CN111653836B - High-temperature molten salt battery with functional layer and preparation method thereof - Google Patents
High-temperature molten salt battery with functional layer and preparation method thereof Download PDFInfo
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- CN111653836B CN111653836B CN202010561288.5A CN202010561288A CN111653836B CN 111653836 B CN111653836 B CN 111653836B CN 202010561288 A CN202010561288 A CN 202010561288A CN 111653836 B CN111653836 B CN 111653836B
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
- H01M10/38—Construction or manufacture
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
- H01M10/39—Accumulators not provided for in groups H01M10/05-H01M10/34 working at high temperature
- H01M10/399—Cells with molten salts
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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
- H01M2300/0048—Molten electrolytes used at high temperature
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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
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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
- H01M2300/0074—Ion conductive at high temperature
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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
- Y02E60/10—Energy storage using batteries
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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
- 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 relates to a high-temperature molten salt battery with a functional layer, which comprises a molten salt electrolyte, a solid electrolyte and the functional layer, wherein the functional layer is an electrolyte with high oxygen ion conduction and positioned between the solid electrolyte and the molten salt electrolyte, and the functional layer comprises more than 75wt% of cerium oxide. The invention also provides a preparation method of the high-temperature molten salt battery with the functional layer. According to the high-temperature molten salt battery with the functional layer, the cerium oxide is used as the substrate of the functional layer, the high-temperature molten salt battery has good corrosion resistance and oxygen ion conduction function, the dissolution and corrosion of the molten salt electrolyte to the solid electrolyte can be reduced, the increase of the internal resistance and internal consumption of the battery can be avoided, and the use requirement of the high-temperature molten salt battery can be well met.
Description
Technical Field
The present invention relates to a high-temperature molten salt battery, and more particularly, to a high-temperature molten salt battery having a functional layer and a method of manufacturing the same.
Background
The installed scales of wind power generation and photovoltaic power generation in China are at the top of the world, and the function of renewable energy power generation in modern power supply is more and more important. However, due to the defects of intermittency, fluctuation and the like of wind energy and solar energy, clean electricity converted from the wind energy and the solar energy is not used, a large amount of wind and electricity abandoning phenomena are generated, and the incredible waste is caused. The energy storage system can solve the problems of discontinuous, unstable and uncontrollable power generation of renewable resources, and is a necessary means for realizing safe and stable power supply. The high-temperature molten salt battery is a battery energy storage technology realized by using high-temperature molten salt, has low cost and capacity far higher than that of a normal-temperature battery energy storage technology, and is suitable for large-scale power grid energy storage.
In recent years, Licht, university of George Washington, USA, develops a high-temperature molten salt battery, which takes high-temperature molten salt as electrolyte to conduct oxygen ions, takes metal as active substance, and realizes the storage and release of electric energy by using the oxidation-reduction reaction between the metal and the oxygen ions. The battery has the advantages of low cost, large capacity and the like, and the theoretical energy storage capacity of the battery is far greater than that of normal-temperature batteries such as lithium ion batteries and the like. However, because the high-temperature molten salt has strong fluidity and the positive electrode and the negative electrode of the battery are isolated only by the high-temperature molten salt, the fluctuation or overflow phenomenon of the molten salt is easy to occur in the use process, so that the direct contact between the positive electrode and the negative electrode or the poor contact between the electrode and the high-temperature molten salt are caused, the short circuit or the open circuit of the battery is caused, and further, the dangers of overheating, service life reduction, failure, even explosion and the like of the battery are caused.
Recently, CN107437636A, the physical institute of shanghai application of chinese academy of sciences, proposed a high-temperature molten salt battery, in which a layer of dense solid electrolyte is added between the positive electrode and the high-temperature molten salt to physically separate the molten salt from the positive electrode. Therefore, the contact between the positive electrode and the negative electrode is effectively avoided, and the area of the positive electrode can be increased, so that the performances of the battery, such as charge-discharge current density, are improved. However, in the high-temperature molten salt battery, the solid electrolyte behaves for a long time in the presence of corrosion in a high-temperature molten salt environment, and a phase transition process of cubic phase to monoclinic phase may occur. The oxygen ion conduction rate is greatly weakened, the battery charge and discharge efficiency is reduced, the battery is finally failed, and the practical prospect of the high-temperature molten salt battery as a large-scale power grid energy storage battery is limited.
