CN111995396A - Method for utilizing oxygen ion conductivity of magnesium modified sodium niobate ceramic - Google Patents
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Abstract
The invention discloses a method for utilizing the oxygen ion conductivity of magnesium modified sodium niobate ceramics, which is prepared by the traditional solid phase sintering process, and low-valent magnesium ions are utilized to replace niobium ions in sodium niobate so as to cause the material to generate oxygen vacancy defects, thereby inducing the oxygen ion conductivity. Since the radius of magnesium ions is larger than that of niobium ions, the gap r in the migration path of oxygen ions is increasedcTo facilitate the migration of oxygen ions, thereby reducing the activation temperature and obtaining the oxygen ion conductive ceramic with high conductivity at medium temperature (600 ℃) (sigma is 2.0 multiplied by 10)‑ 3S/cm). The sodium niobate-based perovskite ceramic provided by the invention shows good oxygen ion conductivity in a medium-temperature region, and is preparedThe method has the advantages of simple process, economy and reasonability, suitability for industrial production and wide application prospect in the field of new energy materials.
Description
Technical Field
The invention relates to the technical field of new energy materials, in particular to a method for utilizing the oxygen ion conductivity of magnesium modified sodium niobate ceramics.
Background
The fuel cell is not limited by Carnot cycle, so the energy conversion efficiency can reach 40-80%, and the fuel cell can uninterruptedly and directly convert the chemical energy in the fuel into electric energy, basically does not produce harmful products in the conversion process, and is a high-efficiency and clean energy conversion device. Solid Oxide Fuel Cell (SOFC) as third generation fuel cell following phosphate fuel cell and molten carbonate fuel cell, and it can use H2And hydrocarbons such as CO, gasoline, petroleum, natural gas and the like are used as fuel gas, so that the applicability of the fuel gas is greatly widened. And noble metal catalysts are not needed when the SOFC is used, so that the cost is reduced. Because of its all solid state structure, easy modularization equipment. The solid oxide fuel cell has wide application prospect (Xianxianni, summary of technical development of solid oxide fuel cell and application analysis [ J)]Electrical industry, 2019,3: 70-74.).
The SOFC is mainly composed of an anode, a solid electrolyte, a cathode and a bonding material 4 part. Among them, the solid electrolyte is the core unit of SOFC and is a key factor affecting the performance of solid oxide fuel cell. The traditional electrolyte material is Yttrium Stabilized Zirconia (YSZ), which still has good stability and high ionic conductivity under the reducing condition and is widely applied to SOFCs. However, it has a significant disadvantage of excessively high operating temperature (>1000 ℃), which often causes deformation and chemical reaction between interfaces among the electrolyte, electrodes, and bonding materials due to the difference in thermal expansion coefficients, thereby greatly reducing the service life of the SOFC (s. anirban, a. duta, An insulation on structure, reduction and ion dynamics of Sr-Sm co-processed carbon oxidation conductors: Effect of defect interaction [ J ]. Solid State Sciences,2018,86: 69-76), which severely limits the choice of materials for preparing the SOFC. Therefore, the development of the electrolyte material with medium-low temperature and high oxygen ion conductivity can not only reduce the manufacturing cost of the SOFC, but also broaden the application range of the SOFC.
NaNbO with perovskite structure3Is a typical lead-free antiferroelectric material, and the antiferroelectric energy storage performance of the material is widely researched in recent years. NaNbO3The ceramic has good structural stability, and a large number of oxygen ion vacancies can be induced and generated by doping A, B sites or doping A/B co-doping low-valence cations, so that the oxygen ion conductivity of the material is improved. In addition, the tolerance factor (0.9) is based on the perovskite structure<t<1.1) a plurality of elements can be selected for doping modification of A site and B site, and the perovskite structure and the electrical conductivity can be optimized.
The invention uses 2-valent Mg ions to replace NaNbO3The Nb ions at the B site of the alloy can form more oxygen vacancies under the condition of the same doping amount, thereby improving the oxygen ion conductivity of the alloy. On the other hand, Mg is cheaper than elements such as Ti, Sm, Gd, etc., and can further reduce the production cost of the electrolyte material.
Disclosure of Invention
The invention aims to solve the problems that: providing a method for utilizing the oxygen ion conductivity of magnesium modified sodium niobate ceramics, and obtaining fine particles and uniform particle size raw powder by adopting a solid-phase reaction method; and preparing the high-performance oxygen ion conductor by adopting a high-temperature sintering process.
