CN110078503B - Method for low-temperature sintering of 8YSZ electrolyte - Google Patents

Method for low-temperature sintering of 8YSZ electrolyte Download PDF

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CN110078503B
CN110078503B CN201910413879.5A CN201910413879A CN110078503B CN 110078503 B CN110078503 B CN 110078503B CN 201910413879 A CN201910413879 A CN 201910413879A CN 110078503 B CN110078503 B CN 110078503B
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8ysz
electrolyte
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nitrate solution
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林枞
李含影
黄雨铭
吴啸
周世勇
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Fuzhou University
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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    • 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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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The invention discloses a method for sintering 8YSZ electrolyte at low temperature, which comprises the steps of firstly preparing Fe2O3The doped 8YSZ powder is subjected to cold sintering by introducing yttrium nitrate solution, and then is sintered at 1000-1100 ℃, so that the compact 8YSZ electrolyte with good stability is obtained, and the electrolyte has good conductivity. The method has the advantages of simple process steps, good repeatability and easy operation, and is mainly used for preparing the solid oxide fuel cell.

Description

Method for low-temperature sintering of 8YSZ electrolyte
Technical Field
The invention belongs to the field of solid oxide fuel cells, and particularly relates to a method for sintering 8YSZ electrolyte at low temperature.
Background
8YSZ is currently the most successful electrolyte material for SOFCs. 8YSZ has higher ionic conductivity in a wider oxygen partial pressure range, good chemical stability and high mechanical strength, and is a commonly used electrolyte material in SOFC. In addition, the ZrO2 solid electrolyte ceramic has the advantages of good mechanical property, excellent oxidation resistance and corrosion resistance, no reaction with electrode materials and the like, so that the ZrO2 solid electrolyte ceramic becomes a preferred material for manufacturing oxygen sensors, solid oxide fuel cells and the like. The sintering temperature of 8YSZ electrolyte is usually higher than 1400 ℃, and the grain size after sintering is large, which is not favorable for the thermal stability. It has become a hot point of research to obtain a dense 8YSZ electrolyte at a lower sintering temperature.
The cold sintering is a novel sintering process for obtaining compact ceramics at an extremely low temperature, a temporary liquid environment is needed with the help of external pressure of 50-500 MPa of cold sintering, and a proper liquid medium can wet a particle interface to dissolve the edge of particles and promote particle rearrangement, so that the density of a ceramic block is improved. Therefore, the sintering temperature of the ceramic is expected to be greatly reduced by the cold sintering technology. Guo et al used a water-mediated cold firing process that reduced the sintering temperature of 8YSZ to 1200 c, but produced a small amount of monoclinic phase. In addition, the addition of a sintering aid is also an effective method for reducing the sintering temperature. By addition of Fe2O3The sintering temperature can be reduced to 1200-1300 ℃ by the additives. The invention adopts yttrium nitrate solution as a cold burning medium and dopes Fe2O3And the 8YSZ electrolyte is densely sintered at the temperature of below 1100 ℃.
Disclosure of Invention
In order to reduce the sintering temperature of the 8YSZ electrolyte and improve the stability of the electrolyte, the invention provides a method for sintering the 8YSZ electrolyte at low temperature, which utilizes metal oxide as a sintering aid, and simultaneously introduces yttrium nitrate solution to carry out cold sintering auxiliary sintering in the sintering process, so that 8YSZ keeps stable cubic phase, and monoclinic phase is avoided, thereby obtaining the 8YSZ electrolyte with better stability and more compactness at lower sintering temperature.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a method of low temperature sintering of 8YSZ electrolyte comprising the steps of:
(1) mixing 8YSZ powder with particle diameter of 20-100nm and Fe2O3And adding the powder into a ball milling tank, adding a ball milling medium into the mixture, performing rapid ball milling for 2 hours, drying the mixture after the ball milling is finished, and then putting the mixture into a mortar for grinding and sieving.
(2) To Fe2O3Adding 8YSZ nano-powder into nitreAnd (3) fully and uniformly grinding the yttrium acid solution (with the concentration of 1-3 mol/L) in a mortar to obtain an electrolyte raw material, and putting the raw material powder into a grinding tool for flattening.
(3) And (3) applying pressure of 200-400 MPa at the temperature of 100-150 ℃ for pressing and forming, and maintaining the pressure for 20-40 minutes to obtain an electrolyte green body.
(4) And (3) placing the electrolyte green body in a muffle furnace, and sintering at 1000-1100 ℃ for 1-4 h to obtain the compact 8YSZ electrolyte.
In the above step (1), Fe2O3The mass fraction of the powder is 2-8%.
In the step (2), the weight of the yttrium nitrate solution added is Fe2O310-30% of the weight of the doped 8YSZ nano powder.
