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NB/T 42007-2013 English PDF

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NB/T 42007-2013: Bipolar plate for vanadium flow battery-test method
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Basic data

Standard ID NB/T 42007-2013 (NB/T42007-2013)
Description (Translated English) Bipolar plate for vanadium flow battery-test method
Sector / Industry Energy Industry Standard (Recommended)
Classification of Chinese Standard K82
Classification of International Standard 27.070
Word Count Estimation 14,174
Quoted Standard GB/T 13465.2-2002
Regulation (derived from) National Energy Board Notice 2013 No. 4; industry standard for filing Notice 2013 No. 9 (No. 165 overall)
Issuing agency(ies) National Energy Administration

NB/T 42007-2013: Bipolar plate for vanadium flow battery-test method

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Bipolar plate for vanadium flow battery-test method NB ICS 27.070 K82 Record number. 41509-2013 Energy Industry Standards of the People's Republic of China Test method of bipolar plate for all vanadium redox flow battery Released on.2013-06-08 2013-10-01 implementation Issued by National Energy Administration

Table of contents

Foreword...Ⅱ 1 Scope...1 2 Normative references...1 3 Terms and definitions...1 4 General requirements...2 5 Test method...2 References...10

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009 "Guidelines for Standardization Work Part 1.Standard Structure and Compilation". This standard was proposed by China Electrical Equipment Industry Association. This standard is under the technical jurisdiction of the Energy Industry Flow Battery Standardization Technical Committee (NEA/TC23). The main drafting organizations of this standard. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian Rongke Energy Storage Technology Development Co., Ltd., Mechanical Engineering Industry Beijing Institute of Electrical Technology and Economics. Participated in the drafting of this standard. Beijing Puneng Century Technology Co., Ltd., China Electrical Equipment Industry Association, Institute of Metal Research, Chinese Academy of Sciences, Tsinghua University, Chengde Wanlitong Industrial Group Co., Ltd., China Electric Power Research Institute, State Grid Electric Power Research Institute, etc. The main drafters of this standard. Liu Zonghao, Zhang Huamin, Wang Xiaoli, Chen Chen, Li Ying, Tian Chaohe. Participating drafters of this standard. Yin Haitao, Yang Qiming, Yan Chuanwei, Lu Chenyu, Wang Baoguo, Zhang Yuxian, Chen Jizhong, Li Aikui, etc. Test method of bipolar plate for all vanadium redox flow battery

1 Scope

This standard specifies the general requirements and test methods for bipolar plates for all-vanadium redox flow batteries, mainly including thickness uniformity testing and warpage testing. Test, corrosion current density test, resistivity test, air permeability test, bending strength test, tensile strength test and compressive strength test. This standard applies to all bipolar plate materials for all vanadium redox flow batteries.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document. For undated references, the latest version (including all amendments) applies to this document. GB/T 13465.2-2002 Test method for flexural strength of impermeable graphite materials

3 Terms and definitions

The following terms and definitions apply to this standard. 3.1 Vanadium flow battery; VFB Also known as the all-vanadium redox flow battery system, it realizes the interaction of electric energy and chemical energy through the electrochemical reaction of vanadium ions in different valence states in the anode and cathode electrolyte Phase inversion energy storage device. Note. All vanadium redox flow batteries are mainly composed of power unit (stack or battery module), energy storage unit (electrolyte and storage tank), electrolyte delivery unit (pipeline, valve, Pumps, heat exchangers, etc.) and battery management systems. 3.2 Bipolar plate A conductive separator that collects and conducts current and separates the positive and negative electrolytes. 3.3 Corrosion current density Under the specified conditions, the current value of the bipolar plate per unit area of the battery due to electrochemical damage under the corrosion potential, unit It is μA/cm2. Note. The value of the corrosion current density reflects the corrosion rate of the bipolar plate, and is a physical quantity that characterizes the corrosion resistance of the bipolar plate material under the corrosion potential. 3.4 Volume resistivity The resistivity per unit cross-sectional area of the bipolar plate per unit length, in Ω·cm. 3.5 Interface contact resistance The resistance between the contact parts of two materials, the unit is Ω·cm2. Note. Use the contact resistance between the bipolar plate material and the electrode material (usually carbon felt) as a characterization. 3.6 Gas permeability Under the test conditions, the amount of gas passing through a unit area of the sample per unit time, in cm3/(cm2·s). 3.7 Bending strength Under specified conditions, the maximum bending stress that the material can withstand during the bending process, in MPa. 3.8 Tensile strength Under specified conditions, the maximum tensile stress that the material can withstand before it breaks during the stretching process, in MPa 3.9 Compressive strength Under specified conditions, the measured value of the ultimate load per unit area of the material, in MPa.

