CN103268946A - A method for sintering and modifying graphite felt electrodes of liquid flow batteries - Google Patents
A method for sintering and modifying graphite felt electrodes of liquid flow batteries Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 69
- 239000010439 graphite Substances 0.000 title claims abstract description 69
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 9
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Abstract
Description
技术领域technical field
本发明属于蓄电池技术领域，尤其涉及氢气-氧化还原电对液流电池。The invention belongs to the technical field of accumulators, and in particular relates to a hydrogen-oxidation-reduction pair liquid flow battery.
背景技术Background technique
氢气-氧化还原电对液流电池是一种新型的液流电池，与传统液流电池由溶解于一定浓度硫酸溶液中的不同价态的金属离子作为正负极电极反应活性物质不同，氢气-氧化还原电对液流电池负极是铂碳电极，铂碳电极催化层中的氢气在催化剂作用下发生电极反应。电池正负极之间以离子交换膜分隔成彼此相互独立的两室（正极侧与负极侧），电池工作时正极电解液由送液泵强制通过反应室循环流动，参与电化学反应。电极上所发生的反应如下：The hydrogen-redox pair flow battery is a new type of flow battery, which is different from the traditional flow battery, which uses metal ions of different valence states dissolved in a certain concentration of sulfuric acid solution as the positive and negative electrode reaction active materials. Hydrogen- The negative electrode of the redox pair flow battery is a platinum carbon electrode, and the hydrogen in the catalytic layer of the platinum carbon electrode undergoes an electrode reaction under the action of the catalyst. The positive and negative electrodes of the battery are separated into two independent chambers (positive electrode side and negative electrode side) by an ion exchange membrane. When the battery is working, the positive electrode electrolyte is forced to circulate through the reaction chamber by the liquid delivery pump to participate in the electrochemical reaction. The reactions that take place at the electrodes are as follows:
正极:MO n++xe-→MR m+ Positive electrode: M O n+ +xe - →M R m+
负极:H2→2H++2e- Negative pole: H 2 →2H + +2e -
正极活性物质M为液态流体氧化还原电对如VO2+/VO2 +、Fe3+/Fe2+、Ce4+/Ce3+等的硫酸溶液。此新型液流电池除了具有传统液流电池自放电效率低、使用寿命长、便于维护、无交叉污染、可深度放等特点外，由于正负极均采用可逆电极，氢气-金属电对的储能电池可以在靠近热力学平衡电位下进行充放电，解决了传统液流电池电极不可逆带来的高过电位损失，可望解决目前储能技术存在的不足。The positive electrode active material M is a sulfuric acid solution of liquid redox couples such as VO 2+ /VO 2 + , Fe 3+ /Fe 2+ , Ce 4+ /Ce 3+ , etc. In addition to the characteristics of traditional flow batteries such as low self-discharge efficiency, long service life, easy maintenance, no cross-contamination, and deep discharge, this new type of flow battery uses reversible electrodes for both the positive and negative electrodes, and the storage capacity of the hydrogen-metal pair The energy battery can be charged and discharged close to the thermodynamic equilibrium potential, which solves the high overpotential loss caused by the irreversibility of the electrodes of the traditional flow battery, and is expected to solve the shortcomings of the current energy storage technology.
虽然氢气-氧化还原电对液流电池比传统液流电池有显著优势,但其正极反应与传统液流电池相同，依然与传统液流电池一样面临许多尚待解决的问题,比如,如何筛选具有良好选择透过性的隔膜,以及如何得到稳定性好、电阻率低、电化学活性好的电极等。其中,电极依然是决定整个氢气-氧化还原电对液流电池性能好坏的关键。Although the hydrogen-redox pair flow battery has significant advantages over the traditional flow battery, its positive electrode reaction is the same as that of the traditional flow battery, and it still faces many unsolved problems like the traditional flow battery, for example, how to screen the A separator with good selective permeability, and how to obtain an electrode with good stability, low resistivity, and good electrochemical activity, etc. Among them, the electrode is still the key to determine the performance of the whole hydrogen-redox flow battery.
