CN115491675A - Preparation method of titanium carbide coating on surface of metal bipolar plate of proton exchange membrane fuel cell - Google Patents
Preparation method of titanium carbide coating on surface of metal bipolar plate of proton exchange membrane fuel cell Download PDFInfo
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- CN115491675A CN115491675A CN202211157836.3A CN202211157836A CN115491675A CN 115491675 A CN115491675 A CN 115491675A CN 202211157836 A CN202211157836 A CN 202211157836A CN 115491675 A CN115491675 A CN 115491675A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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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
- H01M8/0206—Metals or alloys
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- H01M8/021—Alloys based on iron
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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
- H01M8/0215—Glass; Ceramic materials
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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
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- 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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Abstract
The invention discloses a preparation method of a titanium carbide coating on the surface of a metal bipolar plate of a proton exchange membrane fuel cell, which comprises the following steps: 1) Pretreatment of a base material: polishing and washing the stainless steel substrate; 2) Preparing an organic carbon solution: perylene-3, 4,9, 10-tetracarboxylic dianhydride (PTCDA), N-methylpyrrolidone (NMP), epoxy resin and methyltetrahydrophthalic anhydride are ultrasonically mixed to obtain an organic carbon solution; 3) And (3) heat treatment: putting stainless steel into an organic carbon solution, sequentially carrying out segmented heat treatment by using an oven and a tubular furnace, and continuously introducing inert gas into the tubular furnace for reaction to obtain a stainless steel substrate with an organic carbon film formed on the surface; 4) Preparing a TiC coating: putting the stainless steel obtained in the step 3) into a molten salt system in a molten salt crucible, then putting the molten salt system in a well type furnace, continuously introducing inert gas for reaction, and growing a TiC coating on the surface of the base material in the reaction process. The method has simple preparation process, and the obtained TiC coating is continuous and compact and is well combined with the matrix.
Description
Technical Field
The invention belongs to the technical field of metal material surface treatment, and particularly relates to a preparation method of a titanium carbide coating on the surface of a metal bipolar plate of a proton exchange membrane fuel cell.
Background
In recent years, due to the continuous combustion of fossil fuels and the aggravation of environmental pollution problems, people pay more and more attention to the development of low-carbon and clean energy. Meanwhile, proton Exchange Membrane Fuel Cells (PEMFCs) offer great advantages in transportation and application with the advantages of high energy efficiency and low emissions. The metal bipolar plate which is one of the key points in the PEMFC can bear various external loads under different environments, and simultaneously has the advantages of high toughness, easy processing and stability. However, in a long-term acidic environment of PEMFC, the metal bipolar plate forms a passivation film to protect the substrate, which is advantageous for its corrosion resistance, but disadvantageous for its electrical conductivity, and in turn, degrades the cell performance. And the passive film disappears after a long time operation, which deteriorates the long-term performance of the battery. For this reason, it is an economically efficient way to improve the durability of metallic bipolar plates in fuel cells by applying a corrosion-resistant, electrically conductive and hydrophobic coating to the surface thereof.
In previous studies, it was found that a transition metal ceramic coating such as TiC has good electrical conductivity, chemical stability and hydrophobicity, and is an excellent material as a surface protection of a metal bipolar plate. In recent years, there are many methods for preparing TiC coatings, such as Physical Vapor Deposition (PVD), chemical Vapor Deposition (CVD), etc., but all of them have many unavoidable microscopic defects, such as insufficient adhesion of the coating to the substrate, complex preparation process, and large consumable material.
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel method for preparing a titanium carbide coating on the surface of a metal bipolar plate of a proton exchange membrane fuel cell, which is simple in preparation process, firstly preparing an organic carbon layer on stainless steel by adopting segmented annealing treatment, and then preparing a TiC coating in molten salt by utilizing disproportionation reaction to finally obtain the TiC coating which is continuous and compact and has good combination with a matrix.
The invention solves the technical problems by the following technical scheme:
the invention relates to a preparation method of a titanium carbide coating on the surface of a metal bipolar plate of a proton exchange membrane fuel cell, which comprises the following operation steps:
1) Pretreatment of a base material: selecting stainless steel as a base material, and carrying out polishing and water washing pretreatment on the surface of the stainless steel to obtain a continuous flat and rough base material surface;
2) Preparing an organic carbon solution: firstly, mixing an organic carbon source of perylene-3, 4,9, 10-tetracarboxylic dianhydride (PTCDA) and N-methylpyrrolidone (NMP) serving as a solvent, uniformly dispersing the mixture by ultrasonic treatment, adding an epoxy resin and a methyl tetrahydrophthalic anhydride serving as a curing agent, and performing ultrasonic treatment again, wherein the perylene-3, 4,9, 10-tetracarboxylic dianhydride (PTCDA), the N-methylpyrrolidone (NMP), the epoxy resin and the methyl tetrahydrophthalic anhydride are configured according to a mass ratio of 1: 4: 2, and uniformly mixing the mixture by ultrasonic treatment to obtain an organic carbon solution;
3) And (3) heat treatment: putting the stainless steel substrate treated in the step 1) into the organic carbon solution in the step 2), then putting the stainless steel substrate into an oven for heat treatment at the temperature of 140 ℃ for 35min, and then putting the stainless steel substrate into a tubular furnace for segmented heat treatment, wherein inert gas is continuously introduced into the tubular furnace for reaction, and the operation of the segmented heat treatment is as follows: treating at 600 deg.C for 60min, and treating at 800 deg.C for 60min to obtain stainless steel substrate with organic carbon film formed on the surface.