4 General requirements

Unless otherwise specified, the test should be carried out in the environment specified in this standard. For bipolar plate materials with special time and environmental requirements, It should be implemented in accordance with the requirements of the tested material, or determined by the supplier and the buyer through negotiation. The test environmental conditions of this standard are as follows. a) Temperature. (25±2)℃. b) Pressure. 86kPa~106kPa. c) Relative air humidity. 10%~96%.

5 Test method

5.1 Thickness uniformity test 5.1.1 Test equipment The instruments and accuracy requirements used in the test are as follows. a) Thickness gauge. accuracy of 1μm, used to test the thickness of bipolar plate samples. b) Vernier caliper. the accuracy is 0.02mm, used to test the length and width of the bipolar plate sample. 5.1.2 Sample preparation The test sample shall be prepared according to the following requirements. a) Cut rectangular materials of a certain size as samples according to the test requirements. b) The sample is of standard shape, its shape is shown in Figure 1, and its size is 100mm×100mm. c) The surface is smooth and clean, free of wrinkles and damage. 5.1.3 Test procedure Follow the steps below to test the thickness uniformity of the sample. a) Place the sample flat on the test platform of the thickness gauge. b) The zero point of the thickness gauge should be calibrated before each test, and the zero point should be rechecked after each group of samples is tested. c) Slowly put down the measuring head of the thickness gauge until the measuring head touches the surface of the material to be measured. During the operation, avoid sample deformation and damage. d) The thickness measurement position is shown in Figure 1.The test points should be distributed in the center of each demarcated area, and the distance from the edge of the sample should be greater than 5mm. Each test point should be repeated at least 5 times, and the arithmetic mean value shall be taken. e) Thickness uniformity is expressed by the difference between the maximum and minimum thickness, the average thickness of the bipolar plate, the thickness standard deviation and the dispersion coefficient. a) The sample is the entire bipolar plate component. b) The surface should be smooth, free of scratches and damage. 5.2.3 Test procedure Follow the steps below to test the warpage of the sample. a) Place the sample on the surface of the water platform with the concave surface facing up to ensure that no external force acts on the sample. b) Measure the diagonal length of the sample with a steel tape measure to the nearest 1mm. c) Use a height ruler to measure the maximum deviation between the surface of the sample plate and the height (ie the maximum chord height on the diagonal) to the nearest 0.02mm. d) Take 5 samples as a group and calculate the arithmetic mean as the test result. 5.2.4 Result calculation The warpage of the bipolar plate is calculated according to formula (5). 100%h ε = × (5) Where. ε-the degree of warpage of the bipolar plate, %; h --Maximum chord height of the sample diagonal, mm; L-the diagonal length of the sample, mm. 5.3 Corrosion current density test 5.3.1 Test equipment The instruments used in the test are as follows. a) Potentiostat. b) Electrochemical test cell. Use a five-necked flask, mainly used to hold electrolyte solution, the main material is glass or plastic, etc. Corrosion resistance material. The middle mouth of the five-necked flask is used to place the working electrode, and the other four mouths are used to place the reference electrode. The salt bridge, counter electrode, vent tube and replacement solution. 5.3.2 Sample preparation The test sample shall be prepared according to the following requirements. a) Cut rectangular materials of a certain size as samples according to the test requirements. b) The surface should be smooth, free of scratches and damage. c) Clean the surface of the sample with a solvent such as ethanol, and dry it for 30 minutes in a nitrogen atmosphere, at room temperature and pressure. d) Connect the electrode to the surface of the sample. Except for the test surface with an effective test area of 100mm2, the other surfaces are insulated and sealed. 5.3.3 Test procedure Follow the steps below to test the corrosion current density of the sample. a) Use the sample as the working electrode, the mercury electrode/mercurous sulfate electrode as the reference electrode, and the non-porous graphite plate as the counter electrode for testing. b) Soak the working electrode in 1.5M VOSO4 and 3M H2SO4 electrolyte solution. c) Perform a linear potential scan on the sample, the scan rate is 2mV/s, and the potential scan range is -0.2V~1.2V. d) Perform Tafel fitting on the measured polarization curve. The current corresponding to the intersection of the Tafel straight lines is the corrosion current of the sample. e) Take 5 samples as a group, and use the calculated arithmetic mean as the test result. 5.3.4 Result calculation The corrosion current density of the bipolar plate is calculated according to formula (6). corr = (6) Where. corri --corrosion current density, μA/cm2; I --corrosion current, μA; A --The effective test area of the sample, cm2. 