CN112830778A - Method for rapidly sintering solid electrolyte, dense solid electrolyte obtained therefrom and application thereof - Google Patents
Method for rapidly sintering solid electrolyte, dense solid electrolyte obtained therefrom and application thereof Download PDFInfo
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Abstract
本发明涉及一种快速烧结固态电解质的方法，其包括将固态电解质纳米粉末压制成片材；提供具有彼此间隔开的两片碳纸的快速烧结装置，将片材夹持在碳纸之间，给碳纸通电使碳纸在电流作用下产生焦耳热以通过调节碳纸的温度进行烧结，得到致密固态电解质。本发明还提供一种根据上述方法得到的致密固态电解质。本发明又提供一种上述致密固态电解质在熔盐电池中的应用。根据本发明的快速烧结固态电解质的方法，通过廉价的碳纸在电流作用下产生焦耳热，短时间内大量聚集的焦耳热可以通过热辐射和热传导的方式对固态电解质片材进行快速烧结，加快固态电解质的高通量筛选的进度。
The invention relates to a method for rapidly sintering solid electrolyte, which comprises pressing solid electrolyte nano powder into sheets; providing a rapid sintering device with two sheets of carbon paper spaced apart from each other, clamping the sheets between the carbon papers, The carbon paper is energized so that the carbon paper generates Joule heat under the action of the electric current, so that the temperature of the carbon paper is adjusted for sintering, and a dense solid electrolyte is obtained. The present invention also provides a dense solid electrolyte obtained according to the above method. The present invention further provides an application of the above-mentioned dense solid electrolyte in a molten salt battery. According to the method for rapid sintering of solid electrolyte of the present invention, Joule heat is generated by cheap carbon paper under the action of electric current, and a large amount of Joule heat accumulated in a short period of time can rapidly sinter the solid electrolyte sheet by means of thermal radiation and heat conduction, thereby accelerating the sintering of solid electrolyte sheets. Progress in high-throughput screening of solid-state electrolytes.
Description
Technical Field
The present invention relates to solid electrolytes, and more particularly to a method of rapidly sintering a solid electrolyte and the resulting dense solid electrolyte and its applications.
Background
The solid electrolyte is typically used in a fuel cell, and a combustible gas can be directly converted into electric energy at a high temperature, so that the conversion rate is far higher than that of conventional thermal power generation, and the solid electrolyte is environmentally friendly. With the development of the computer level, the computer simulation is far beyond the experimental progress, and accelerating the experimental progress of the solid electrolyte is an important task of current scientific research work.
The conventional process of sintering the solid electrolyte in an electric furnace takes several hours or tens of hours, the spark plasma sintering equipment is expensive, the flash sintering generally needs expensive Pt electrodes, and the flash sintering condition depends on the electrical properties of the material, so that the flash sintering has no universality and limits the practicability of the flash sintering equipment for high-flux treatment when the material performance is unknown. The photon sintering temperature is typically not as high as the temperature at which the solid electrolyte is sintered. The rapid annealing furnace can only provide sintering temperature as high as 1200 ℃, commercial equipment is expensive, high-end rapid firing equipment is difficult to prepare for a common laboratory, and the conventional electric furnace has long sintering service time.
In conclusion, it is necessary to develop a simple and fast sintering method, and some fast sintering devices exist at present, but the methods cannot be popularized and used in solid electrolyte sintering due to high price or insufficient temperature.
Disclosure of Invention
In order to solve the problems that the sintering temperature of the solid electrolyte in the prior art is insufficient or cannot be popularized, the invention provides a method for rapidly sintering the solid electrolyte, a compact solid electrolyte obtained by the method and application of the compact solid electrolyte.
The invention provides a method for rapidly sintering a solid electrolyte, which comprises the following steps: s1, pressing the solid electrolyte nano powder into a sheet; and S2, providing a rapid sintering device with two carbon papers spaced from each other, clamping the sheets between the carbon papers, electrifying the carbon papers to enable the carbon papers to generate Joule heat under the action of current so as to sinter by adjusting the temperature of the carbon papers, and obtaining the dense solid electrolyte.
Preferably, the solid electrolyte is yttria stabilised zirconia or ceria. In a preferred embodiment, the solid electrolyte is 8 YSZ.
Preferably, in step S1, the solid electrolyte nanopowder is placed in a tabletting mold and slowly pressurized to 400MPa to 600MPa to obtain a sheet. In a preferred embodiment, 0.09g of 8YSZ nanopowder is placed in a tabletting mold with a diameter of 5mm, slowly pressurized to 500MPa and left to stand for about 30 seconds to obtain a sheet. It should be understood that the tableting operation should use as much pressure as possible within the safe use range of the tableting die to promote sufficient contact of the solid electrolyte nanopowder to form the sheet.
Preferably, the thickness of the sheet is within 2 mm.
