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CN114113230A - Method for measuring proton surface exchange rate of material by applying conductance relaxation - Google Patents

Method for measuring proton surface exchange rate of material by applying conductance relaxation Download PDF

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CN114113230A
CN114113230A CN202111341736.1A CN202111341736A CN114113230A CN 114113230 A CN114113230 A CN 114113230A CN 202111341736 A CN202111341736 A CN 202111341736A CN 114113230 A CN114113230 A CN 114113230A
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sample
conductivity
exchange rate
proton
surface exchange
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洪涛
任柯柯
黄容
潘翔
程继贵
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Hefei University of Technology
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    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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Abstract

The invention discloses a method for measuring the proton surface exchange rate of a material by applying conductance relaxation, which is used for directly testing BaCo0.4Fe0.4Zr0.1Y0.1O3‑δWhen the electric conductivity of the mixed conductor of protons and electrons is in the atmosphere with different water vapor contents, the water content in the air is changed at a certain fixed temperature, and the change process of the corresponding electric conductivity along with the time is recorded, so that the corresponding proton surface exchange rate is calculated. The test method has the characteristics of convenience in sample preparation, strong operability, simple steps, stable result, small influence of external factors, capability of directly obtaining the proton exchange rate through calculation and the like.

Description

Method for measuring proton surface exchange rate of material by applying conductance relaxation
Technical Field
The invention relates to the field of proton ceramic fuel cells, in particular to a method for measuring the exchange rate of a proton surface of a material by applying conductance relaxation.
Background
In Solid Oxide Fuel Cell (SOFC) cathodes, mixed ion/electron conductor electrodes are of great interest because of their ability to increase the air/electrode/electrolyte three-phase interface and to enhance the cathode reaction rate. The proton conducting fuel cell in the middle temperature range (400-700 ℃) has the following advantages: (1) proton conducting electrolytes possess higher electrical conductivity than oxygen ion conductor SOFCs; (2) water is generated at the cathode to avoid diluting the fuel. The catalytic activity of the cathode decreases with decreasing temperature, which is often an important factor in rate limiting, so the cathode material must possess a high hole concentration and high electrical conductivity. However, it has not been easy to quantify the proton conductivity of the oxygen vacancy/proton/hole mixed conducting oxide so far.
The formation concentration and the formation rate of protons in the cathode material are key indexes influencing the performance of the cathode material, and the accurate measurement of the surface exchange rate of the protons in the cathode material has important referential significance for evaluating the application potential of the cathode material on a battery and further improving the cathode material. However, it is very difficult to measure the proton concentration and the proton formation rate in the material, and even by using secondary ion mass spectrometry, the accurate concentration of the proton defect in the material cannot be accurately detected. Meanwhile, the generation of protons inside the cathode material must depend on the presence of water in the external environment, which also greatly limits the application of various measurement means.
Before Daniel Poetzsch and R.Zohourian et al, thermogravimetric relaxation was mainly used, the proton defect concentration was determined by measuring the change of the mass of the sample after the change of the water vapor content in the ambient atmosphere, the proton concentration was determined by the reaction absorption of protons, and the proton conductivity range was given from the proton diffusivity. However, the thermogravimetric relaxation method has certain influence on the sample amount, the atmosphere flow rate, the filling mode and the like, and many chemical defect reactions need to be analyzed, so that certain errors are eliminated by utilizing various assumptions. Therefore, it is urgently needed to develop a method for simply and efficiently measuring the proton exchange rate of the cathode, which is simple and easy to implement, has little influence of external factors, and can more accurately represent the proton exchange rate.
Disclosure of Invention
The invention aims to provide a method for measuring the proton surface exchange rate of a material by applying conductance relaxation, which can automatically realize the complete separation of oil, slag and water and greatly reduce the labor intensity of workers.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for measuring the proton surface exchange rate of a material by using conductance relaxation, which comprises the following steps:
(1) testing the conductivity of the sample at the temperature of 550-700 ℃ by adopting a direct-current four-terminal method;
