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NB/T 42080-2023 English PDF

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NB/T 42080-2023: Ion conductive membrane for Vanadium flow battery-technical conditions and test methods
Status: Valid

NB/T 42080: Evolution and historical versions

Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
NB/T 42080-2023	English	419	Add to Cart	4 days [Need to translate]	Ion conductive membrane for Vanadium flow battery-technical conditions and test methods	Valid	NB/T 42080-2023
NB/T 42080-2016	English	839	Add to Cart	4 days [Need to translate]	Ion conductive membrane for Vanadium flow battery-Test method	Obsolete	NB/T 42080-2016

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Basic data

Standard ID	NB/T 42080-2023 (NB/T42080-2023)
Description (Translated English)	Ion conductive membrane for Vanadium flow battery-technical conditions and test methods
Sector / Industry	Energy Industry Standard (Recommended)
Classification of Chinese Standard	K82
Classification of International Standard	27.070
Word Count Estimation	21,255
Date of Issue	2023-02-06
Date of Implementation	2023-08-06
Issuing agency(ies)	National Energy Administration

NB/T 42080-2016: Ion conductive membrane for Vanadium flow battery-Test method

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Ion conductive membrane for Vanadium flow battery-Test method NB 10mm 23.5mm ICS 27.070 K 82 Record number. 55689-2016 Energy Industry Standards of the People's Republic of China Test method of ion conducting membrane for vanadium redox flow battery Released on.2016-08-16 2016-12-01 implementation Issued by National Energy Administration 40mm 182mm 12mm

Foreword... II 1 Scope... 1 2 Normative reference documents... 1 3 Terms and Definitions... 1 4 Sampling methods and general conditions... 2 5 Test method... 2 Appendix A (informative appendix) Pretreatment method of ion conducting membrane... 13 Appendix B (informative appendix) Blasting strength test method... 14 Appendix C (informative appendix) Preparation method for ion selection coefficient test... 15 Appendix D (informative appendix) Method of deriving the formula of apparent ion diffusion coefficient... 16 Appendix E (informative appendix) Calculation example of the selection coefficient of ion-conducting membrane for H and VO2... 17

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 jurisdiction of the Energy Industry Flow Battery Standardization Technical Committee (NEA/TC 23). The main drafting organizations of this standard. Tsinghua University, Beijing Institute of Electrical Technology and Economics of Mechanical Industry, Dalian Chemical Physics, Chinese Academy of Sciences Research Institute, Chengde Wanlitong Industrial Group Co., Ltd., Shanghai Shenli Technology Co., Ltd., Dalian Rongke Energy Storage Technology Development Co., Ltd. Participated in the drafting of this standard. Beijing Jinneng Fuel Cell Co., Ltd., China Electrical Equipment Industry Association, TBEA Shenyang Transformer Group Group Co., Ltd. Automation Branch, the First Research Institute of Anti-chemical Research Institute, etc. The main drafters of this standard. Wang Baoguo, Li Bingyang, Tian Chaohe, Zhang Huamin, Zhang Yuxian, Lu Chenyu, Hu Liqing, Zhang Ruogu, Wang Xiaoli, Li Ying. Participating drafters of this standard. Chen Chen, Luo Xin, Xu Jinliang, Cheng Jie, Li Xia, etc. This standard is formulated for the first time. Test method of ion conducting membrane for vanadium redox flow battery

1 Scope

This standard specifies the sampling method and general conditions of ion-conducting membranes for all-vanadium redox flow batteries, as well as membrane thickness uniformity, moisture content, and scale. Test methods for size change rate, tensile properties, electrical conductivity, membrane surface resistance, ion selectivity, and oxidation resistance. This standard applies to various types of ion conductive membranes used in 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 article Pieces. For undated references, the latest version (including all amendments) applies to this document. GB/T 601-2002 Preparation of chemical reagent standard titration solution GB/T 1040.3 Determination of tensile properties of plastics Part 3.Test conditions for films and sheets GB/T 6672 Plastic film and sheet thickness determination mechanical measurement method GB/T.20103 Membrane separation technical terms GB/T 29840-2013 Terminology for all vanadium redox flow batteries