5.4 Resistivity test 5.4.1 Test equipment The test equipment and accuracy requirements are as follows. a) Measure the resistance value with a four-probe low-resistance meter, and the measuring electrode is a gold-plated copper electrode. Volume resistivity of four-probe low resistance measuring instrument It is 0.01mΩ·cm. b) The accuracy of the low resistance measuring instrument is 0.01mΩ. 5.4.2 Sample preparation The test sample shall be prepared according to the following requirements. a) Cut rectangular materials of a certain size as samples according to the test requirements. b) The sample is a standard rectangular material (100mm×100mm), and the edge of the sample should not exceed the edge of the fixture. c) The surface should be smooth, free of scratches and damage. 5.4.3 Test procedure 5.4.3.1 Volume resistivity test Follow the steps below to test the volume resistivity of the sample. a) The zero point of the tester should be calibrated before each measurement. b) The influence of factors such as sample deformation and dust on the surface of the sample should be avoided during measurement. c) Use a four-probe low-resistance measuring instrument to measure the sample at 5 positions near the edge and the center, and record the body resistance values of different parts. d) Take 5 samples as a group and calculate the arithmetic mean as the test result. 5.4.3.2 Contact resistance test Follow the steps below to test the contact resistance of the sample. a) As shown in Figure 2, mount the sample on the test instrument. b) During the test, record the resistance value every time the pressure increases by 0.05 MPa, when the resistance test value changes from the previous resistance test value When the rate is less than or equal to 5%, it is considered that the minimum resistance is reached, the test is stopped, and the resistance value R1 under different pressures is recorded. c) The measuring pressure range is generally 0MPa~0.6MPa. d) Follow the same steps as a) to c) to remove the bipolar plate sample between the two layers of carbon felt, and record the resistance value R2 under different pressures. 5.4.4 Result calculation 5.4.4.1 Volume resistivity The resistivity of the bipolar plate is calculated according to formula (7). bulk 5 G Dρ ρ = × × (7) Where. bulkρ-the resistivity of the sample body, mΩ·cm; iρ --measured value of resistivity at different parts, mΩ·cm; G-sample thickness correction factor; D-sample shape correction factor. 5.4.4.2 Contact resistance The contact resistance of the bipolar plate is calculated according to formula (8). 1 2 BP() RRR AR--×= (8) Where. R-contact resistance between bipolar plate and carbon felt, Ω·cm2; 1R-Bipolar plate material body resistance, two carbon felt body resistance, contact resistance between the bipolar plate and two carbon felts, two copper electrodes The total volume resistance and the contact resistance between the two carbon felts and the copper electrode, Ω; 2R-the sum of the body resistance of the two copper electrodes, the body resistance of the two carbon felts and the contact resistance between the carbon felt and the copper electrode, Ω; BPR --Body resistance of bipolar plate material, Ω. A-The contact area between the bipolar plate sample and the carbon felt, cm2. Take 5 samples as a group and calculate the arithmetic mean as the test result. 5.5 Air permeability test 5.5.1 Test equipment The instruments used in the test are as follows. a) Gas chromatograph. b) Infiltration pool. 5.5.2 Sample preparation The test sample shall be prepared according to the following requirements. a) The sample is round with a diameter of 6cm. b) The surface of the sample should be smooth and free of wrinkles and damage. 5.5.3 Test procedure Follow the steps below to test the air permeability of the sample. a) Clamp the sample between two stainless steel fixtures with gas inlets and outlets, so that the two sides form gas chambers as test permeation Through the pool. b) Install the permeation cell on the test device according to the schematic diagram of the test device shown in Figure 3. c) Feed hydrogen with a pressure of 0.1 MPa on one side of the gas chamber, and feed helium with the same conditions on the other side to keep the pressure on both sides of the gas chamber Keep balance. Pressure balance is controlled by precision pressure gauges on both sides. d) Stabilize for at least 2h at a pressure of 0.1MPa, install the gas chromatograph at the outlet of the helium gas, and measure the concentration of the measured gas Degree and record the chromatogram. e) Take 5 samples as a group and calculate the arithmetic mean as the test result. 1- helium; 2- permeation cell; 3- gas chromatography; 4- tail gas; 5- hydrogen Description. The permeation cell consists of two stainless steel plate clamps with gas inlet and outlet, and the sample is placed in the middle of the two clamps. Used between fixture and sample The line is sealed and air chambers are formed on both sides. After entering the permeation cell, hydrogen and helium flow on both sides of the sample, so that the pressure balance on both sides of the membrane can be maintained. The pressure balance monitoring on both sides is mainly obtained through precision pressure gauges. The driving force of the measured gas permeation is the partial pressure of the gas on both sides of the sample. The helium gas flowing out of the cell contains the gas to be measured permeating from the other side of the bipolar plate, and the gas chromatograph is used to detect the gas to be measured at the outlet of the permeation cell concentration. Figure 3 Schematic diagram of bipolar plate air permeability test device 5.5.4 Result calculation The air permeability of the bipolar plate is calculated according to formula (9). qC = (9) Where. C--The gas permeability of the bipolar plate per unit time and unit area, cm3/(cm2·s); q --Gas penetration per unit time, cm 3/s; A --The effective test area of the penetrating cell, cm2. 