Disclosure of Invention
The invention provides a high-temperature molten salt battery with a functional layer and a preparation method thereof, aiming at solving the problems of corrosion, phase change and the like of a solid electrolyte in the prior art.
The invention provides a high-temperature molten salt battery with a functional layer, which comprises a molten salt electrolyte, a solid electrolyte and the functional layer, wherein the functional layer is an electrolyte with high oxygen ion conduction and positioned between the solid electrolyte and the molten salt electrolyte, and the functional layer comprises more than 75wt% of cerium oxide.
Preferably, the functional layer is integrated with the solid electrolyte. Particularly, the pressure generated by the difference of the expansion coefficients of the functional layer and the solid electrolyte at high temperature can be reduced through integration, and the cracking phenomenon of the functional layer and the solid electrolyte can be avoided.
Preferably, YSZ (i.e. Yttria-stabilized Zirconia) is selected as the solid electrolyte if the operating temperature of the high temperature molten salt battery is >800 ℃, and GDC (i.e. Gadolinia-Doped Ceria) or SSZ (i.e. Scandium-stabilized Zirconia) is selected as the solid electrolyte if the operating temperature of the high temperature molten salt battery is >600 ℃.
Preferably, the functional layer further comprises at least one dopant selected from the group consisting of zirconia, calcia and gadolinia. It will be appreciated that it is also fully feasible that the functional layer consists of only cerium oxide (i.e. no dopant), the selection of a particular dopant being contingent on the circumstances. For example, when the solid electrolyte is YSZ, the matching between the two can be improved and the functional layer can be made to withstand high temperatures by selecting zirconia as a dopant. Further, depending on the charge/discharge conditions, the resistance of the dopant must be considered in consideration of the current level, the charge/discharge time, and other problems.
Preferably, the mass fraction of the dopant in the functional layer is 1-25%.
Preferably, the mass ratio of the functional layer to the solid electrolyte is 0.2 to 0.45.
Preferably, the molten salt electrolyte is potassium carbonate, sodium carbonate, lithium carbonate, a mixed salt or eutectic salt thereof.
Preferably, the high temperature molten salt battery further includes a positive electrode separated from the molten salt electrolyte by the solid electrolyte and a negative electrode provided in the molten salt electrolyte.
The present invention also provides a method for preparing the high temperature molten salt battery having the functional layer, wherein the functional layer is formed by at least one process selected from the group consisting of an isostatic pressing method, a tape casting method, a chemical vapor deposition method, an electrochemical vapor deposition method, an electrical pulse deposition method, a sol-gel method, a sputtering method, an electron beam evaporation coating method, a physical vapor deposition method, and a spray coating process.
Preferably, the solid electrolyte is provided by a first powder and the functional layer is provided by a second powder, the first powder and the second powder are brought into intimate contact by tabletting and sintering, while the stable transition layer is formed by dense sintering of the interface. In particular, the particle size of the first powder is close to that of the second powder, so that an interface layer formed between the two phases is more stable during high-temperature sintering, and cracks and breakage are not easy to occur. In particular, the particle size of the first powder and the particle size of the second powder are equal. In a preferred embodiment, the particle size of the first powder and the particle size of the second powder are both 2 microns.
Preferably, the functional layer is directly formed on the solid electrolyte sheet by a casting method, and an excess component is removed by calcination.
According to the high-temperature molten salt battery with the functional layer, the cerium oxide is used as the substrate of the functional layer, the high-temperature molten salt battery has good corrosion resistance and oxygen ion conduction function, the dissolution and corrosion of the molten salt electrolyte to the solid electrolyte can be reduced, the increase of the internal resistance and internal consumption of the battery can be avoided, and the use requirement of the high-temperature molten salt battery can be well met. In particular, according to the high-temperature molten salt battery with the functional layer, the phase transition of the solid electrolyte in the high-temperature long-time operation (for example, the ZrO in YSZ can be caused by the high-temperature long-time operation) can be avoided by the functional layer2Phase transformation occurs) to avoid a decrease in the oxygen ion conductivity of the solid electrolyte. The preparation method provided by the invention has the advantages of simple process, short flow, no need of complex equipment, and easiness in realization and popularization in the high-temperature molten salt battery.