3 Terms and definitions

The following terms and definitions defined in GB/T 29840-2013 and GB/T.20103 apply to this standard. 3.1 Ion conductive membrane A separator that separates the positive and negative electrolytes and selectively conducts ions. Note 1.Both ion exchange membranes and porous ion conducting membranes belong to ion conducting membranes, and the mechanisms for conducting ions are ion exchange mechanism and sieving mechanism respectively. Note 2.Rewrite GB/T 29840-2013, definition 2.2. 3.2 Ion exchange membrane With ion-exchange groups, ion-conducting membranes that can selectively permeate ions. 3.3 Porous ion conductive membrane An ion-conducting membrane that uses nano-pore size to realize the screening and conducting functions of hydrogen ions and vanadium ions. 3.4 Membrane resistance The resistance in the thickness direction of the film at a given temperature and solution composition. Note. The unit of membrane resistance is Ω. 3.5 Effective area The geometric area of the ion-conducting membrane that is perpendicular to the direction of current flow to achieve ion conduction. 3.6 Membrane area resistance The product of the membrane resistance and the effective area of the membrane during measurement. Note. The unit of membrane surface resistance is Ω·cm2. 3.7 Membrane conductivity The membrane's ability to transfer ions is equal to the ratio of membrane thickness to membrane surface resistance. Note. The unit of membrane conductivity is S/cm. 3.8 Ion diffusion coefficient The flux of a given ion through an ion-conducting membrane under given conditions. Note. The unit of diffusion coefficient is cm2/s. 3.9 Ion permeation selectivity The characteristic of ion-conducting membrane for selective transmission of different ions, and its value is equal to the ion diffusion of different ions measured under given conditions Ratio of coefficients. 3.10 Bursting strength Continuously apply pressure to the ion-conducting membrane through liquid or air until the sample ruptures, the maximum pressure measured. Note. The unit of burst strength is MPa.

4 Sampling methods and general conditions

Samples are randomly selected from the same batch or different batches. Unless otherwise specified, the test shall be carried out in the environment specified in this standard. For ion-conducting membranes with special environmental requirements, press The requirements of the tested materials may be negotiated between the supplier and the buyer. The test environmental conditions of this standard are as follows. --Temperature. 25℃±5℃; --Relative humidity. 5% to 95%. Each test is tested at least 3 times (make sure to get 3 valid values).