4) Preparing a TiC coating: putting the stainless steel substrate obtained in the step 3) into a molten salt system in a molten salt crucible, then putting the stainless steel substrate into a well type furnace, continuously introducing inert gas for reaction at the reaction temperature of 600 ℃ for 2h, and growing a TiC coating on the surface of the substrate in the reaction process to obtain the titanium carbide coating for the surface of the metal bipolar plate of the proton exchange membrane fuel cell.
In step 4), the molten salt system comprises molten salt and a titanium source, wherein the molten salt is formed by mixing LiCl, KCl and NaCl according to the molar ratio of LiCl to KCl to NaCl =55 to 33 to 12, and the titanium source is formed by mixing Ti and K 2 TiF 6 According to the mass ratio of Ti to K 2 TiF 6 And the molten salt is 8:5 in mass ratio to the titanium source.
In the step 3) and the step 4), the inert gas is high-purity argon.
In step 1), the stainless steel is 316L stainless steel or 304 stainless steel, and is cut into a thin piece having a length × width × height =10mm × 10mm × 2 mm.
In step 1), the grinding operation in the pretreatment of the base material adopts 600-mesh sand paper.
The method prepares the titanium carbide composite coating by preparing the organic carbon film on the surface of the stainless steel and then utilizing the molten salt disproportionation reaction, and has the following beneficial effects:
1) The invention adds a carbon source for the occurrence of disproportionation reaction by developing an organic carbon film and converting the organic carbon film into a TiC coating.
2) The invention adopts the method of sectional annealing treatment at the stage of preparing the organic carbon film, and the sectional annealing can reduce the stress between the stainless steel substrate and the carbon layer, so that the binding force between the coating and the substrate is better, and the distribution is more uniform.
3) The TiC coating is prepared by a molten salt disproportionation reaction method, the TiC coating is quickly and effectively prepared while the melting point of ternary salt is reduced and the carbon layer is protected from being damaged, the operation is simple, resources are saved, and the prepared TiC coating is complete and compact.
4) The method of the invention integrally improves the production efficiency of the coating, reduces the pollution to the environment to a certain extent and achieves the aim of green production.
Drawings
Fig. 1 is a raman scan of an organic carbon coating in example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of the surface of an organic carbon coating layer in example 1 of the present invention.
FIG. 3 is a cross-sectional scanning electron micrograph of an organic carbon coating in example 1 of the present invention.
FIG. 4 is a cross-sectional scanning EDS plot of an organic carbon coating in example 1 of the present invention.
FIG. 5 is a Raman scan of a TiC coating in example 1 of the present invention.
FIG. 6 is a surface scanning electron micrograph of a TiC coating in example 1 of the present invention.
FIG. 7 is a scanning electron micrograph of a TiC coating layer in a cross section in inventive example 1.
FIG. 8 is a cross-sectional scanning EDS plot of a TiC coating in inventive example 1.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings.
The invention relates to a preparation method of a titanium carbide coating on the surface of a metal bipolar plate of a proton exchange membrane fuel cell, which comprises the following specific operation steps:
1) Pretreatment of a base material: 316L stainless steel or 304 stainless steel is selected as a base material, and the surface of the stainless steel is pretreated by polishing, washing and the like.
The stainless steel is cut into thin pieces of length × width × height =10mm × 10mm × 2 mm.
The base material can be polished by 600-mesh sand paper during polishing treatment so as to obtain a continuous flat and rough base material surface, and the binding force between the base material and the carbon layer can be improved in the subsequent annealing process.
2) Preparing an organic carbon solution: first, an organic carbon source, namely, perylene-3, 4,9, 10-tetracarboxylic dianhydride (PTCDA), was uniformly dispersed by ultrasonic mixing with N-methylpyrrolidone (NMP) as a solvent, and then, an epoxy resin and a methyltetrahydrophthalic anhydride as a curing agent were added and again subjected to ultrasonic mixing, wherein the perylene-3, 4,9, 10-tetracarboxylic dianhydride (PTCDA), the N-methylpyrrolidone (NMP), the epoxy resin and the methyltetrahydrophthalic anhydride were arranged in a mass ratio of 1: 4: 2, and a uniformly viscous organic carbon solution was obtained after ultrasonic mixing.