现有技术中，最好的液流电池正极电极是石墨毡。石墨毡需要通过适当的前处理来增加其对液流电池的氧化还原反应催化作用。常用的方法为：热处理、浓硫酸处理、化学氧化处理等。现有技术的不足是：In the prior art, the best positive electrode for a flow battery is graphite felt. Graphite felt needs to be properly pre-treated to increase its catalytic effect on redox reactions in flow batteries. Commonly used methods are: heat treatment, concentrated sulfuric acid treatment, chemical oxidation treatment, etc. The deficiencies of prior art are:
常规热处理法虽工艺简单,但操作弹性较小,能量消耗大,氧化反应不易控制。并且传统的碳化、活化方式中的加热模式是通过热传导加热，热量由表面传到内部。这种传热方式达到热平衡需要较长的时间，热损失大，耗能高；Although the conventional heat treatment method is simple in process, the operation flexibility is small, the energy consumption is large, and the oxidation reaction is not easy to control. And the heating mode in the traditional carbonization and activation method is heating by heat conduction, and the heat is transferred from the surface to the inside. It takes a long time for this heat transfer method to achieve heat balance, with large heat loss and high energy consumption;
浓硫酸处理是使用的处理剂是浓硫酸，十分危险,工业化生产难度大；电化学氧化处理方法处理的时间长，耗能耗时。Concentrated sulfuric acid treatment uses concentrated sulfuric acid as a treatment agent, which is very dangerous and difficult for industrial production; the electrochemical oxidation treatment method takes a long time and consumes energy and time.
发明内容Contents of the invention
本发明的目的是提供一种节能的液流电池正极电极石墨毡前处理方法，克服现有技术的不足。The purpose of the present invention is to provide an energy-saving pretreatment method for the graphite felt of the positive electrode of the liquid flow battery, so as to overcome the deficiencies of the prior art.
本发明的基本思路是：利用微波加热来处理液流电池正极电极石墨毡，微波加热能量转变所需的时间近似即时，可达到快速加热的目的，避免了长时间加热所造成的热散失，是一种节能加热方式。The basic idea of the present invention is: using microwave heating to process the graphite felt of the positive electrode electrode of the liquid flow battery, the time required for microwave heating energy conversion is approximately instantaneous, which can achieve the purpose of rapid heating and avoid heat loss caused by long-term heating, which is An energy-saving heating method.
本发明的技术方案是：一种液流电池石墨毡电极烧结改性处理方法，包括热处理方法，其特征在于：所述热处理方法是将石墨毡电极表面清理干净后放在微波烧结炉内用微波加热处理。The technical solution of the present invention is: a method for sintering and modifying the graphite felt electrode of a liquid flow battery, including a heat treatment method, characterized in that: the heat treatment method is to clean the surface of the graphite felt electrode and place it in a microwave sintering furnace with microwave heat treatment.
本发明所述一种液流电池石墨毡电极烧结改性处理方法，其特征在于：所述将石墨毡电极表面清理干净后放在微波烧结炉内用微波加热处理，是将石墨毡电极中心置于微波烧结炉的微波中心加热处理。The method for sintering and modifying the graphite felt electrode of the liquid flow battery according to the present invention is characterized in that: after the surface of the graphite felt electrode is cleaned, it is placed in a microwave sintering furnace for microwave heating treatment, and the center of the graphite felt electrode is placed Heat treatment in the microwave center of the microwave sintering furnace.
本发明所述一种液流电池石墨毡电极烧结改性处理方法，其特征在于：所述将石墨毡电极中心置于微波烧结炉的微波中心，是将石墨毡电极置于微波烧结炉内的碳化硅坩埚中，碳化硅坩埚外用保温棉包裹，碳化硅坩埚置于微波烧结炉的微波中心加热处理。The method for sintering and modifying the graphite felt electrode of the liquid flow battery according to the present invention is characterized in that: the center of the graphite felt electrode is placed in the microwave center of the microwave sintering furnace, and the graphite felt electrode is placed in the microwave sintering furnace In the silicon carbide crucible, the silicon carbide crucible is wrapped with thermal insulation cotton, and the silicon carbide crucible is placed in the microwave center of the microwave sintering furnace for heating.
本发明所述一种液流电池石墨毡电极烧结改性处理方法，其特征在于：所述微波加热处理的温度为300℃-500℃，加热处理时间为5-30min。The method for sintering and modifying the graphite felt electrode of the liquid flow battery according to the present invention is characterized in that: the temperature of the microwave heating treatment is 300°C-500°C, and the heating treatment time is 5-30min.