5 Test method

5.1 Sample requirements Sampling is carried out in accordance with the requirements of Chapter 4.Detect with visual method, supplemented with inspection box to observe if necessary, ion conduction membrane should be free of wrinkles and surface View defects and breakages. For the same batch of ion conducting membranes, at least 3 samples shall be randomly selected for testing. 5.2 Instrument accuracy requirements The instruments used in this standard have accuracy requirements as follows. --Thickness measuring instrument, used to test the thickness of ion conducting membrane, with an accuracy of not less than 0.1μm; --Length measuring instrument, used to test the length and width of the ion conductive membrane, the accuracy is not less than 0.1mm; --Ordinary oven, temperature control accuracy is not less than 1℃; --Analytical balance, the accuracy is not less than 0.1mg; -Constant temperature bath, temperature control accuracy is not less than 0.5℃; doz --the thickness of the sample film before pretreatment, in micrometers (μm). b) Calculation of linear swelling rate of ion conducting membrane in x direction. 100%wx oxx ox ll Φ -= × (6) Where. Linear swelling rate in Φx --x direction, the unit is percentage (%); lwx - The length of the sample film after pretreatment in the x direction, in millimeters (mm); lox - The length of the sample film before pretreatment in the x direction, in millimeters (mm). c) Calculation of linear swelling rate in y direction of ion conducting membrane. 100%wy oyy oy ll = × (7) Where. Linear swelling rate in Φy --y direction, the unit is percentage (%); lwy - The length of the sample film after pretreatment in the y direction, in millimeters (mm); The length of the sample film before pretreatment in the loy --y direction, in millimeters (mm). Take 3 samples as a group and calculate the average value as the test result. 5.6 Tensile performance 5.6.1 Apparatus and equipment Instruments and equipment include. --Testing machine. Any testing machine that can meet the test requirements of this part is fine. --Test fixture. The test fixture should not cause the sample to break at the clamping position; when the load is applied, it should satisfy the longitudinal axis of the The stretching directions with the center line coincide. --Thickness gauge and calipers. 5.6.2 Sample preparation Prepare samples according to the following steps, specifically. a) Cut the pretreated film at equal intervals along the length (x-direction) and width (y-direction) of the test material. According to GB/T According to 1040.3, cut into a certain size dumbbell or long strip shape. The edge of the sample should be smooth without gaps, and can be inspected with a low-power magnifying glass Check for gaps and discard samples with defective edges. b) The samples are divided into one group for each test direction, and the number of samples in each group should meet the requirements of 3 effective tests. c) Accurately print or draw markings according to the sample size requirements. This marking should not have any effect on the sample. d) The sample should be tested under the condition of relative humidity of 50%±10%, and the storage time should be at least 4h. Placement conditions can also be tested Both parties negotiated and determined. 5.6.3 Test method a) The thickness and width of each sample shall be measured at 3 points within the gauge length, and the average value shall be taken as the thickness of the film and recorded as d. Place the sample in In the test fixture, make the longitudinal axis of the sample coincide with the center line of the upper and lower fixtures and clamp it. The pressure of the pneumatic clamp is Select within the range of 0.3MPa～0.7MPa. b) The tensile speed of the testing machine is selected within the range of 50mm/min～200mm/min. c) After the sample is broken, read the corresponding load value and the corresponding elongation value between markings. If the sample breaks at a position outside the marking line, the This trial is invalid. 5.6.4 Data processing According to the measured stretch curve, read the required load and the corresponding film thickness and width, and calculate the maximum stretch of the film according to formula (8) strength. /p bdσ = (8) Where. σ-the maximum tensile strength of the film, in megapascals (MPa); p --Maximum load, the unit is Newton (N); b-the width of the sample, in millimeters (mm); d-the thickness of the sample, in millimeters (mm). Note. The tensile properties of ion-conducting membranes can also be characterized by bursting strength. Refer to Appendix B for test methods. According to the difference between the distance between the marking lines when the specimen is broken and the distance between the original marking lines, use formula (9) to calculate the tensile strain at break. 0t 100% LL = × (9) Where. tε-tensile strain at break; 0L-the distance between the original markings of the sample, in millimeters (mm); L-The distance between the marking lines when the sample is broken, in millimeters (mm). Take 3 samples as a group and calculate the average value as the test result. The maximum tensile strength and tensile strain at break can characterize the tensile properties of the ion conductive membrane. 5.7 Conductivity and membrane surface resistance 5.7.1 Test Principle Using high frequency AC scanning technology to measure impedance, by quickly changing the direction of the voltage applied on both sides of the membrane, eliminating the concentration polarization caused Error. Ion-conducting membrane can be regarded as a positively or negatively charged solid electrolyte system, an electric double layer that exists at the interface between the membrane and the solution It can be equivalent to a physical capacitor, and the two together form a series equivalent circuit of a resistor and a capacitor. Using the AC impedance method of electrochemical workstation, Measure the resistance of the electrolyte and the resistance of the sum of the membrane and the electrolyte. After subtracting the resistance of the electrolyte, the membrane surface resistance can be obtained. 