CN110875481B - Method for modifying PEMFC stainless steel bipolar plate through constant-current electrochemical nitridation - Google Patents
Method for modifying PEMFC stainless steel bipolar plate through constant-current electrochemical nitridation Download PDFInfo
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- CN110875481B CN110875481B CN201811027969.2A CN201811027969A CN110875481B CN 110875481 B CN110875481 B CN 110875481B CN 201811027969 A CN201811027969 A CN 201811027969A CN 110875481 B CN110875481 B CN 110875481B
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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
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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- 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
Abstract
A method for constant-current electrochemical nitridation modification of a PEMFC stainless steel bipolar plate belongs to the field of fuel cells. The method is characterized in that: a. electrochemical polishing removal of surfaces from commercial stainless steelsCleaning an oxidation layer and the processed steel sheet by using deionized water, and drying in a drying box for later use; b. preparing a mixed solution of nitrate (such as potassium nitrate, sodium nitrate and the like) and potassium hydroxide with a certain concentration, and controlling the pH value of the solution to be 7-14. c. A three-electrode system is used for constant-current electrochemical nitridation treatment, wherein stainless steel is used as a working electrode, a platinum sheet is used as a counter electrode, a saturated calomel electrode is used as the counter electrode, and the current density is 1-50 mA/cm 2 The time is 0.5 h-8 h, and the treatment temperature is 30-50 ℃. d. And cleaning the treated stainless steel sample by using deionized water, and drying by using a blower. The test result shows that the corrosion and conductivity of the stainless steel bipolar plate after the constant-current electrochemical nitridation treatment can meet the requirements of the fuel cell on the performance of the bipolar plate.
Description
Technical Field
The invention belongs to the technical field of fuel cells, relates to a modification method of a PEMFC stainless steel bipolar plate, and particularly relates to a method for manufacturing a PEMFC bipolar plate by performing constant-current electrochemical nitridation treatment on stainless steel by using an alkaline nitrate solution.
Background
The limited reserves of fossil energy and the environmental pollution problems that arise during the utilization of fossil energy have led to the research of clean energy utilization. One must find a way to utilize this capability that is different from the current direct combustion availability. A Proton Exchange Membrane Fuel Cell (PEMFC) is a power generation device that directly converts chemical energy in fuel into electrical energy using an electrochemical reaction process. The energy conversion efficiency is up to more than 80 percent without the limit of Carnot cycle because the energy conversion process does not pass through the combustion process of the traditional internal combustion engine, and the emission of polluting gases is avoided. In particular, in recent years, fuel cell technology has been the focus of research and has made a great breakthrough. At the same time, it is an environmentally friendly, fast-starting, low-noise energy conversion device with little emissions of nitrogen and sulfur oxides at room temperature. Due to the outstanding physical and chemical properties, research and development of fuel cell technology are paid high attention by governments and large companies of various countries, and the fuel cell technology is likely to be used in the fields of mobile power supplies, standby power supplies, power supplies and the like in the future, is considered as a preferred clean and efficient power source in the 21 st century, and has great development potential.
The wide spread use of fuel cells at present still presents problems, in particular problems of cost and of lifetime. These have severely limited the development and application of fuel cell technology. The bipolar plate serves as a key component in the fuel cell, and the manufacturing cost and the service life directly determine the large-scale commercial application of the fuel cell. At present, the PEMFC bipolar plate is mainly made of graphite and composite materials or metal materials thereof, and various aspects, particularly the factors of the electrical conductivity, the corrosion resistance, the volume, the processing performance, the cost and the like of the material must be comprehensively considered for the selection of the material according to the functions and the characteristics of the bipolar plate. Bipolar Plates (also called current collector Plates) are the skeletons of fuel cells, and are stacked with MEAs to form a cell stack, which is one of the key components of PEMFC stacks. The mass of the bipolar plate accounts for 60-80% of the total cell stack, the processing cost accounts for 45% of the total cell cost, and the bipolar plate is one of important factors for restricting the commercial production of the PEMFC, so that the development and research of the bipolar plate with low cost and excellent performance have important significance.
Metal materials are potential materials for manufacturing bipolar plates due to the advantages of excellent toughness, electrical and thermal conductivity, compactness, capability of being manufactured into very thin plates and the like. At present, metal bipolar plates, particularly stainless steel and the like, are receiving wide attention. The PEMFC operates in an acidic, high-temperature and high-humidity environment, an aqueous solution often contains fluoride ions which can easily cause stainless steel pitting, the voltage difference between a cathode and an anode can reach more than 1.0V at the maximum when the PEMFC is started, under the severe service condition, common metal materials can be seriously corroded, stainless steel bipolar plates can be corroded generally, and the service life of the metal bipolar plates is shortened. In addition, a passivating film with poor conductivity formed on the surface of the stainless steel in an acidic and oxidative environment increases the contact resistance between the bipolar plate and the carbon paper, reduces the output power of the battery, and is not convenient for thermal management of the battery.