Drawings
FIG. 1 shows an integrated solid electrolyte and functional layers of a high temperature molten salt battery according to a preferred embodiment of the invention;
fig. 2 is a graph comparing discharge curves of high-temperature molten salt batteries.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
A high-temperature molten salt battery having a functional layer according to a preferred embodiment of the present invention includes a functional layer with high oxygen ion conductivity between a solid electrolyte 1, as shown in fig. 1, and a molten salt electrolyte, not shown in fig. 1, integrated with the functional layer 2.
Example 1
Yttria stabilized zirconia powder having a particle size of 2 microns and a mass of about 1.5g was placed inside the mill of a tablet press.
The powder was slightly pressed to flatten the upper surface, and then cerium oxide powder having a particle size of 2 μm and a mass of about 0.5g was added.
And (3) putting the grinding tool filled with the powder into a tabletting machine, and tabletting at normal temperature. The pressure was first slowly increased to 25 tons, and after the pressure was maintained for 1 minute, the pressure was slowly released.
And putting the obtained sheet into a tube furnace for high-temperature sintering. The sintering step is as follows: heating to 800 deg.C at 5 deg.C/min in a tubular furnace, holding for 2 hr, heating to 1500 deg.C at the same heating rate, holding for 5 hr, and cooling to room temperature at 5 deg.C/min.
Example 2
The yttrium oxide stabilized zirconia sheet is prepared by a tape casting method. The specific method comprises the following steps: weighing 100g of yttria-stabilized zirconia powder, 40mL of ethanol and 110mL of butanone solvent, uniformly mixing, then adding 13g of polyvinyl butyral binder, plasticizer diethyl phthalate, polyethylene glycol and 3mL of triethanolamine dispersant, and uniformly ball-milling by using a ball mill to obtain electrolyte slurry. After the slurry is defoamed, the slurry is poured above a film belt of a casting machine, after a scraper is adjusted in height as required, the casting machine is started to form a uniform biscuit, and after the biscuit is dried, the operation is repeated for many times so as to achieve the required thickness.
Adding a zirconia-doped ceria functional layer on the yttria-stabilized zirconia film. The specific method comprises the following steps: and replacing the yttria-stabilized zirconia in the formula with zirconia-stabilized ceria, adding nano-graphite powder as a pore-forming agent, and preparing a zirconia-stabilized ceria functional layer on the upper surface of the dried biscuit according to the steps of the tape casting method. Wherein the mass ratio of zirconia to ceria was 1:9, and the mass of zirconia-doped ceria (functional layer) was 0.2 times the mass of yttria-stabilized zirconia (solid electrolyte layer).
The biscuit was cut into a circular biscuit having a diameter of 20mm, calcined at 1300 ℃ for 10 hours in an air atmosphere, and burned to remove components including a pore-forming agent except yttria-stabilized zirconia and zirconia-stabilized ceria.
Example 3
The yttria-stabilized zirconia powder was tabletted inside the grinding tool of a tabletting machine, with a particle size of 2 microns and a mass of about 1.5 g.
And (3) placing the wafer into a tube furnace, and sintering at high temperature. The sintering step is as follows: heating to 800 deg.C at 5 deg.C/min in a tubular furnace, holding for 2 hr, heating to 1500 deg.C at the same heating rate, holding for 5 hr, and cooling to room temperature at 5 deg.C/min.
And placing the sintered yttria-stabilized zirconia wafer in a Chemical Vapor Deposition (CVD) manner to be used as a substrate, and performing chemical vapor deposition for 8 hours by using butanol containing Ca and cerium as a precursor to obtain the calcium oxide doped ceria with the thickness of about 10 mu m.