The technical scheme provided by the invention for solving the problems is as follows: a method for utilizing the oxygen ion conductivity of magnesium modified sodium niobate ceramics comprises the following steps,
1) weighing a certain proportion of Na2CO3、Nb2O5And MgO for preparing NaNb1-xMgxO3-1.5xWherein x is 0.005-0.2;
2) putting the mixed powder into a ball milling tank for wet ball milling, drying, sieving and pressing into a blank for presintering;
3) grinding the pre-sintered blank, then ball-milling, drying and sieving again;
4) granulating the powder and pressing into a wafer by using a die;
5) sintering the wafer after removing the glue;
6) and carrying out test analysis on the sintered sample.
Preferably, the mass ratio of the powder, the ball milling balls and the ball milling medium in the wet ball milling in the step 2) and the step 3) is 1:0.8:2, the ball milling speed is 360r/min, the ball milling time is 4 hours, the drying temperature is 80 ℃, and the drying time is 6 hours.
Preferably, the pre-sintering process in the step 2) is that the temperature rising rate is 3 ℃/min, the pre-sintering temperature is 850 ℃, and the heat preservation time is 2 hours.
Preferably, the granulation process in the step 4) is that the mass ratio of the powder to the PVA solution is 1:0.05, the PVA solution concentration was 5 wt%.
Preferably, the sheet pressing forming conditions in the step 4) are as follows: maintaining the pressure at 300MPa for 5 min.
Preferably, the glue discharging process in the step 5): the heating rate is 1.5 ℃/min, the glue discharging temperature is 550 ℃, and the glue discharging time is 2 h.
Preferably, the sintering process in the step 5): the heating rate is 3 ℃/min, the sintering temperature is 1050-1200 ℃, and the sintering time is 2 h.
Compared with the prior art, the invention has the advantages that:
(1) replacement of NaNbO with Mg ions of valency 23The 5-valent Nb ions at the B site can form more oxygen vacancies and improve the oxygen ion conductivity under the condition of the same doping amount.
(2) And the radius of the magnesium ions is larger than that of the niobium ions, so that the clearance r in an oxygen ion migration path is increasedcThe method is favorable for the migration of oxygen ions, thereby further improving the conductivity of the oxygen ions of the sodium niobate ceramic.
(3) The pre-sintering process effectively decomposes carbonate in the raw materials, so that the powder is better combined in the sintering process, and a pure phase is conveniently obtained.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a graph of complex impedance of example 2 at 600 ℃ under different atmospheres.
Fig. 2 is an XRD pattern of sodium niobate ceramics with different magnesium doping amounts.
Detailed Description
The embodiments of the present invention will be described in detail with reference to the accompanying drawings and examples, so that how to implement the technical means for solving the technical problems and achieving the technical effects of the present invention can be fully understood and implemented.
Example 1:
10g of Na was taken2CO3、23.8217g Nb2O50.1901g of MgO is put into a ball milling tank, wet ball milling is carried out for 4h at the rotating speed of 360r/min, the powder liquid after ball milling is dried for 6h in a drying box at the temperature of 80 ℃, then a 200-mesh screen is sieved, and the powder is pressed into a green body to be kept at the temperature of 850 ℃ for 2 h. And grinding the pre-sintered blank, then ball-milling, drying and sieving again. Then, 5 wt% of PVA solution (the mass ratio of the powder to the PVA solution is 1:0.05) was added to the powder, the powder was continuously milled to be uniformly mixed, and then the powder was pressed into a wafer by a die. Heating to 550 ℃ at the heating rate of 1.5 ℃/min and preserving heat for 2h, then heating to 1150 ℃/min at the heating rate of 3 ℃/min and preserving heat for 2h, wherein the sintered sample has obvious size shrinkage. After the surface of the sample is ground flat, the sample is subjected to impedance test by a gold electrode by using an electrochemical workstation, and the test result shows that: the oxygen ion conductivity of the sample at 600 ℃ is 1.6 multiplied by 10-3S/cm。
Example 2:
10g of Na was taken2CO3、22.5679g Nb2O50.3802g of MgO is put into a ball milling tank, wet ball milling is carried out for 4h at the rotating speed of 360r/min, the powder liquid after ball milling is dried for 6h in a drying box at the temperature of 80 ℃, then a 200-mesh screen is sieved, and the powder is pressed into a green body to be kept at the temperature of 850 ℃ for 2 h. And grinding the pre-sintered blank, then ball-milling, drying and sieving again. Then, 5 wt% of PVA solution (the mass ratio of the powder to the PVA solution is 1:0.05) was added to the powder, the powder was continuously milled to be uniformly mixed, and then the powder was pressed into a wafer by a die. Heating to 550 deg.C at a heating rate of 1.5 deg.C/min and holding for 2 hr, and then heating at 3 deg.C/min is heated to 1100 ℃/min at the heating rate and is kept for 2h, and the sintered sample has obvious size shrinkage. After the surface of the sample is ground flat, the sample is subjected to impedance test by a gold electrode by using an electrochemical workstation, and the test result shows that: the oxygen ion conductivity of the sample at 600 ℃ is 2 multiplied by 10-3S/cm。