The main problems faced by the application of metallic bipolar plates are to solve the problems of corrosion phenomena in the range of operating potentials on the anode side of the cell and of increased contact resistance due to oxidation during operation on the cathode side. The metal corrosion process not only damages the bipolar plate structure, but also reduces the performance of the battery because metal ions generated by corrosion pollute the electrolyte membrane. Therefore, one of the key technologies for using metal materials as PEMFC bipolar plates is surface modification of metals, which reduces contact resistance and improves anode metal corrosion resistance by forming a corrosion-resistant coating with good conductivity on the surface. A number of surface modification techniques have been used to improve the corrosion resistance and electrical conductivity of stainless steels. Nitriding is the formation of metal nitrides on metal surfaces to improve the mechanical properties and corrosion resistance of the substrate material. Through various chemical reactions, chromium nitride, chromium carbide, titanium nitride and other coatings with excellent conductive and corrosion resistant properties can be prepared on the surface of stainless steel, and the requirements of fuel cells on the performance of the bipolar plate are met. However, the kinetics of the nitridation reaction process is slow, and the process generally takes a long time (about 8-16 h) to react at high temperature (usually more than 550 ℃) to form a nitrided layer. And the properties of the base material can also change in the high-temperature process, which affects the properties of the final product.
The current methods for preparing the coatings on the surface of the stainless steel mainly comprise the following steps: high temperature Physical Vapor Deposition (PVD), nitrogen ion implantation, and gas nitriding, among others. The stainless steel modified by the advanced nitriding treatment method forms a metal nitride coating with excellent conductivity and corrosion resistance on the surface, but the nitriding treatment cost of the stainless steel surface is high, the commercialization of a fuel cell is seriously hindered, and the modified bipolar plate material can generate damage phenomena such as pitting corrosion after long-time operation. Therefore, the development of a simple, efficient and low-cost nitridation treatment method instead of the conventional high-energy-consumption nitridation process is forced. The research shows that the stainless steel can form a nano-scale nitride layer on the surface after being subjected to electrochemical treatment in a nitrate solution, the nitride layer is compact and has no defects, and the performance can reach the effect after the current thermal nitriding treatment. Electrochemical nitridation, a low-temperature nitridation process, is promising to greatly reduce the manufacturing cost of stainless steel metal bipolar plates and promote the development of fuel cell technologies.
Disclosure of Invention
1. The invention provides a method for modifying a PEMFC stainless steel bipolar plate by constant-current electrochemical nitridation, which can be used for preparing the stainless steel bipolar plate with excellent performance in batch, high efficiency and low cost and is easy to realize the low-cost mass production of the metal bipolar plate.
In order to achieve the purpose, the invention adopts the following technical scheme, which comprises the following specific steps:
(1) Pretreatment of commercial stainless steel:
in order to remove the passive film formed on the surface of commercial stainless steel and to smooth the surface of stainless steel, stainless steel was electrochemically polished. The electrochemical polishing solution consists of citric acid, phosphoric acid, sulfuric acid and additive, and is washed by deionized water and dried at room temperature after being polished in a constant-current mode.
(2) Preparing a constant-current electrochemical nitriding solution:
the electrochemical nitriding solution of the stainless steel bipolar plate consists of alkaline nitrate and an additive, and the solution controls a proper pH value.
(3) Constant-current electrochemical nitriding connecting device:
and (3) placing the stainless steel with the bright and flat surface obtained in the step (1) in the alkaline nitrate solution prepared in the step (2), maintaining the process temperature to be higher than room temperature (25 ℃), and performing electrochemical treatment by using a three-electrode system, wherein the stainless steel is used as a working electrode, a platinum sheet is used as a counter electrode, and a Saturated Calomel Electrode (SCE) is used as the counter electrode.
(4) Constant-current electrochemical nitridation process of PEMFC stainless steel bipolar plate:
the constant-current electrochemical nitridation process is carried out in two sections, and the first section is kept stand in an open-circuit state; the second section is nitrided for a time at a selected current density. And cleaning the treated stainless steel sample by using deionized water, and then carrying out tests such as electrochemistry and the like by blow drying.
Further, the electrochemical polishing solution in the step (1) comprises 200mL/L of citric acid (1.5M) +650mL/L of phosphoric acid +100mL/L of sulfuric acid +20mL/L of glycerin +1.04g/L of urotropine +0.5g/L of saccharin. The urotropine and saccharin were dissolved in 25mL of hot water at 80 ℃ prior to addition and the above solutions were added together.
Further, in the step (2), the pH value of the solution is controlled to be between 7 and 14, and the concentration of nitrate is controlled to be 0.5 to 1.0M.