Example 4
In Ce (OH)4Gadolinium nitrate is added into the water solution, then nitric acid is added, the pH is adjusted to 3-4, and the mixture is placed at 60 ℃ and stirred to obtain transparent sol.
Dropping the gel on the surface of a substrate by using yttria stabilized zirconia as the substrate, rotating the substrate for 20s at 2000 rpm by using a rotary coating instrument, heating the substrate to 600 ℃ at 0.5 ℃/min, preserving the heat for 2h, and cooling the substrate to room temperature at 2 ℃/min.
The above steps are repeated until the gadolinium oxide doped cerium oxide reaches the required thickness, for example, 10 μm to 100 μm determined by the range of the spin coater, and the coating thickness of the spin coater is generally less than hundred micrometers.
And (3) putting the substrate and the film on the substrate into a tube furnace, heating to 1400 ℃ at the speed of 2 ℃/min, preserving heat for 2 hours, and then cooling to room temperature to obtain the required functional layer.
Fig. 2 is a graph comparing the discharge curves of the high temperature molten salt battery using the functional layer prepared in example 1 and the high temperature molten salt battery not using the functional layer prepared in example 1 of the present invention. It can be seen that the high-temperature molten salt battery to which the functional layer prepared in example 1 was added had a higher discharge voltage and a longer operation time and more stable battery performance than the high-temperature molten salt battery to which the functional layer prepared in example 1 was not added under the same charge condition and discharge current.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (9)
1. A high-temperature molten salt battery with functional layers comprises a molten salt electrolyte and a solid electrolyte, and is characterized in that the high-temperature molten salt battery also comprises the functional layers, the functional layers are the electrolyte with high oxygen ion conduction and positioned between the solid electrolyte and the molten salt electrolyte, the functional layers comprise more than 75wt% of cerium oxide, the molten salt electrolyte is potassium carbonate, sodium carbonate, lithium carbonate, a mixed salt or eutectic salt of the potassium carbonate, the sodium carbonate and the lithium carbonate, and the solid electrolyte is yttria-stabilized zirconia, gadolinium oxide-doped ceria or scandium-stabilized zirconia.
2. A high temperature molten salt battery as in claim 1 wherein the functional layer is integral with the solid electrolyte.
3. A high temperature molten salt battery as in claim 1, wherein the functional layer further includes at least one dopant selected from the group consisting of zirconia, calcia and gadolinia.
4. A high temperature molten salt battery as claimed in claim 1, characterised in that the mass fraction of dopants in the functional layer is 1-25%.
5. A high temperature molten salt battery as in claim 1, wherein the mass ratio of the functional layer to the solid electrolyte is 0.2-0.45.
6. A high temperature molten salt battery as in claim 1 further including a positive electrode separated from the molten salt electrolyte by a solid electrolyte and a negative electrode disposed in the molten salt electrolyte.
7. A method of manufacturing a high temperature molten salt battery having a functional layer as claimed in any one of claims 1 to 6 wherein the functional layer is formed using at least one process selected from the group consisting of isostatic pressing, tape casting, chemical vapour deposition, electrochemical vapour deposition, electro-pulse deposition, sol-gel, sputtering, electron beam evaporation coating, physical vapour deposition and spray coating.
8. The production method according to claim 7, wherein the solid electrolyte is provided by a first powder and the functional layer is provided by a second powder, and the first powder and the second powder are brought into close contact with each other by tableting and sintering while forming a stable transition layer by dense sintering of the contact surface.
9. The method of claim 8, wherein the first powder has a particle size equal to that of the second powder.
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| US9325036B2 (en) * | 2010-04-19 | 2016-04-26 | Siemens Aktiengesellschaft | Molten salt-containing metal electrode for rechargeable oxide-ion battery cells operating below 800°C |
| US20130115528A1 (en) * | 2011-11-04 | 2013-05-09 | Chun Lu | Rechargeable anion battery cell using a molten salt electrolyte |
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| CN103825058B (en) * | 2014-02-28 | 2016-05-25 | 华中科技大学 | A kind of paste electrolyte and preparation method thereof for new type high temperature molten salt battery |
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