Preferably, the rapid sintering device further comprises an outer cover, a support plate, electrodes and a power supply, wherein the outer cover provides a closed space, the support plate is fixedly installed in the closed space, two ends of the carbon paper are respectively and fixedly installed between the electrodes and carried on the support plate, and the power supply is connected with the electrodes through cables outside the outer cover to supply current to the carbon paper.
Preferably, the power supply is a low voltage dc power supply.
Preferably, the outer envelope is a quartz glass envelope and the support plate is a quartz plate. It is understood that the quartz material of the quartz glass cover and the quartz plate has good heat resistance and high light transmittance, and a large amount of heat radiation is not absorbed, which is advantageous for structural stability and is not damaged by high temperature.
Preferably, the diameter of the sheet is less than 2/3 the width of the carbon paper to prevent the sheet from being heated unevenly.
Preferably, the temperature of the carbon paper is adjusted to be between 2/3 f, the melting point of the solid electrolyte, and the melting point, ensuring rapid sintering while the sheet remains massive.
Preferably, the carbon paper is sintered by adjusting the temperature to 1786-2680 ℃. It will be appreciated that the temperature range of 1786 deg.C to 2680 deg.C lies between 2/3 deg.C and the melting point of pure zirconia, ensuring rapid sintering while the sheet remains massive. In a preferred embodiment, the temperature of the carbon paper is adjusted to 2400 ℃ for 25 seconds, and then the carbon paper is sintered for 30 seconds while maintaining the temperature of 2400 ℃ to obtain a dense solid electrolyte.
The invention also provides a dense solid electrolyte obtained according to the above method.
The invention also provides an application of the compact solid electrolyte in a molten salt battery.
According to the method for rapidly sintering the solid electrolyte, the cheap carbon paper generates the Joule heat under the action of the current, the Joule heat which is gathered in a large amount in a short time can rapidly sinter the solid electrolyte sheet in a heat radiation and heat conduction mode, and the progress of high-flux screening of the solid electrolyte is accelerated. In conclusion, according to the method for rapidly sintering the solid electrolyte, the rapid sintering device for sintering is low in price, simple to implement, capable of being used without strict training, high in sintering temperature provided by the carbon paper, capable of meeting the sintering requirement of the solid electrolyte, short in time, fast in speed, capable of finishing the whole sintering process within one minute, for example, the average temperature rise rate is about 96 ℃ per second, and the method for rapidly sintering the solid electrolyte greatly improves the sintering efficiency of the solid electrolyte and has a good application prospect.
Drawings
Fig. 1 is a schematic structural view of a rapid sintering apparatus used in a method of rapidly sintering a solid electrolyte according to a preferred embodiment of the present invention;
fig. 2 is an SEM image of a dense solid electrolyte obtained by a method of rapidly sintering a solid electrolyte according to a preferred embodiment of the present invention;
fig. 3 is a photograph of a dense solid electrolyte obtained by a method of rapidly sintering a solid electrolyte according to a preferred embodiment of the present invention;
fig. 4 is a graph of impedance test data of a dense solid electrolyte obtained by a method of rapidly sintering a solid electrolyte according to a preferred embodiment of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
8YSZ nanopowder with a mass of 0.09g was put into a tabletting mold with a diameter of 5mm, slowly pressurized to 500MPa, and left to stand for about 30 seconds to obtain a sheet 6 with a thickness of 1 mm.
There is provided a rapid sintering apparatus as shown in fig. 1, which comprises a quartz glass cover 1, a quartz plate 2, carbon paper 3, electrodes 4 and a power supply 5, wherein the quartz glass cover 1 provides a closed space, the quartz plate 2 is fixedly mounted in the closed space, two ends of two carbon papers 3 spaced apart from each other are respectively fixedly mounted between the electrodes 4 and carried on the quartz plate 2, and the power supply 5 is connected with the electrodes 4 through cables outside the quartz glass cover 1 to supply current to the carbon paper 3.
The sheet 6 was sandwiched between the carbon papers 3, the power supply 5 was turned on, and the current was gradually increased to a temperature of about 2400 ℃ for 25 seconds, and the carbon paper was sintered at 2400 ℃ for 30 seconds to obtain a dense solid electrolyte.
As shown in fig. 2, the sintered solid electrolyte obtained by the method of rapidly sintering a solid electrolyte according to the present invention has a dense structure. As shown in FIG. 3, the method of rapidly sintering a solid electrolyte according to the present invention results in a dense solid electrolyteThe material is not broken due to too large a temperature rise and fall rate of sintering. As shown in fig. 4, the method of rapidly sintering a solid electrolyte according to the present invention resulted in a dense solid electrolyte having a resistance of about 1.8 ohms (impedance complex Z (ω) ═ Z)Re-jZImThe abscissa is a real part, the ordinate is an imaginary part, and the intersection of the data fitting and the abscissa is about 1.8), and can be used in a molten salt battery.
