CN107146899A - Surface coating structure and preparation of stainless steel bipolar plates for proton exchange membrane fuel cells - Google Patents
Surface coating structure and preparation of stainless steel bipolar plates for proton exchange membrane fuel cells Download PDFInfo
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- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 36
- 239000010935 stainless steel Substances 0.000 title claims abstract description 36
- 239000000446 fuel Substances 0.000 title claims abstract description 18
- 239000012528 membrane Substances 0.000 title claims abstract description 16
- 239000011248 coating agent Substances 0.000 title claims description 15
- 238000000576 coating method Methods 0.000 title claims description 15
- 238000002360 preparation method Methods 0.000 title claims description 3
- 239000000463 material Substances 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000007733 ion plating Methods 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 150000004767 nitrides Chemical class 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 11
- 230000007797 corrosion Effects 0.000 abstract description 11
- 238000005260 corrosion Methods 0.000 abstract description 11
- 229910052799 carbon Inorganic materials 0.000 abstract description 9
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract 1
- 238000002715 modification method Methods 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0223—Composites
- H01M8/0228—Composites in the form of layered or coated products
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fuel Cell (AREA)
Abstract
本发明涉及质子交换膜燃料电池领域中一种金属双极板表面新型改性方法。这种改性双极板由基体不锈钢和表面改性层两部分组成，改性层通过离子镀方法沉积于基体不锈钢表面，并分为基层、中间层和最外层三部分。本发明能够提高基体不锈钢的耐腐蚀性能，降低双极板与扩散层材料(碳纸)的接触电阻，能用冲压等方式对其进行加工，用其组装的电堆质量比功率和体积比功率得到提高。The invention relates to a novel modification method for the surface of a metal bipolar plate in the field of proton exchange membrane fuel cells. This modified bipolar plate consists of two parts: base stainless steel and surface modification layer. The modification layer is deposited on the surface of base stainless steel by ion plating, and is divided into three parts: the base layer, the middle layer and the outermost layer. The invention can improve the corrosion resistance of the base stainless steel, reduce the contact resistance between the bipolar plate and the diffusion layer material (carbon paper), process it by stamping and other methods, and use it to assemble the mass specific power and volume specific power of the stack get improved.
Description
技术领域technical field
本发明涉及一种质子交换膜燃料电池技术领域中不锈钢双极板表面改性方法。The invention relates to a method for modifying the surface of a stainless steel bipolar plate in the technical field of proton exchange membrane fuel cells.
背景技术Background technique
质子交换膜燃料电池(PEMFC)是一种清洁的能量转换装置，将储存在氢气和氧气中的化学能转化为电能，产物只有水。质子交换膜燃料电池因为其环境友好性、高的能量转化效率和快速启动性能等特点而备受关注。此外，其在汽车工业、备用应急电源、分散电站及军事等领域具有广阔的应用前景。A proton exchange membrane fuel cell (PEMFC) is a clean energy conversion device that converts chemical energy stored in hydrogen and oxygen into electricity with only water as the product. Proton exchange membrane fuel cells have attracted much attention because of their environmental friendliness, high energy conversion efficiency and fast start-up performance. In addition, it has broad application prospects in the fields of automobile industry, backup emergency power supply, distributed power station and military affairs.
双极板是质子交换膜燃料电池的关键部件之一，具有连接单池、支撑电堆、提供气体流场、收集电流、散热、排水等作用，因此，要求作为双极板的材料应该具有机械强度高、渗气率低、电导率高、导热性好、耐腐蚀、与碳纸之间的接触电阻低、低成本等性质。The bipolar plate is one of the key components of the proton exchange membrane fuel cell. It has the functions of connecting the single cell, supporting the stack, providing a gas flow field, collecting current, dissipating heat, and draining water. Therefore, the material required for the bipolar plate should have mechanical properties. High strength, low gas permeability, high electrical conductivity, good thermal conductivity, corrosion resistance, low contact resistance with carbon paper, and low cost.