Has the advantages that: the invention adopts the technical scheme that Fe is used for preparing the iron-based alloy2O3Doping 8YSZ and introducing Y during sintering3 +8YSZ electrolyte with high density can be obtained, and the prepared electrolyte has stable cubic phase and higher conductivity; the 8YSZ electrolyte prepared by the method not only effectively reduces the sintering temperature to a large extent, solves the problem of large grain size caused by high sintering temperature, but also can improve the stability of 8YSZ, broadens the sintering temperature range of 8YSZ, improves the flexibility of the production process, and lays theoretical and practical foundation for the industrial production of solid oxide fuel cells.
Drawings
FIG. 1 is an XRD pattern of a sample of 8YSZ electrolyte obtained from example 3;
FIG. 2 is an SEM image of an 8YSZ electrolyte sample obtained in example 3;
fig. 3 is a conductivity curve of the 8YSZ electrolyte sample obtained in example 3.
Detailed Description
The invention will be further elucidated with reference to the drawings and the detailed description:
example 1
A method of low temperature sintering of 8YSZ electrolyte comprising the steps of:
(1) having a particle diameter of 20 nm8YSZ powder and Fe2O3Adding the powder into a ball milling tank, adding a ball milling medium into the mixture, performing rapid ball milling for 2 hours, drying the mixture after the ball milling is finished, and then putting the mixture into a mortar for grinding and sieving; fe as described above2O3The mass fraction of the powder is 4%.
(2) Fe to step (1)2O3Adding 8YSZ doped nano powder into yttrium nitrate solution (the solubility is 1 mol/L) accounting for 10% of the weight of the nano powder, fully and uniformly grinding in a mortar to obtain electrolyte raw material, and putting the raw material powder into a grinding tool to flatten the raw material powder under 50 MPa.
(3) And (3) applying 300 MPa pressure at the temperature of 100 ℃ for pressing and forming, and keeping the pressure for 20 minutes to obtain an electrolyte green body.
(4) Sintering the electrolyte green body in a muffle furnace at 1000 ℃ for 3 h to obtain 8YSZ electrolyte with the density of 91.2%;
(5) coating silver paste on two sides of the electrolyte, connecting with silver wires, testing the conductivity at a certain temperature by using an electrochemical workstation, and reaching 0.009S-cm at 800 deg.C-1。
Example 2
A method of low temperature sintering of 8YSZ electrolyte comprising the steps of:
(1) mixing 8YSZ powder with particle diameter of 50 nm and Fe2O3Adding the powder into a ball milling tank, adding a ball milling medium into the mixture, performing rapid ball milling for 2 hours, drying the mixture after the ball milling is finished, and then putting the mixture into a mortar for grinding and sieving; fe as described above2O3The mass fraction of the powder is 8%.
(2) Fe to step (1)2O3Adding the doped 8YSZ nano powder into 20% yttrium nitrate solution (the solubility is 2 mol/L) of the weight of the nano powder, fully and uniformly grinding the mixture in a mortar to obtain an electrolyte raw material, and putting the raw material powder into a grinding tool to flatten the raw material powder under 50 MPa.
(3) And (3) applying 200 MPa pressure at the temperature of 120 ℃ for pressing and forming, and keeping the pressure for 30 minutes to obtain an electrolyte green body.
(4) And (3) sintering the electrolyte green body in a muffle furnace at 1050 ℃ for 1 h to obtain the 8YSZ electrolyte with the density of 92.3%.
(5) Coating silver paste on two sides of the electrolyte, connecting with silver wires, testing the conductivity at a certain temperature by using an electrochemical workstation, and reaching 0.012S-cm at 800 deg.C-1。
Example 3
A method of low temperature sintering of 8YSZ electrolyte comprising the steps of:
(1) mixing 8YSZ powder with particle diameter of 100nm and Fe2O3Adding the powder into a ball milling tank, adding a ball milling medium into the mixture, performing rapid ball milling for 2 hours, drying the mixture after the ball milling is finished, and then putting the mixture into a mortar for grinding and sieving; fe as described above2O3The mass fraction of the powder is 2%.
(2) Fe to step (1)2O3Adding a yttrium nitrate solution (the solubility is 3 mol/L) accounting for 30% of the weight of the doped 8YSZ nano powder into the nano powder, fully and uniformly grinding the mixture in a mortar to obtain an electrolyte raw material, and putting the raw material powder into a grinding tool to flatten the raw material powder under 50 MPa.
(3) And (3) applying 350 MPa pressure at the temperature of 150 ℃ for pressing and forming, and keeping the pressure for 40 minutes to obtain an electrolyte green body.
(4) And (3) sintering the electrolyte green body in a muffle furnace at 1100 ℃ for 4 h to obtain the 8YSZ electrolyte with the density of 95.5%.
(5) Coating silver paste on two sides of the electrolyte, connecting with silver wires, testing the conductivity at a certain temperature by using an electrochemical workstation, and reaching 0.016S-cm at 800 deg.C-1。
The XRD patterns, SEM patterns, and conductivity curves of the 8YSZ sample obtained in example 3 are shown in fig. 1-3. Fig. 1 shows that the resulting 8YSZ electrolyte is a cubic phase structure with little hetero-phase present; fig. 2 shows the surface SEM of the ceramic wafer obtained after sintering, and it can be seen that the sample is dense, the grain size is fine (< 300 nm) and is uniformly distributed, and the shape is close to a cubic structure with high symmetry; fig. 3 shows that the sample has better conductivity.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (1)