Example 3:
10g of Na was taken2CO3、21.3142g Nb2O5And 0.5703g of MgO are put into a ball milling tank, wet ball milling is carried out for 4h at the rotating speed of 360r/min, the powder liquid after ball milling is dried for 6h in a drying box at the temperature of 80 ℃, then the powder liquid is sieved by a 200-mesh screen, and the powder is pressed into a blank body and is kept warm for 2h at the temperature of 850 ℃. And grinding the pre-sintered blank, then ball-milling, drying and sieving again. Then, 5 wt% of PVA solution (the mass ratio of the powder to the PVA solution is 1:0.05) was added to the powder, the powder was continuously milled to be uniformly mixed, and then the powder was pressed into a wafer by a die. Heating to 550 ℃ at the heating rate of 1.5 ℃/min and preserving heat for 2h, then heating to 1090 ℃/min at the heating rate of 3 ℃/min and preserving heat for 2h, wherein the sintered sample has obvious size shrinkage. After the surface of the sample is ground flat, the sample is subjected to impedance test by a gold electrode by using an electrochemical workstation, and the test result shows that: the oxygen ion conductivity of the sample at 600 ℃ is 1.2 multiplied by 10-3S/cm。
The foregoing is merely illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the claims. The present invention is not limited to the above embodiments, and the specific structure thereof is allowed to vary. All changes which come within the scope of the invention as defined by the independent claims are intended to be embraced therein.
Claims (7)
1. A method for utilizing the oxygen ion conductivity of magnesium modified sodium niobate ceramics is characterized in that: the method comprises the following steps of,
1) weighing a certain proportion of Na2CO3、Nb2O5And MgO for preparing NaNb1-xMgxO3-1.5xWherein x is 0.005-0.2;
2) putting the mixed powder into a ball milling tank for wet ball milling, drying, sieving and pressing into a blank for presintering;
3) grinding the pre-sintered blank, then ball-milling, drying and sieving again;
4) granulating the powder and pressing into a wafer by using a die;
5) sintering the wafer after removing the glue;
6) and carrying out test analysis on the sintered sample.
2. The method for utilizing the oxygen ion conductivity of the magnesium-modified sodium niobate ceramic according to claim 1, wherein the method comprises the following steps: the mass ratio of the powder, the ball milling balls and the ball milling medium in the wet ball milling in the step 2) and the step 3) is 1:0.8:2, the ball milling speed is 360r/min, the ball milling time is 4 hours, the drying temperature is 80 ℃, and the drying time is 6 hours.
3. The method for utilizing the oxygen ion conductivity of the magnesium-modified sodium niobate ceramic according to claim 1, wherein the method comprises the following steps: the pre-sintering process in the step 2) is that the heating rate is 3 ℃/min, the pre-sintering temperature is 850 ℃, and the heat preservation time is 2 hours.
4. The method for utilizing the oxygen ion conductivity of the magnesium-modified sodium niobate ceramic according to claim 1, wherein the method comprises the following steps: the granulation process in the step 4) is that the mass ratio of powder to PVA solution is 1:0.05, the PVA solution concentration was 5 wt%.
5. The method for utilizing the oxygen ion conductivity of the magnesium-modified sodium niobate ceramic according to claim 1, wherein the method comprises the following steps: the sheet pressing molding conditions in the step 4) are as follows: maintaining the pressure at 300MPa for 5 min.
6. The method for utilizing the oxygen ion conductivity of the magnesium-modified sodium niobate ceramic according to claim 1, wherein the method comprises the following steps: the glue discharging process in the step 5): the heating rate is 1.5 ℃/min, the glue discharging temperature is 550 ℃, and the glue discharging time is 2 h.
7. The method for utilizing the oxygen ion conductivity of the magnesium-modified sodium niobate ceramic according to claim 1, wherein the method comprises the following steps: the sintering process in the step 5): the heating rate is 3 ℃/min, the sintering temperature is 1050-1200 ℃, and the sintering time is 2 h.
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