在移动式应用方面，要求PEMFC电堆具有较高的质量比功率和体积比功率，但在传统PEMFC电堆中，石墨为制作双极板的主要材料，由于石墨气密性不佳、机械强度低、脆性大等问题，造成传统双极板厚度大、质量重、不耐机械震动、加工难度大、成本高，使得石墨在移动式应用中受限。金属具有较高的电导率、较好的机械强度、透气率低、导热性好、成本低、可进行冲压加工等特点，是制作双极板的潜在材料之一，但不锈钢等金属表面存在几纳米厚的氧化钝化膜，使得金属与碳纸间的接触电阻过大，进而造成电池内部较大的欧姆阻抗，这将显著降低不锈钢等金属作为双极板时，电堆的输出性能。因此，不锈钢等金属制作的双极板表面必须进行适当的改性处理。目前很多研究者在基体不锈钢表面沉积TiN镀层，这显著降低了不锈钢与碳纸之间的接触电阻，但TiN镀层稳定性较差。Ho-Young Jung在钛板表面制备了1μm的金镀层，阻止了钝化层的形成，电池性能较好，但是金的价格昂贵，难以实现大规模商业化应用。B.Yang通过热氮化在不锈钢表面制备了Cr的氮化物，但膜不连续，对基体的保护性较差。在金属双极板表面制备致密、耐腐蚀、导电性好并且与碳纸间接触电阻小的改性涂层，则可以提高基体金属的耐蚀性，降低质子交换膜燃料电池电堆的内阻，提高电堆输出性能。In mobile applications, PEMFC stacks are required to have high mass specific power and volume specific power, but in traditional PEMFC stacks, graphite is the main material for making bipolar plates. The traditional bipolar plate is thick, heavy, not resistant to mechanical vibration, difficult to process, and high in cost due to problems such as low density and high brittleness, which limit the use of graphite in mobile applications. Metal has the characteristics of high electrical conductivity, good mechanical strength, low air permeability, good thermal conductivity, low cost, and can be stamped. It is one of the potential materials for making bipolar plates. The nanometer-thick oxide passivation film makes the contact resistance between the metal and the carbon paper too large, which in turn causes a large ohmic impedance inside the battery, which will significantly reduce the output performance of the stack when metals such as stainless steel are used as bipolar plates. Therefore, the surface of bipolar plates made of metals such as stainless steel must be properly modified. At present, many researchers deposit TiN coating on the surface of base stainless steel, which significantly reduces the contact resistance between stainless steel and carbon paper, but the stability of TiN coating is poor. Ho-Young Jung prepared a 1 μm gold coating on the surface of the titanium plate, which prevented the formation of a passivation layer, and the battery performance was good. However, gold is expensive and difficult to achieve large-scale commercial applications. B. Yang prepared Cr nitrides on the surface of stainless steel by thermal nitriding, but the film was discontinuous and the protection of the substrate was poor. Prepare a modified coating on the surface of the metal bipolar plate that is dense, corrosion-resistant, good in conductivity, and has low contact resistance with carbon paper, which can improve the corrosion resistance of the base metal and reduce the internal resistance of the proton exchange membrane fuel cell stack. , improve the output performance of the stack.
发明内容Contents of the invention
本发明的目的在于针对现有质子交换膜燃料电池不锈钢双极板表面改性技术的不足，提供一种质子交换膜燃料电池不锈钢双极板的表面涂层结构的制备方法，在降低极板与碳纸之间接触电阻的同时，提高其耐腐蚀性，满足质子交换燃料电池高质量比功率和高体积比功率的发展要求。The object of the present invention is to aim at the deficiencies in the surface modification technology of the stainless steel bipolar plate of the existing proton exchange membrane fuel cell, to provide a kind of preparation method of the surface coating structure of the stainless steel bipolar plate of the proton exchange membrane fuel cell, in reducing the polar plate and While increasing the contact resistance between carbon papers, it improves its corrosion resistance and meets the development requirements of high-quality specific power and high volume specific power of proton exchange fuel cells.
本发明通过以下技术方案实现：不锈钢基材经机械打磨后，进行超声清洗，然后在基材表面通过离子镀方法沉积由基层、中间层和最外层组成的多层涂层结构的改性层，获得表面改性的燃料电池不锈钢双极板。The present invention is realized through the following technical scheme: after the stainless steel substrate is mechanically polished, ultrasonic cleaning is performed, and then a modified layer of a multi-layer coating structure composed of a base layer, an intermediate layer and an outermost layer is deposited on the surface of the substrate by ion plating , to obtain surface-modified stainless steel bipolar plates for fuel cells.
所述不锈钢基材，其厚度为0.05mm～1mm。The stainless steel base material has a thickness of 0.05 mm to 1 mm.