(2) regulating the content of water vapor in gas entering a sample through a heater, gradually reducing and stabilizing the conductivity under the humid atmosphere with the water pressure of 5% -10%, and then converting the conductivity into a dry atmosphere, wherein the conductivity can be gradually increased and reaches an equilibrium state;
(3) placing the sample at 550-700 ℃, instantly changing the content of water vapor in the gas introduced into the sample after the conductivity of the sample is stable, continuously recording the change process of the conductivity sigma of the sample along with the time, and ending the measurement process after the conductivity gradually reaches the stability;
(4) changing the test temperature of the sample, and measuring the change process of the conductivity of the sample after the water vapor content in the gas is changed at different temperatures within the range of 550-700 ℃;
(5) normalizing the change curve of the conductivity, and then obtaining the normalized change curve of the conductivity by the formula NC (t) ═ 1-expAtFitting to obtain an index A, the surface exchange rate K of the sample δ1/2AD, where D is the thickness of the sample.
Preferably, in the step (1), the sample comprises BaCo0.4Fe0.4Zr0.1Y0.1O3-δ。
Preferably, in the step (3), the gas with different water vapor content is switched under an equilibrium state, and then the conductivity of the sample gradually reaches another equilibrium state.
Preferably, in the step (5), the proton surface exchange rate K is obtained by normalizing the change process of the conductivity with time and further fittingδ。
Compared with the prior art, the invention has the beneficial effects that:
1) the invention directly tests the perovskite material BaCo0.4Fe0.4Zr0.1Y0.1O3-δ(BCFZY) in a humid atmosphere andthe conductivity under dry atmosphere, by suddenly changing the water vapor content in the external atmosphere, the following reaction occurs on the surface of the material immediately
Figure BDA0003352360720000021
In the process, the proton enters the material along with the consumption of the cavity in the material, so that the conductivity of the material is changed, and therefore, the proton surface exchange rate of the material is measured by utilizing the change process of measuring the conductivity of the material, and the method has the characteristics of simplicity and feasibility.
2) The invention can simply and rapidly measure the proton surface exchange coefficient of the cathode material of the proton conductor. The measuring method is reliable, the data is accurate, and the measuring process is highly similar to the working process of the proton conductor cathode material.
Drawings
FIG. 1 is a graph of the conductivity of BCFZY in accordance with the present invention;
FIG. 2 is a graph showing the change in conductivity of BCFZY at 600 ℃ under 10% moisture pressure in example 1 of the present invention;
FIG. 3 shows the BCFZY gas (21% O) at 600 ℃ in example 1 of the present invention2) Normalizing the conductivity change graph at a flow rate of 100 ml/min;
FIG. 4 shows the BCFZY gas (21% O) at 600 ℃ in example 2 of the present invention2) Normalized conductivity plot at flow rate 50 ml/min;
FIG. 5 shows the BCFZY gas (100% O) at 600 ℃ in example 3 of the present invention2) Normalizing the conductivity change graph at a flow rate of 100 ml/min;
FIG. 6 shows the proton surface exchange coefficient of BCFZY at 550-700 ℃ in example 4 of the present invention;
FIG. 7 shows the proton surface exchange coefficients of BCFZY of different masses at 600 ℃ in example 5 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for measuring the proton surface exchange rate of a material by using conductance relaxation, which comprises the following steps:
(1) testing the conductivity of the sample at 600 ℃ by adopting a direct current four-terminal method;
(2) the water vapor content of the gas entering the sample was adjusted by means of a heater, the gas flow rate was 100ml/min, and the sample was humidified under a 10% water partial pressure (21% O) atmosphere2) The conductivity gradually decreases and stabilizes and reaches an equilibrium state;
(3) normalizing the change curve of the conductivity, and then obtaining the normalized change curve of the conductivity by the formula NC (t) ═ 1-expAtFitting to obtain an index A, the surface exchange rate K of the sample δ1/2AD, where D is the thickness of the sample.
FIG. 2 is a graph of the change in conductivity of BCFZY at 600 deg.C under 10% moisture, with the void content in BCFZY being depleted and the conductivity decreasing; the conductivity change curve was normalized and fitted to obtain the curve shown in fig. 3, with a fitting coefficient a of 9.32 x 10-4Calculating the exchange coefficient K of the surface of the protonδ＝3.26*10-5cm s-1。
Example 2
A method for measuring the proton surface exchange rate of a material by using conductance relaxation, which comprises the following steps:
(1) testing the conductivity of the sample at 600 ℃ by adopting a direct current four-terminal method;
(2) the water vapor content of the gas entering the sample was adjusted by a heater at a gas flow rate of 50ml/min under a 10% partial pressure of water in a humid atmosphere (21% O)2) The conductivity gradually decreases and stabilizes and reaches an equilibrium state;