Furthermore, the additive in the step (2) is a surfactant such as sodium dodecyl benzene sulfonate and the like, and the concentration is 0.02g/L.
Further, the temperature of the solution in the step (3) is maintained at a temperature higher than room temperature, and is selected from 30 to 50 ℃ in order to reduce the difficulty in handling.
Further, the standing time in the step (3) is more than 10 minutes, and generally 25 to 35 minutes is selected.
Further, the current density of the second section of constant current nitridation in the step (3) is 1-50 mA/cm 2 The time of a certain constant current value is 0.5 h-8 h.
The innovation of the invention is that: after a dense and uniform modified layer is formed on the surface of the stainless steel in the alkaline nitrate solution through constant-current electrochemical nitridation, the corrosion resistance of the stainless steel is improved, and meanwhile, the contact resistance is obviously reduced compared with that of bare steel. The requirement of the fuel cell stack on the performance of the bipolar plate is achieved by a low-cost means. The test result shows that the performance of the stainless steel after constant-current electrochemical nitridation is almost the same as that of the sample after thermal nitridation treatment, but the treatment time and the treatment cost are obviously reduced. As a novel method for modifying the stainless steel bipolar plate, the constant-current electrochemical nitridation treatment is expected to greatly reduce the manufacturing cost of a fuel cell stack and accelerate the commercialization of the fuel cell.
Drawings
FIG. 1 is a potentiodynamic polarization plot of example 1 electrochemically nitrided modified 316L stainless steel and untreated bare steel;
FIG. 2 is a plot of potentiodynamic polarization of example 2 electrochemical nitriding modified 316L stainless steel and untreated bare steel;
FIG. 3 is a potentiodynamic polarization plot of example 3 electrochemically nitrided modified 316L stainless steel and untreated bare steel;
FIG. 4 is a surface SEM image of the 316L stainless steel and untreated bare steel after electrochemical nitriding modification of example 1;
FIG. 5 is a surface SEM image of the 316L stainless steel and untreated bare steel after electrochemical nitriding modification of example 2;
FIG. 6 is a surface SEM image of example 3 electrochemically nitrided modified 316L stainless steel and untreated bare steel;
Detailed Description
The technical scheme of the invention is further explained by the concrete examples and the attached drawings:
example one:
after electrochemical polishing, the stainless steel is subjected to ultrasonic treatment in alcohol by 30Min to remove grease on the surface, and then the stainless steel is cleaned by deionized water and dried by a blower for storage.
The solution for electrochemical nitriding of stainless steel consisted of a potassium nitrate solution, the pH was adjusted to 12 ± 0.5 with potassium hydroxide, and the potassium nitrate concentration was 0.5M. 10mL of a surfactant solution prepared from 0.02g/L sodium dodecylsulfamate is added dropwise into the solution. The solution temperature was maintained at 40. + -. 3 ℃. A three-electrode system is used for constant-current electrochemical nitridation treatment, wherein stainless steel is used as a working electrode, a platinum sheet is used as a counter electrode, and a Saturated Calomel Electrode (SCE) is used as the counter electrode. The electrochemical nitridation process is divided into two sections, wherein the first section is kept stand in an open-circuit state for 30Min; then selecting the current density of nitridation as 10mA/cm 2 And (4) carrying out nitridation modification, wherein the treatment time is 8h. And cleaning the treated stainless steel sample by using deionized water, and drying by using a blower for testing electrochemistry and the like.
Example two:
after electrochemical polishing, the stainless steel is subjected to ultrasonic treatment in alcohol by 30Min to remove grease on the surface, and then is cleaned by deionized water and dried by a blower for storage.
The solution for electrochemical nitriding of stainless steel consisted of a potassium nitrate solution, the pH was adjusted to 13 ± 0.5 with potassium hydroxide, the concentration of potassium nitrate being 1.0M. 10mL of a surfactant solution prepared from 0.02g/L sodium dodecylsulfamate is added dropwise into the solution. The solution temperature was maintained at 40. + -. 3 ℃. A three-electrode system is used for constant-current electrochemical nitridation treatment, wherein stainless steel is used as a working electrode, a platinum sheet is used as a counter electrode, and a Saturated Calomel Electrode (SCE) is used as the counter electrode. The electrochemical nitridation process is composed of two sections, the first section is placed still under open-circuit stateThe time period is 30Min; then selecting the current density of nitridation as 15mA/cm 2 And (4) carrying out nitridation modification, wherein the treatment time is 3h. And cleaning the treated stainless steel sample by using deionized water, and drying by using a blower for testing electrochemistry and the like.