所述机械打磨，其所用砂纸为600目～2500目。For the mechanical grinding, the sandpaper used is 600 mesh to 2500 mesh.
所述基层，其为Ti、Ni、Cu、Au、Ag中的一种或二种以上。The base layer is one or more of Ti, Ni, Cu, Au and Ag.
所述中间层，其为Cr、Al、V、Co、Pt中的一种或二种以上。The intermediate layer is one or two or more of Cr, Al, V, Co, and Pt.
所述最外层，其为Cr、Ti、Ni、Al、V中的一种或多种的氮化物。The outermost layer is one or more nitrides of Cr, Ti, Ni, Al, V.
所述离子镀，其真空度为1×10-2Pa～10Pa。The vacuum degree of the ion plating is 1×10 -2 Pa～10Pa.
所述离子镀，其沉积电流为20A～120A。The ion plating has a deposition current of 20A-120A.
所述离子镀，其沉积时间总共为10min～200min。The deposition time of the ion plating is 10 minutes to 200 minutes in total.
所述基层、中间层和最外层，其厚度分别在10nm～1μm、10nm～1μm和100nm～30μm之间。The thicknesses of the base layer, middle layer and outermost layer are respectively between 10nm-1μm, 10nm-1μm and 100nm-30μm.
本发明选择的不锈钢厚度为0.05mm～1mm，由于不锈钢的机械加工性能较好，用此种方法改性的双极板可采用较成熟的金属板加工工艺进行流场等部件的加工。基层金属具有较好的耐局部腐蚀能力，起到阻隔局部腐蚀的作用。中间层金属与最外层所用金属晶格常数相近，能有效缓解涂层的应力，提高最外层的耐久性。最外层具有电阻率低、耐腐蚀、与碳纸之间接触电阻小等特性。150牛顿每平方厘米压紧力下，316L不锈钢的接触电阻为421毫欧姆平方厘米，而改性样品的接触电阻可降低到4.2毫欧姆平方厘米。0.5摩尔每升硫酸溶液中，316L不锈钢的腐蚀电流为177.8微安每平方厘米，而改性样品的腐蚀电流为0.18微安每平方厘米。改性层显著降低了不锈钢与碳纸间的接触电阻和腐蚀电流。此外，改性层价格较低而且易得，适合大规模应用，可降低质子交换膜燃料电池的成本。The thickness of the stainless steel selected in the present invention is 0.05 mm to 1 mm. Due to the good machining performance of stainless steel, the bipolar plate modified by this method can be processed by relatively mature metal plate processing technology for flow field and other components. The base metal has good local corrosion resistance and plays a role in blocking local corrosion. The metal in the middle layer is similar to the lattice constant of the metal used in the outermost layer, which can effectively relieve the stress of the coating and improve the durability of the outermost layer. The outermost layer has the characteristics of low resistivity, corrosion resistance, and small contact resistance with carbon paper. Under the compression force of 150 Newtons per square centimeter, the contact resistance of 316L stainless steel is 421 milliohm square centimeters, while the contact resistance of the modified sample can be reduced to 4.2 milliohm square centimeters. In 0.5 moles per liter of sulfuric acid solution, the corrosion current of 316L stainless steel is 177.8 microamps per square centimeter, while the corrosion current of the modified sample is 0.18 microamps per square centimeter. The modified layer significantly reduces the contact resistance and corrosion current between stainless steel and carbon paper. In addition, the modified layer is cheap and easy to obtain, suitable for large-scale application, and can reduce the cost of proton exchange membrane fuel cells.
附图说明Description of drawings
图1是实施例1表面改性样品和316L不锈钢与碳纸之间接触电阻随压力变化的示意图。Fig. 1 is a schematic diagram of the change of contact resistance with pressure between the surface modified sample of Example 1 and 316L stainless steel and carbon paper.
图2是实施例1表面改性样品和316L不锈钢在0.5摩尔每升硫酸溶液中的极化曲线示意图。Fig. 2 is a schematic diagram of the polarization curves of the surface modified sample in Example 1 and 316L stainless steel in 0.5 moles per liter of sulfuric acid solution.
图3是本发明实施例1的扫描电子显微镜图。Fig. 3 is a scanning electron microscope image of Example 1 of the present invention.