(3) normalizing the change curve of the conductivity, and then obtaining the normalized change curve of the conductivity by the formula NC (t) ═ 1-expAtFitting to obtain an index A, the surface exchange rate K of the sample δ1/2AD, where D is the thickness of the sample.
FIG. 4 is the conductance of BCFZY at 600 ℃ gas flow rate of 50ml/minRate normalization of the fitted graph, the fitting resulted in an index A of 9.19 x 10-4Calculating the exchange coefficient K of the surface of the protonδ＝3.22*10-5cm s-1。
When the gas flow rate was switched from 100ml/min in example 1 to 50ml/min in example 2, the proton surface exchange coefficients of the samples were each Kδ＝3.26*10-5cm s-1And Kδ＝3.21*10-5cm s-1And the small error existing between the results of the two measurements belongs to artificial error, which shows that the gas flow rate has no influence on the proton surface exchange coefficient.
Example 3
A method for measuring the proton surface exchange rate of a material by using conductance relaxation, which comprises the following steps:
(1) testing the conductivity of the sample at 600 ℃ by adopting a direct current four-terminal method;
(2) regulating the content of water vapor in the gas entering the sample by a heater, wherein the gas flow rate is 100ml/min, and the pure oxygen (100% O) is humidified at 10% water partial pressure2) The conductivity gradually decreases and stabilizes and reaches an equilibrium state;
(3) normalizing the change curve of the conductivity, and then obtaining the normalized change curve of the conductivity by the formula NC (t) ═ 1-expAtFitting to obtain an index A, the surface exchange rate K of the sample δ1/2AD, where D is the thickness of the sample.
FIG. 5 is a graph of BCFZY humidified pure oxygen (100% O) at 10% water partial pressure at a gas flow rate of 100ml/min2) Normalized fitted graph of conductivity under, fitting coefficient a was 2.25 x 10-3And calculating to obtain the exchange coefficient K of the BCFZY proton surfaceδ＝7.89*10-5cm s-1The proton surface exchange coefficient of BCFZY is 100% O2Under the condition of (1) to 21% of O2The improvement is nearly 2.5 times.
Example 4
A method for measuring the proton surface exchange rate of a material by using conductance relaxation, which comprises the following steps:
(1) testing the conductivity of the sample at the temperature of 550-700 ℃ by adopting a direct-current four-terminal method;
(2) regulating the content of water vapor in gas entering a sample through a heater, and gradually reducing and stabilizing the conductivity under the wet atmosphere with 10% of water partial pressure to reach an equilibrium state;
(3) placing the sample at 550-700 ℃, instantly changing the content of water vapor in the gas introduced into the sample after the conductivity of the sample is stable, continuously recording the change process of the conductivity sigma of the sample along with the time, and ending the measurement process after the conductivity gradually reaches the stability;
(4) changing the test temperature of the sample, and measuring the change process of the conductivity of the sample after the water vapor content in the gas is changed at different temperatures within the range of 550-700 ℃;
(5) normalizing the change curve of the conductivity, and then obtaining the normalized change curve of the conductivity by the formula NC (t) ═ 1-expAtFitting to obtain an index A, the surface exchange rate K of the sample δ1/2AD, where D is the thickness of the sample.
FIG. 6 shows that the proton surface exchange coefficients of BCFZY at 550 ℃ and 700 ℃ are 2.12 x 10 respectively-5、3.26*10-5、7.11*10-5、1.02*10-4The proton surface exchange coefficient of the BCFZY is continuously increased along with the increase of the temperature, and the method can accurately measure the proton surface exchange coefficient at each temperature.
Example 5
A method for measuring the proton surface exchange rate of a material by using conductance relaxation, which comprises the following steps:
(1) samples of different masses (0.7g, 1.05g, 1.4g, 1.75g and 2.1g) were tested for conductivity at 600 ℃ using the direct current four terminal method;
(2) regulating the content of water vapor in gas entering a sample through a heater, and gradually reducing and stabilizing the conductivity under the wet atmosphere with 10% of water partial pressure to reach an equilibrium state;
(3) placing the sample at 600 ℃, instantly changing the content of water vapor in the gas introduced into the sample after the conductivity of the sample is stable, continuously recording the change process of the conductivity sigma of the sample along with the time, and ending the measurement process after the conductivity gradually reaches the stability;
(4) normalizing the change curve of the conductivity, and then obtaining the normalized change curve of the conductivity by the formula NC (t) ═ 1-expAtFitting to obtain an index A, the surface exchange rate K of the sample δ1/2AD, where D is the thickness of the sample.
FIG. 7 shows the proton surface exchange coefficients of BCFZY samples of different masses, the proton surface exchange coefficient of BCFZY samples being 3.26 x 10-5s cm-1Slight deviation occurs on the left and right, different sample amounts have no influence on the proton surface exchange coefficient of a sample, and the deviation is caused by human errors.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the present invention as defined in the accompanying claims.