5.6 Bending strength test 5.6.1 Test equipment The instruments and accuracy requirements used in the test are as follows. a) Universal testing machine. a testing machine that can meet the test requirements of this standard with a measurement accuracy of not less than 0.5. b) Vernier caliper. the accuracy is 0.02mm, used to test the width and thickness of the sample. 5.6.2 Sample preparation The test sample shall be prepared according to the following requirements. a) Cut a 100mm×10mm rectangular material on the bipolar plate as a test sample, or determine the size according to the test requirements. b) Adjust the span of the universal testing machine so that the span of the support is smaller than the length of the sample. c) The surface of the sample should be smooth and free of scratches and damage. 5.6.3 Test procedure Follow the steps below to test the bending strength of the sample. a) Measure the width and thickness of the sample to the nearest 0.02mm. b) Conduct the bending strength test in accordance with the regulations in GB/T 13465.2-2002. c) The indenter applies the load uniformly and without impact at a loading speed of 1mm/min~3mm/min until the sample breaks, and read the breaking load Charge value. d) Take 5 samples as a group and calculate the arithmetic mean as the test result. 5.6.4 Result calculation The bending strength of the bipolar plate is calculated according to formula (10). PL σ δ (10) Where. σ-bending strength, MPa; P-breaking load value, N; L-bearing span, mm; b-the width of the sample, mm; δ-the thickness of the sample, mm. 5.7 Tensile strength test 5.7.1 Test equipment The instruments and accuracy requirements used in the test are as follows. a) Universal testing machine. a testing machine that can meet the test requirements of this standard with a measurement accuracy of not less than 0.5. b) Vernier caliper. the accuracy is 0.02mm, used to test the width and thickness of the sample. 5.7.2 Sample preparation The test sample shall be prepared according to the following requirements. a) Cut a 70mm×10mm rectangular material on the bipolar plate as a test sample, or determine the sample size according to the test requirements. b) The gauge length of the sample is 50mm. c) The surface should be smooth, free of scratches and damage. 5.7.3 Test procedure Follow the steps below to test the tensile strength of the sample. a) Measure the thickness and width of the sample within the gauge length of the sample to an accuracy of 0.02mm. b) Clamp the sample into the fixture of the testing machine, put it into the upper end of the testing machine, sag naturally, and then clamp it into the lower end of the testing machine. c) Clamp the clamp to prevent the specimen from slipping off or breaking in the clamp during stretching. d) Start the testing machine, stretch at a speed of 3mm/min~7mm/min, and record the load value when the sample breaks. e) When the sample breaks at a position outside the gauge length, this test is invalid, and another sample should be taken and repeated. f) Take 5 samples as a group and calculate the arithmetic mean as the test result. 5.7.4 Result calculation The tensile strength of the bipolar plate is calculated according to formula (11). σ δ= × (11) Where. tσ --tensile strength, MPa; P-breaking load, N; b-the width of the sample, mm; δ-the thickness of the sample, mm. 5.8 Compressive strength test 5.8.1 Test equipment The instruments and accuracy requirements used in the test are as follows. a) Universal testing machine. a testing machine that can meet the test requirements of this standard, and the measurement accuracy is not less than level 1. b) Vernier caliper. the accuracy is 0.02mm, used to test the width and thickness of the sample. 5.8.2 Sample preparation The test sample shall be prepared according to the following requirements. a) Cut a rectangular material of 10mm×10mm on the bipolar plate as a test sample, or determine the sample size according to the test requirements. b) The surface should be smooth, free of scratches and damage. 5.8.3 Test procedure 5.8.3.1 The test and calculation methods of the sample are as follows. a) Length detection. Measure 3 times across the surface of the sample and take the average value. b) Width detection. Measure 3 times along the longitudinal direction of the sample surface, and take the average value. c) Use the measured length and width to calculate the pressure area. 5.8.3.2 Place the sample at the center of the working surface of the testing machine on the designated pressure surface. There is a protective cover around the sample to prevent the sample from breaking. The debris flew out. 5.8.3.3 Start the testing machine and apply the load continuously, uniformly, and without impact at a load of 1.0kN~1.5kN per second until the sample is broken. Read the failure load value of the sample. Note. The displacement value of the indenter of the testing machine should be less than the sample thickness. 5.8.3.4 Take 5 samples as a group, and calculate the arithmetic mean as the test result. 5.8.4 Result calculation The compressive strength of the bipolar plate is calculated according to formula (12). σ = (12) Where. cσ --Compressive strength, MPa; P --load limit value, N; --The cross-sectional area of the sample under pressure, mm2. references [1] GB/T.20042.6-2011 Proton Exchange Membrane Fuel Cell Part 6.Bipolar Plate Characteristics Test Method

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