation 10min；800 DEG C of heat preservation 10min；
5h is kept the temperature at 1350 DEG C；Then room temperature is down to the rate of 3 DEG C/min.
3. the preparation method of the electrolytic thin-membrane barrier layer of a kind of intermediate temperature SOFC according to claim 1, which is characterized in that institute
State the terpinol that the organic bond in step S5 contains 6% ethyl cellulose.
4. the preparation method of the electrolytic thin-membrane barrier layer of a kind of intermediate temperature SOFC according to claim 1, which is characterized in that institute
The setting operation parameter for stating spin coater in step S6 is：V1=800r/min at a slow speed, t1=10s；Quick v2=3 500r/min,
T2=30s.
5. the preparation method of the electrolytic thin-membrane barrier layer of a kind of intermediate temperature SOFC according to claim 1, which is characterized in that institute
It states in step S6 and is pre-sintered mode：Heating rate is 3 DEG C/min；300 DEG C of heat preservation 10min；500 DEG C of heat preservation 30min；Then with 3
DEG C/rate of min is down to room temperature.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111933980A (en) * | 2020-06-20 | 2020-11-13 | 中国矿业大学 | Method for preparing solid oxide fuel cell |
| CN113540489A (en) * | 2021-05-15 | 2021-10-22 | 山东工业陶瓷研究设计院有限公司 | Barrier layer slurry, preparation method, barrier layer preparation method and battery monomer |
| CN113929498A (en) * | 2021-09-16 | 2022-01-14 | 山东工业陶瓷研究设计院有限公司 | Coating for preparing barrier layer, preparation method of barrier layer and barrier layer |
| CN114725454A (en) * | 2022-04-06 | 2022-07-08 | 山东工业陶瓷研究设计院有限公司 | SOFC (solid oxide Fuel cell) and preparation method thereof |
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| CN113929498A (en) * | 2021-09-16 | 2022-01-14 | 山东工业陶瓷研究设计院有限公司 | Coating for preparing barrier layer, preparation method of barrier layer and barrier layer |
| CN114725454A (en) * | 2022-04-06 | 2022-07-08 | 山东工业陶瓷研究设计院有限公司 | SOFC (solid oxide Fuel cell) and preparation method thereof |
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