5.7.2 Apparatus and equipment The recommended equipment for this test is as follows. a) Electrochemical workstation; b) Conductivity test device. It is mainly composed of two identical half tanks combined into a whole. Half groove with platinum electrode, usually organic It is made of glass. The diameter of the semi-slot round hole is 10mm and the groove depth is 8mm. The structure of the conductivity cell is shown in Figure 1. In addition, any test equipment that meets the test principles and technical conditions can be used. 5.7.3 Reagents The chemical reagents needed in this test are mainly 3.0mol/L sulfuric acid aqueous solution, according to the relevant operations given in 4.3 of GB/T 601-2002 Rules. 5.7.4 Sample preparation Cut the pre-treated film to a certain size (15mm×15mm) and immerse it in a 3.0mol/L sulfuric acid aqueous solution, and let it stand at room temperature 24h, or oscillate at 40℃ for more than 4h in a thermostatic mechanical oscillator. The impedance R2 of the conductivity cell of the film sample. e) Repeat the measurement 3 times, record all impedance data and calculate the average value, which is recorded as 1R and 2R. f) Measure the average thickness of the film according to the method given in 5.3 and record it as d. 5.7.6 Data processing 5.7.6.1 The membrane resistance in the conductivity cell is calculated as follows according to formula (10). m 2 1R RR=-(10) Where. Rm-membrane resistance, the unit is ohm (Ω); 2R-the impedance value of the conductivity cell with the membrane sample installed, in ohms (Ω); 1R-the impedance value of the conductivity cell without the membrane sample installed, in ohms (Ω). 5.7.6.2 The surface resistance of the membrane in the conductivity cell is calculated as follows according to formula (11). mAR RA= (11) Where. RA-membrane surface resistance, in ohm square centimeter (Ω·cm2); Rm-membrane resistance, the unit is ohm (Ω); A --The effective area of the membrane, in square centimeters (cm2). 5.7.6.3 The conductivity of the ion conductive membrane in the conductivity cell is calculated as follows according to formula (12). κ (12) Where. κ-membrane conductivity, the unit is (S/cm); RA-membrane surface resistance, in ohm square centimeter (Ω·cm2); d-the average thickness of the film, in centimeters (cm). Take 3 samples as a group and calculate the average value as the test result. 5.8 Ion selectivity coefficient 5.8.1 Test Principle Use 1.5mol/L VOSO4, 3 mol/L sulfuric acid aqueous solution to simulate the electrolyte of the all-vanadium redox flow battery to measure the permeation ions of H and VO2 The ion diffusion coefficient when the conductive membrane diffuses to the blank side of deionized water, and the ratio of the diffusion coefficient of H and VO2 is used to characterize the ions of the membrane Selective. The change of H concentration on the blank side with time is measured by a pH composite electrode, and the change of VO2 concentration with time is measured by ultraviolet-visible spectroscopy. Measured by the meter. 5.8.2 Apparatus and equipment The equipment required for this test is as follows. -Constant temperature bath, temperature control accuracy is not less than 0.5℃; --pH meter with accuracy not less than 0.01 level; --pH composite electrode; --Magnetic stirrer; --Ultraviolet visible spectrophotometer, the photometric accuracy is not less than 0.5%T; --The conduction pool is composed of two identical half grooves combined into a whole, which is made of corrosion-resistant materials. The structure is shown in Figure 2. a-absorbance; 2VO The concentration of C --VO2, in moles per liter (mol/L). 5.8.5.2 Calculate the diffusion coefficients of H and VO2 according to the formula in Appendix D (D.3) D and 2VOD. 5.8.5.3 Calculate the selectivity coefficient of the membrane to H and VO2 according to formula (14). VO = (14) Where. α --The selectivity coefficient of the membrane to H and VO2; D --H diffusion coefficient in the membrane; 2VO D --The diffusion coefficient of VO2 in the film. The average value of the measured 3 sample membranes is recorded as the ion selectivity coefficient of the membrane. Note. Refer to Appendix D and Appendix E for specific formula derivation process and calculation examples. 5.9 Antioxidant 5.9.1 Test method The oxidation resistance of the ion-conducting membrane reflects the stability of the membrane material during actual use. Two methods can be used for quantitative characterization. ①Five Valence vanadium ion oxidation method; ②Fenton reagent oxidation method. Note. It is recommended to choose the pentavalent vanadium ion oxidation method first. 5.9.2 Pentavalent vanadium ion oxidation method 5.9.2.1 Test Principle The ion conducting membrane is immersed in a sulfuric acid aqueous solution containing pentavalent vanadium ions, and after a certain period of time, by detecting whether tetravalent vanadium appears in the solution The concentration of ions and tetravalent vanadium ions increases to indirectly reflect the oxidation of the membrane, which serves as an indicator of the oxidation resistance of the ion-conducting membrane. 5.9.2.2 Instruments and equipment The equipment used is an ultraviolet-visible spectrophotometer. Note. VO2 has the maximum absorption peak for ultraviolet light with a wavelength of 765.5nm. 5.9.2.3 Reagents The reagents used include. --Deionized water. at 25℃, the conductivity is less than 10μS/cm; --Sulfuric acid aqueous solution of pentavalent vanadium ion. 1.5mol/L pentavalent vanadium ion solution, 3mol/L H2SO4. Note. Preparation method of sulfuric acid aqueous solution of pentavalent vanadium ion. Put the vanadium sulfate solution with the vanadium ion concentration of 1.5 mol/L and the sulfuric acid concentration of 3 mol/L in the electric The positive side of the cell is charged until the concentration of the tetravalent vanadium ion is lower than the lower limit of detection by the UV-visible spectrophotometer, indicating that the tetravalent vanadium ion is completely transformed into Pentavalent vanadium ion. The prepared sulfuric acid aqueous solution containing only pentavalent vanadium ions is used as a solution for impregnating the ion conductive membrane. 