具体实施方式detailed description
下面结合附图对本发明的实施例作详细说明：本实施例在以本发明技术方案为前提下进行实施，但本发明的内容不仅仅局限于下面的实施例。The embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings: this embodiment is implemented on the premise of the technical solution of the present invention, but the content of the present invention is not limited to the following embodiments.
实施例1：Example 1:
取0.1mm厚的316L不锈钢板，裁剪为100mm×150mm的基材，用600目～2000目砂纸逐级打磨；用丙酮和水超声清洗30min；抽真空至1×10-3Pa～1×10-2Pa，充入氩气调节压力为0.8Pa～1.2Pa之间，沉积Ti基层，电流60A，时间10min。关闭Ti靶，开启Cr靶，沉积中间层，电流60A，时间10min。通入氮气，调整压力为1Pa～1.5Pa之间，沉积最外层，靶电流60A，时间40min。实施例2：Take a 0.1mm thick 316L stainless steel plate, cut it into a substrate of 100mm×150mm, and polish it step by step with 600-2000-grit sandpaper; ultrasonically clean it with acetone and water for 30 minutes; vacuumize to 1×10 -3 Pa～1×10 -2 Pa, filled with argon gas to adjust the pressure between 0.8Pa and 1.2Pa, deposit the Ti base layer, current 60A, time 10min. Turn off the Ti target, turn on the Cr target, deposit the intermediate layer, the current is 60A, and the time is 10min. Introduce nitrogen, adjust the pressure between 1Pa and 1.5Pa, deposit the outermost layer, the target current is 60A, and the time is 40min. Example 2:
取0.5mm厚的316L不锈钢板，裁剪为100mm×150mm的基材，用600目～2000目砂纸逐级打磨；用丙酮和水超声清洗30min；抽真空至3×10-3Pa～7×10-3Pa，充入氩气调节压力为0.8Pa～1.1Pa之间，沉积Cu基层，电流70A，时间15min。关闭Cu靶，开启V靶，沉积中间层，电流70A，时间10min。关闭V靶，通入氮气调整压力为1Pa～1.3Pa之间，开启Ti靶，沉积最外层，电流65A，时间35min。Take a 0.5mm thick 316L stainless steel plate, cut it into a substrate of 100mm×150mm, and polish it step by step with 600-2000-mesh sandpaper; ultrasonically clean it with acetone and water for 30 minutes; vacuumize to 3×10 -3 Pa～7×10 -3 Pa, filled with argon gas to adjust the pressure between 0.8Pa and 1.1Pa, deposit Cu base layer, current 70A, time 15min. Turn off the Cu target, turn on the V target, deposit the intermediate layer, the current is 70A, and the time is 10min. Close the V target, feed nitrogen to adjust the pressure between 1Pa and 1.3Pa, open the Ti target, and deposit the outermost layer with a current of 65A and a time of 35min.
实施例3：Example 3:
取1mm厚的316L不锈钢板，裁剪为100mm×150mm的基材，用600目～2000目砂纸逐级打磨；用丙酮和水超声清洗30min；抽真空至5×10-3Pa～9×10-3Pa，充入氩气调节压力为1.5Pa～1.9Pa之间，沉积Ag过渡层，电流60A，时间15min。关闭Ag靶，开启Al靶，沉积中间层，电流100A，时间10min。关闭Al靶，通入氮气调整压力为1.6Pa～1.9Pa之间，开启V靶，沉积最外层，电流100A，时间30min。Take a 1mm thick 316L stainless steel plate, cut it into a substrate of 100mm×150mm, and polish it step by step with 600-2000-grit sandpaper; ultrasonically clean it with acetone and water for 30 minutes; vacuumize to 5×10 -3 Pa～9×10 - 3 Pa, filled with argon gas to adjust the pressure between 1.5Pa and 1.9Pa, deposit Ag transition layer, current 60A, time 15min. Turn off the Ag target, turn on the Al target, deposit the intermediate layer, the current is 100A, and the time is 10min. Close the Al target, feed nitrogen gas to adjust the pressure between 1.6Pa and 1.9Pa, open the V target, and deposit the outermost layer with a current of 100A for 30 minutes.
本发明工艺参数上下限取值都可能实现本发明，在此不一一列举实施例。Both the upper and lower limits of the process parameters in the present invention may realize the present invention, and the embodiments are not listed here one by one.
Claims (6)
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