微波加热过程中，石墨毡纤维表面发生脱羧反应和脂肪链的氧化降解反应，使石墨毡纤维产生点蚀及水的分解析氧反应，产生“氧化剥离”效应使石墨毡纤维表面出现片状剥蚀，石墨毡纤维表面的片状剥蚀现象随加热时间延长而加剧。微波加热处理后，石墨毡表面的有益于电化学反应的官能团的含量有所增加，可提高石墨毡电极电化学活性。During the microwave heating process, the decarboxylation reaction and the oxidative degradation reaction of the fatty chain occur on the surface of the graphite felt fiber, which causes pitting corrosion of the graphite felt fiber and the decomposition and oxygenation reaction of water, resulting in an "oxidative peeling" effect that causes flake erosion on the surface of the graphite felt fiber , the exfoliation phenomenon on the surface of graphite felt fibers intensifies with the heating time prolonging. After microwave heating treatment, the content of functional groups on the surface of graphite felt that is beneficial to electrochemical reactions increases, which can improve the electrochemical activity of graphite felt electrodes.
本发明的有益效果是：本发明的石墨毡电极处理方法，可提高石墨毡电极电化学活性，能大大缩短处理时间，降低成本，是一种新型石墨毡电极提高电化学活性的表面改性方法。The beneficial effects of the present invention are: the graphite felt electrode treatment method of the present invention can improve the electrochemical activity of the graphite felt electrode, can greatly shorten the processing time and reduce the cost, and is a new surface modification method for the graphite felt electrode to improve the electrochemical activity .
附图说明Description of drawings
图1是常规热处理方法处理的石墨毡表面SEM扫描图Figure 1 is a SEM scan of the surface of graphite felt treated by conventional heat treatment methods
图2是微波热处理方法处理的石墨毡表面SEM扫描图Fig. 2 is the SEM scanning picture of the graphite felt surface processed by microwave heat treatment method
图3是常规热处理处理方法处理的石墨毡电极与用微波热处理方法处理的石墨毡电极的循环伏安比较图Fig. 3 is the comparison chart of cyclic voltammetry between graphite felt electrode processed by conventional heat treatment method and graphite felt electrode processed by microwave heat treatment method
图4是常规热处理方法处理的石墨毡电极与微波热处理方法处理的石墨毡电极的充放电性能比较图Figure 4 is a comparison chart of the charging and discharging performance of the graphite felt electrode treated by the conventional heat treatment method and the graphite felt electrode treated by the microwave heat treatment method
图3中，实线表示用常规热处理方法处理的石墨毡电极的循环伏安曲线，虚线表示用本发明的微波热处理方法处理的石墨毡电极的循环伏安曲线，图4中，方形点曲线是用微波热处理方法处理的石墨毡电极的放电性能曲线，菱形点曲线是用微波热处理方法处理的石墨毡电极的充电性能曲线，正三角形点曲线是常规热处理方法处理的石墨毡电极的放电性能曲线，倒三角形点曲线是常规热处理方法处理的石墨毡电极的放电性能曲线。Among Fig. 3, solid line represents the cyclic voltammetry curve of the graphite felt electrode processed with conventional heat treatment method, and dotted line represents the cyclic voltammetry curve of the graphite felt electrode processed with microwave heat treatment method of the present invention, and among Fig. 4, square point curve is The discharge performance curve of the graphite felt electrode processed by the microwave heat treatment method, the rhombus point curve is the charge performance curve of the graphite felt electrode processed by the microwave heat treatment method, and the regular triangle point curve is the discharge performance curve of the graphite felt electrode processed by the conventional heat treatment method, The inverted triangle point curve is the discharge performance curve of the graphite felt electrode treated by the conventional heat treatment method.
具体实施方式Detailed ways
以下结合实施例对本发明做进一步说明书。Below in conjunction with embodiment the present invention is described further.
将3mm厚4*7平方厘米的石墨毡表面清理干净后，放入微波烧结炉内的碳化硅坩埚中，碳化硅坩埚外用保温棉包裹，碳化硅坩埚处于微波烧结炉的微波中心；关闭炉门，并使炉门密封，防止微波泄漏；设定微波加热温度为400℃，加热时间为15min，接通电源加热处理，按设定加热温度和加热时间加热处理完后取出，得到经过微波加热改性的石墨毡。After cleaning the surface of graphite felt with a thickness of 3mm and 4*7 square centimeters, put it into the silicon carbide crucible in the microwave sintering furnace. The silicon carbide crucible is wrapped with thermal insulation cotton. The silicon carbide crucible is in the microwave center of the microwave sintering furnace; , and seal the furnace door to prevent microwave leakage; set the microwave heating temperature to 400°C, and the heating time to 15 minutes, turn on the power supply for heating treatment, take it out after heating treatment according to the set heating temperature and heating time, and obtain the modified microwave oven. permanent graphite felt.