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 (10)
1. A method of rapidly sintering a solid electrolyte, the method comprising the steps of:
s1, pressing the solid electrolyte nano powder into a sheet;
and S2, providing a rapid sintering device with two carbon papers spaced from each other, clamping the sheets between the carbon papers, electrifying the carbon papers to enable the carbon papers to generate Joule heat under the action of current so as to sinter by adjusting the temperature of the carbon papers, and obtaining the dense solid electrolyte.
2. The method of claim 1, wherein the solid electrolyte is yttria stabilized zirconia or ceria.
3. The method as claimed in claim 1, wherein the solid electrolyte nanopowder is placed in a tabletting mold and slowly pressurized to 400 to 600MPa to obtain a sheet.
4. The method of claim 1, wherein the sheet has a thickness of within 2 mm.
5. The method of claim 1, wherein the rapid sintering device further comprises a housing, a support plate, electrodes and a power supply, wherein the housing provides a closed space, the support plate is fixedly installed in the closed space, two ends of the carbon paper are respectively and fixedly installed between the electrodes and supported on the support plate, and the power supply is connected with the electrodes through cables outside the housing to supply current to the carbon paper.
6. The method of claim 5, wherein the housing is a quartz glass housing and the support plate is a quartz plate.
7. The method of claim 1, wherein the diameter of the sheet is less than 2/3 the width of the carbon paper to prevent uneven heating of the sheet.
8. The method of claim 1, wherein the temperature of the carbon paper is adjusted to be between 2/3 f the melting point of the solid electrolyte and the melting point to ensure rapid sintering while the sheet remains massive.
9. A dense solid electrolyte obtained according to the method of any one of claims 1-8.
10. Use of the dense solid-state electrolyte of claim 9 in a molten salt battery.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113247962A (en) * | 2021-06-26 | 2021-08-13 | 深圳中科精研科技有限公司 | Battery anode material and method for rapidly synthesizing battery anode material |
| CN114516752A (en) * | 2021-12-23 | 2022-05-20 | 内蒙古工业大学 | Porous calcium silicate ceramic and ultra-fast preparation method thereof |
| CN114907100A (en) * | 2022-05-19 | 2022-08-16 | 中国科学院长春应用化学研究所 | An Instantaneous Synthesis Process for a Ba-based Proton Conductor Electrolyte |
| CN116040628A (en) * | 2022-12-23 | 2023-05-02 | 中国人民解放军军事科学院防化研究院 | Method for rapidly preparing highly graphitized porous carbon |
| CN118724582A (en) * | 2024-06-06 | 2024-10-01 | 昆明理工大学 | A method for rapidly densifying solid oxide electrolyte for lithium-ion batteries |
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| US20030027033A1 (en) * | 2001-06-29 | 2003-02-06 | Seabaugh Matthew M. | Nano-composite electrodes and method of making the same |
| WO2014003591A1 (en) * | 2012-06-29 | 2014-01-03 | Lneg - Laboratório Nacional De Energia E Geologia | Process for manufacturing a solid oxide fuel cell electrolyte using microwave sintering |
| WO2020236767A1 (en) * | 2019-05-17 | 2020-11-26 | University Of Maryland, College Park | High temperature sintering systems and methods |
| CN112153764A (en) * | 2020-09-28 | 2020-12-29 | 中国农业大学 | Rapid heating method for preparing ceramic material |
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2021
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| US20030027033A1 (en) * | 2001-06-29 | 2003-02-06 | Seabaugh Matthew M. | Nano-composite electrodes and method of making the same |
| WO2014003591A1 (en) * | 2012-06-29 | 2014-01-03 | Lneg - Laboratório Nacional De Energia E Geologia | Process for manufacturing a solid oxide fuel cell electrolyte using microwave sintering |
| WO2020236767A1 (en) * | 2019-05-17 | 2020-11-26 | University Of Maryland, College Park | High temperature sintering systems and methods |
| CN112153764A (en) * | 2020-09-28 | 2020-12-29 | 中国农业大学 | Rapid heating method for preparing ceramic material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113247962A (en) * | 2021-06-26 | 2021-08-13 | 深圳中科精研科技有限公司 | Battery anode material and method for rapidly synthesizing battery anode material |
| CN114516752A (en) * | 2021-12-23 | 2022-05-20 | 内蒙古工业大学 | Porous calcium silicate ceramic and ultra-fast preparation method thereof |
| CN114907100A (en) * | 2022-05-19 | 2022-08-16 | 中国科学院长春应用化学研究所 | An Instantaneous Synthesis Process for a Ba-based Proton Conductor Electrolyte |
| CN116040628A (en) * | 2022-12-23 | 2023-05-02 | 中国人民解放军军事科学院防化研究院 | Method for rapidly preparing highly graphitized porous carbon |
| CN118724582A (en) * | 2024-06-06 | 2024-10-01 | 昆明理工大学 | A method for rapidly densifying solid oxide electrolyte for lithium-ion batteries |
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Application publication date: 20210525 |