Claims (4)

1.一种应用电导弛豫测量材料质子表面交换速率的方法，其特征在于，包括以下步骤：1. a method for applying conductivity relaxation measurement material proton surface exchange rate, is characterized in that, comprises the following steps: (1)采用直流四端子法测试样品在550-700℃范围内的电导率；(1) Use the DC four-terminal method to test the conductivity of the sample in the range of 550-700 °C; (2)通过加热器调节进入样品内气体中水蒸气的含量，在5％-10％水分压湿润大气下电导率逐渐降低稳定后转变为干燥气氛，电导率会逐渐升高并达到平衡状态；(2) The content of water vapor in the gas entering the sample is adjusted by the heater. Under the humid atmosphere of 5%-10% moisture pressure, the conductivity gradually decreases and stabilizes, and then the atmosphere is changed to a dry atmosphere, and the conductivity will gradually increase and reach an equilibrium state; (3)将样品置于550-700℃下，待样品电导率稳定后，瞬间改变通入样品内气体中水蒸气含量，同时连续记录样品电导率σ随时间的变化过程，待该电导率逐渐达到稳定后，测量过程结束；(3) Place the sample at 550-700°C. After the conductivity of the sample is stable, change the water vapor content in the gas in the sample instantaneously, and continuously record the change process of the conductivity σ of the sample with time. After reaching stability, the measurement process ends; (4)改变样品测试温度，在550-700℃范围内的不同温度下，测量样品电导率在气体中水蒸气含量改变后的变化过程；(4) Change the test temperature of the sample, and at different temperatures in the range of 550-700 °C, measure the change process of the sample conductivity after the water vapor content in the gas is changed; (5)将电导率变化曲线归一化处理后，通过公式NC(t)＝1-expAt拟合得到指数A，则样品的表面交换速率Kδ＝1/2AD，其中D为样品的厚度。(5) After normalizing the conductivity change curve, the index A is obtained by fitting the formula NC(t)=1-exp At , then the surface exchange rate of the sample K δ = 1/2AD, where D is the thickness of the sample . 2.根据权利要求1所述的一种应用电导弛豫测量材料质子表面交换速率的方法，其特征在于：所述步骤(1)中，样品包括BaCo0.4Fe0.4Zr0.1Y0.1O3-δ。2 . The method for measuring the proton surface exchange rate of a material using conductance relaxation according to claim 1 , wherein in the step (1), the sample comprises BaCo 0.4 Fe 0.4 Zr 0.1 Y 0.1 O 3-δ 2 . . 3.根据权利要求1所述的一种应用电导弛豫测量材料质子表面交换速率的方法，其特征在于：所述步骤(3)中，平衡状态下切换不同水蒸气含量的气体，然后样品电导率逐渐达到另一个平衡状态。3. A method for measuring the proton surface exchange rate of a material using conductance relaxation according to claim 1, wherein in the step (3), gases with different water vapor contents are switched in an equilibrium state, and then the sample conductance The rate gradually reaches another equilibrium state. 4.根据权利要求1所述的一种应用电导弛豫测量材料质子表面交换速率的方法，其特征在于：所述步骤(5)中，通过对电导率随时间的变化过程进行归一化处理，并进一步拟合得到质子表面交换速率Kδ。4 . The method for measuring the proton surface exchange rate of a material using conductance relaxation according to claim 1 , wherein in the step (5), normalization is performed on the change process of the conductance over time. 5 . , and further fitted to obtain the proton surface exchange rate K δ .
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CN105393132A (en) * 2013-03-29 2016-03-09 皇家飞利浦有限公司 Amide Proton Transfer (APT) and Electrical Performance Tomography (EPT) Imaging in a Single MR Acquisition
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Application publication date: 20220301