5.9.2.4 Test method Cut the pretreated membrane into a 5cm×5cm membrane sample and place it in a beaker, add 30ml of sulfuric acid aqueous solution containing only pentavalent vanadium ions, and keep it The card film is completely submerged. After being immersed for 7 days at room temperature, the film was taken out, and the concentration of tetravalent vanadium ions in the solution was detected by an ultraviolet spectrophotometer. And compared with the blank sample of sulfuric acid aqueous solution of pentavalent vanadium ion without adding membrane. 5.9.2.5 Evaluation of antioxidant performance According to the measured relationship between the absorbance of the UV-visible spectrophotometer and the concentration of VO2, if the absorbance of the solution is detected to be greater than that of the instrument The lower limit of measurement proves that the solution contains tetravalent vanadium ions. It shows that the membrane is oxidized by pentavalent vanadium ions, and localized polymer materials have occurred degradation. 5.9.3 Fenton reagent oxidation method 5.9.3.1 Test principle The ion-conducting membrane is treated by Fenton reagent oxidation method, and the weight change and conductivity change of the membrane are used as a characterization of the membrane's oxidation resistance method. 5.9.3.2 Reagents --Hydrogen peroxide. analytically pure, with a mass fraction of 30%; --3% H2O2 solution. Dilute 30% hydrogen peroxide directly by 10 times; --3.0mol/L sulfuric acid aqueous solution; --Ferrous sulfate (FeSO4·7H2O). analytically pure; --0.01mol/L Fe2 solution. Weigh 6.9508g of ferrous sulfate (FeSO4·7H2O) and dissolve it in a beaker, in a 250mL volume Constant volume in the bottle; --Fenton reagent. 50 mL of H2O2 solution with a mass fraction of 3%, to which 0.1mL 0.01mol/L Fe2 solution is added dropwise, namely Equipped with Fenton reagent. Fenton reagents should be prepared and used. 5.9.3.3 Evaluation method of oxidation resistance 5.9.3.3.1 Quality change method 5.9.3.3.1.1 Cut the pretreated film fragments (2cm×2cm) and place them in an oven (70℃～80℃) to dry them until the weight is weighed twice before and after The difference is less than 1 mg, and its mass is weighed with a balance as om. 5.9.3.3.1.2 Put the dried membrane fragments into a beaker, add the prepared Fenton reagent to ensure that the membrane is completely submerged, and then place the beaker Heat in a water bath at 60°C and maintain a constant temperature for 3 hours. 5.9.3.3.1.3 Take the membrane out, put it into a beaker containing 3 moL/L dilute sulfuric acid aqueous solution, soak for a few minutes and gently shake the beaker, then Rinse the membrane sample with deionized water until the pH of the water after washing is neutral. Note. If the pH value is 7 tested with a wide pH test paper, it is regarded as neutral. 5.9.3.3.1.4 Put the rinsed film in an oven (70℃～80℃) and dry it again until the difference in mass between the two weighings is less than 1mg. The balance weighs its mass as am. Use formula (15) to compare the quality change of the film before and after Fenton reagent treatment to characterize the anti-oxidation performance of the film. The larger the value, the more The more severe the degradation of the polymer membrane during the Fenton reagent treatment process, the worse the oxidation resistance of the membrane. The oxidation resistance coefficient is represented by Sfm. o af 100% m mS = × (15) Where. Sf-Fenton reagent oxidation method measured, the oxidation resistance coefficient characterized by mass change; mo --The quality of the membrane before Fenton reagent treatment; ma - The quality of the film after drying with Fenton reagent. 5.9.3.3.2 Conductivity change method 5.9.3.3.2.1 Cut a certain membrane fragment (2cm×2cm), test its conductivity according to 5.7, and record it as κo. 5.9.3.3.2.2 After testing the surface resistance, rinse the membrane fragments with deionized water, put them in a beaker, and add the prepared Fenton test To ensure that the film is completely immersed, place the beaker in a water bath at 60°C and heat it at a constant temperature for 3 hours. 5.9.3.3.2.3 Take the membrane out, put it in a beaker containing 3moL/L dilute sulfuric acid, soak the membrane for a few minutes and shake the beaker gently, then use it to remove The sub-water rinses the membrane sample until the pH of the water after washing is neutral. Note. If the pH value is 7 tested with a wide pH test paper, it is regarded as neutral. 5.9.3.3.2.4 Test the conductivity of the cleaned membrane again in accordance with 5.7 and record it as κa. Use formula (16) to compare the conductivity change rate of the membrane before and after Fenton reagent treatment to characterize the oxidation resistance of the membrane. The larger the value, the table Shows the greater the stability of the film. The oxidation resistance coefficient is expressed by Sfk. af 100%S κ κκ = × (16) Where. fS κ-Fenton reagent oxidation method, the oxidation resistance coefficient characterized by the change of conductivity; oκ-membrane conductivity before Fenton reagent treatment; aκ-the membrane conductivity after Fenton reagent treatment. 5.9.3.3.3 Tensile strength change method 5.9.3.3.3.1 According to 5.6, the maximum tensile strength of the test sample film is recorded as oσ. 5.9.3.3.3.2 Put the parallel membrane sample into a beaker, add the prepared Fenton reagent to ensure that the membrane is completely submerged, and then place the beaker Heat in a water bath at 60°C and maintain a constant temperature for 3 hours. 5.9.3.3.3.3 Take the membrane out, put it in a beaker containing 3moL/L dilute sulfuric acid, soak the membrane for a few minutes and shake the beaker gently, then use it to remove Wash the membrane sa...

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