Example three:
after electrochemical polishing, the stainless steel is subjected to ultrasonic treatment in alcohol by 30Min to remove grease on the surface, and then the stainless steel is cleaned by deionized water and dried by a blower for storage. The solution for electrochemical nitriding of stainless steel consisted of a potassium nitrate solution, the pH was adjusted to 14 ± 0.5 with potassium hydroxide, and the potassium nitrate concentration was 0.8M. 10mL of surfactant solution prepared from 0.02g/L sodium dodecyl sulfate is added into the solution dropwise. The solution temperature was maintained at 50. + -. 3 ℃. A three-electrode system is used for constant-current electrochemical nitridation treatment, wherein stainless steel is used as a working electrode, a platinum sheet is used as a counter electrode, and a Saturated Calomel Electrode (SCE) is used as the counter electrode. The electrochemical nitridation process is divided into two sections, wherein the first section is kept stand in an open-circuit state for 30Min; then, the nitridation current density is selected to be 20mA/cm < 2 > to carry out nitridation modification, and the treatment time is 1h. And cleaning the treated stainless steel sample by using deionized water, and then drying by using a blower for testing electrochemistry and the like.
The technical features in the above-mentioned examples can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above-mentioned embodiments are not described, however, as long as there is no contradiction between the combinations of the technical features, the scope of the present description should be considered as being described in the present specification.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
The above examples are merely illustrative of several embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention.
Claims (5)
1. A method for modifying a PEMFC stainless steel bipolar plate by constant-current electrochemical nitridation is characterized by comprising the following specific steps of:
(1) Pretreatment of commercial stainless steel:
in order to remove a passive film formed on the surface of the stainless steel and to level the surface of the stainless steel, performing electrochemical polishing on the stainless steel; the electrochemical polishing solution consists of citric acid, phosphoric acid, sulfuric acid and an additive, is polished in a constant-current mode, is washed by deionized water and is dried at room temperature;
(2) Preparing a constant-current electrochemical nitriding solution:
the electrochemical nitriding solution of the stainless steel bipolar plate consists of alkaline nitrate and an additive, and the proper pH value of the solution is controlled;
(3) Constant-current electrochemical nitriding connection device:
placing the stainless steel with the bright and flat surface obtained in the step (1) in the alkaline nitrate solution prepared in the step (2), maintaining the process temperature at a certain temperature higher than the room temperature by 25 ℃, and performing electrochemical treatment by using a three-electrode system, wherein the stainless steel is used as a working electrode, a platinum sheet is used as a counter electrode, and a Saturated Calomel Electrode (SCE) is used as the counter electrode;
(4) The constant-current electrochemical nitridation process of the PEMFC stainless steel bipolar plate comprises the following steps:
the constant-current electrochemical nitridation process is carried out in two sections, wherein the first section of stainless steel is kept standing in a solution under an open-circuit state; the second section is nitrided for a certain time under a certain current density; cleaning the treated stainless steel sample by using deionized water, and drying the stainless steel sample by blowing for electrochemical test;
the electrochemical polishing solution in the step (1) comprises 1.5M of 200mL/L citric acid, 650mL phosphoric acid, 100mL/L sulfuric acid, 20mL/L glycerin, 1.04g/L urotropin and 0.5g/L saccharin; dissolving urotropine and saccharin in 25mL hot water at 80 deg.C before adding 1.5M of 200mL/L citric acid +650mL phosphoric acid +100mL/L sulfuric acid +20mL/L glycerol, and finally adding 1.5M of a mixed solution of 200mL/L citric acid +650mL phosphoric acid +100mL/L sulfuric acid +20mL/L glycerol;
in the step (2), the pH value of the solution is controlled to be between 7 and 14, and the concentration of the nitrate is controlled to be 0.5 to 1.0M.
2. A method for constant current electrochemical nitridation modification of a PEMFC stainless steel bipolar plate according to claim 1, wherein the additive in step (2) is sodium dodecylbenzenesulfonate surfactant with a concentration of 0.02g/L.
3. A constant current electrochemical nitridation method of modified PEMFC stainless steel bipolar plate according to claim 1, wherein the temperature of the solution in step (3) is maintained at 30-50 ℃.
4. A constant current electrochemical nitridation method of modified PEMFC stainless steel bipolar plate according to claim 1, wherein the standing time in step (3) is 25-35 minutes.
5. The method for constant-current electrochemical nitridation modification of the PEMFC stainless steel bipolar plate according to claim 1, wherein the current density of the second constant-current nitridation section in the step (3) is 1-50 mA/cm 2 The time of a certain constant current value is 0.5 h-8 h.
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| WO2004070083A1 (en) * | 2003-02-07 | 2004-08-19 | Honda Motor Co., Ltd. | Method for passivating stainless steel product and method for producing stainless steel separator for fuel cell |
| WO2011109020A1 (en) * | 2010-03-03 | 2011-09-09 | Alliance For Sustainable Energy, Llc | Electrochemical nitridation of metal surfaces |
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