将该微波处理过的石墨毡裁成0.3*1*7立方厘米和0.3*3*4立方厘米的石墨毡电极各一片，另取常规热处理30小时的同样的的石墨毡电极进行性能对比测试：Cut the microwave-treated graphite felt into 0.3*1*7 cubic centimeters and 0.3*3*4 cubic centimeters graphite felt electrode, and take the same graphite felt electrode that has been conventionally heat-treated for 30 hours for performance comparison test:
用0.3*1*7立方厘米电极作循环伏安测试，将0.3*1*7立方厘米电极用石蜡封样，尺寸为0.3*1*1立方厘米，循环伏安测试采用经典三电极体系，以Pt片作为对电极，饱和甘汞电极作为参比电极，封样后的石墨毡作为工作电极，用带有鲁金毛细管的盐桥连接参比电极和工作电极。循环伏安扫描速率为2mV/s,扫描电压范围为0～1.6V。测试结果如图3，测试结果表明，常规热处理石墨毡电极的氧化峰、还原峰电流密度分别为62mA/cm2、46mA/cm2；经微波加热处理的石墨毡电极氧化峰、还原峰电流密度为120mA/cm2、82mA/cm2，皆大于常规热处理法处理石墨毡电极，数据分析可知：经微波加热处理的石墨毡电极的电化学反应速度更快，与常规热处理石墨毡相比体现了更好的动力学性能。A 0.3*1*7 cubic centimeter electrode is used for cyclic voltammetry test. The 0.3*1*7 cubic centimeter electrode is sealed with paraffin, and the size is 0.3*1*1 cubic centimeter. The cyclic voltammetry test adopts the classic three-electrode system, with The Pt sheet was used as the counter electrode, the saturated calomel electrode was used as the reference electrode, the sealed graphite felt was used as the working electrode, and the reference electrode and the working electrode were connected by a salt bridge with a Lukin capillary. The scanning rate of cyclic voltammetry was 2mV/s, and the scanning voltage range was 0-1.6V. The test results are shown in Figure 3. The test results show that the oxidation peak and reduction peak current densities of conventional heat-treated graphite felt electrodes are 62mA/cm 2 and 46mA/cm 2 respectively; the oxidation peak and reduction peak current densities of graphite felt electrodes treated by microwave heating It is 120mA/cm 2 and 82mA/cm 2 , both of which are greater than the graphite felt electrode treated by the conventional heat treatment method. According to the data analysis, the electrochemical reaction speed of the graphite felt electrode treated by microwave heating is faster, which reflects that compared with the conventional heat treatment graphite felt Better dynamic performance.
用0.3*3*4立方厘米石墨毡电极组装氢气-金属电对液流电池单电池，在室温条件下进行充放电性能测试，电解液为0.5mol/LVOSO4与3mol/LH2SO4的混合溶液，采用Nafion212膜分隔电池正负两极，比较两种电极的充放电性能。测试结果表明：在相同电流密度下，微波加热处理方法处理的石墨毡电极比常规热处理方法处理的石墨毡电极放电电压更高，充电电压更低，微波加热处理方法处理的石墨毡电极性能明显优于常规热处理方法处理的石墨毡电极性能。Use 0.3*3*4 cubic centimeter graphite felt electrodes to assemble hydrogen-metal counterflow battery cells, and conduct charge and discharge performance tests at room temperature. The electrolyte is a mixture of 0.5mol/LVOSO 4 and 3mol/LH 2 SO 4 Solution, using Nafion212 membrane to separate the positive and negative poles of the battery, and compare the charge and discharge performance of the two electrodes. The test results show that: under the same current density, the graphite felt electrode treated by microwave heating treatment method has higher discharge voltage and lower charging voltage than graphite felt electrode treated by conventional heat treatment method, and the performance of graphite felt electrode treated by microwave heating treatment method is obviously better. Electrode properties of graphite felt treated by conventional heat treatment methods.
由常规热处理石墨毡和微波加热处理石墨毡表面SEM扫描图中可以看出：经常规热处理的石墨毡表面有一些细小的、平行于纤维轴向的刻蚀、沟槽等缺陷。而微波加热处理的石墨毡表面刻蚀加剧，沟槽变深。It can be seen from the SEM scanning images of the conventional heat-treated graphite felt and the microwave-heated graphite felt surface that there are some small defects such as etching and grooves parallel to the fiber axis on the surface of the conventional heat-treated graphite felt. However, the surface etching of the graphite felt treated by microwave heating is intensified, and the grooves become deeper.
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