1. A method for low-temperature sintering of 8YSZ electrolyte is characterized in that: metal oxide is used as a sintering aid, and meanwhile, yttrium nitrate solution is introduced in the sintering process to carry out cold sintering auxiliary sintering, so that 8YSZ keeps stable cubic phase, monoclinic phase is avoided, and a compact 8YSZ electrolyte with good stability is obtained at low sintering temperature;
the preparation method comprises the following steps:
(1) mixing 8YSZ powder with Fe2O3Adding the powder into a ball milling tank, adding a ball milling medium into the mixture for rapid ball milling for 2 hours, drying the mixture, and then putting the dried mixture into a mortar for grinding and sieving;
(2) fe obtained in step (1)2O3Adding the doped 8YSZ nano powder into yttrium nitrate solution, placing the yttrium nitrate solution into a mortar, fully and uniformly grinding the yttrium nitrate solution to obtain electrolyte raw material, and placing the raw material powder into a die to be pressed and pressed.
(3) Pressing and forming the raw material powder obtained in the step (2), and maintaining the pressure for 20-40 min to obtain an electrolyte green body;
(4) sintering the electrolyte green compact obtained in the step (3) to obtain a compact 8YSZ electrolyte;
the pressure of the pressing forming in the step (3) is 200-400 MPa, and the pressing temperature is 100-150 ℃; in the step (4), the sintering temperature is 1000-1100 ℃, and the time is 1-4 h; fe in step (1)2O3The mass of the powder is 8YSZ powder and Fe2O32-8% of the total mass of the powder; in the step (1), the particle size of 8YSZ powder is 20-100 nm; in the step (2), the concentration of the yttrium nitrate solution is 1-3 mol/L; the mass of the yttrium nitrate solution added in the step (2) is Fe2O3The mass of the doped 8YSZ nano powder is 10-30%.
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WO2011056418A2 (en) * 2009-10-28 2011-05-12 University Of Florida Research Foundation, Inc. Fabrication of dual structure ceramics by a single step process
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WO2011056418A2 (en) * 2009-10-28 2011-05-12 University Of Florida Research Foundation, Inc. Fabrication of dual structure ceramics by a single step process
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"Fe-doped YSZ electrolyte for the fabrication of metal supported-SOFC by co-sintering";Pradnyesh Satardekar et al.;《Ceramics International》;20150423;第41卷;第4157-4164页 *
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