The epoxy resin and the curing agent adopted by the invention can improve the binding force between the carbon film and the stainless steel substrate.
3) And (3) heat treatment: putting a stainless steel substrate into a prepared organic carbon solution, firstly putting the stainless steel substrate into an oven for heat treatment for 35min at the temperature of 140 ℃, evaporating a solvent by reaction, then putting the stainless steel substrate into a tubular furnace for segmented heat treatment, and continuously introducing inert gas into the tubular furnace for reaction, wherein the operation of the segmented heat treatment is as follows: treating at 600 deg.C for 60min, and treating at 800 deg.C for 60min.
During the stage heat treatment, the inert gas introduced into the tube furnace is high-purity argon, and the tube furnace is a quartz tube.
After the heat treatment is finished, the stainless steel is taken out slightly, and a complete organic carbon film is obtained on the surface of the stainless steel.
The preparation of a continuous and compact carbon layer which is tightly combined with a matrix on the surface of stainless steel is the key for preparing the TiC coating, and the preparation of the carbon layer is the basis of the TiC coating.
4) Preparing a TiC coating: and (2) putting the stainless steel substrate with the organic carbon film formed on the surface into a molten salt system in a molten salt crucible, then putting the stainless steel substrate into a well furnace, continuously introducing inert gas for reaction at the temperature of 600 ℃ for 2 hours, and growing a TiC coating on the surface of the substrate in the reaction process to obtain the titanium carbide coating for the surface of the metal bipolar plate of the proton exchange membrane fuel cell.
The molten salt system comprises molten salt and a titanium source, wherein the molten salt is formed by mixing LiCl, KCl and NaCl according to a molar ratio of LiCl to KCl to NaCl =55 to 33 to 12, and the titanium source is formed by Ti and K 2 TiF 6 According to the mass ratio of Ti to K 2 TiF 6 And the molten salt is 8:5 in mass ratio to the titanium source.
The inert gas adopted in the reaction process is high-purity argon.
The method prepares the organic carbon film on the surface of the stainless steel substrate, then grows the TiC coating in situ at the carbon layer through disproportionation, and finally obtains the continuous and compact TiC coating with good combination with the matrix by controlling the parameters such as time, temperature, titanium source and the like, thereby providing a new preparation method for preparing the TiC coating, and the method has simple operation.
Example 1
The element contents of 316L stainless steel in the experiment are shown in table one, wherein the dimensions of 316L stainless steel are length × width × height =10mm × 10mm × 2mm, and 316L stainless steel are listed in table one. The 316L stainless steel was first sanded with 600 mesh sandpaper and rinsed to obtain a continuous flat and rougher substrate surface. And then preparing an organic carbon solution, wherein the solution is prepared by mixing the following raw materials in mass ratio: perylene-3,4,9,10-tetracarboxylic dianhydride, N-methylpyrrolidone, epoxy resin and methyltetrahydrophthalic anhydride = 1: 4: 2. When in preparation, the perylene-3, 4,9, 10-tetracarboxylic dianhydride (PTCDA) and the N-methylpyrrolidone (NMP) are mixed and then are subjected to ultrasonic separationDispersing uniformly, then adding epoxy resin and methyltetrahydrophthalic anhydride, and carrying out ultrasonic mixing treatment again to obtain more uniform organic carbon solution. Then putting the polished 316L stainless steel into a prepared organic carbon solution for annealing heat treatment, firstly carrying out heat treatment in a blast oven at 140 ℃ for 35min, and evaporating the solvent by reaction to volatilize most of the solvent; and then placing the tube furnace for segmented heat treatment, firstly treating at 600 ℃ for 60min, and then treating at 800 ℃ for 60min, wherein high-purity argon is continuously introduced into the tube furnace. After the heat treatment is finished, a uniform and dense coating is obtained on the surface of 316L stainless steel (fig. 1 is a Raman scanning image of the coating, fig. 2 is a surface scanning electron microscope image of the coating, fig. 3 is a cross-sectional scanning electron microscope image of the coating, fig. 4 is an element distribution diagram in an EDS scanning coating, in order to distinguish a carbon coating from resin more obviously, a layer of nickel is plated on the carbon coating), and the coating is known to be a carbon layer by combining the information in the Raman image and the electron microscope image, namely, an organic carbon film is formed on the surface of the stainless steel substrate. Finally, the stainless steel substrate is placed in a molten salt system of a molten salt crucible, then the stainless steel substrate is placed in a well type furnace, inert gas is introduced into the well type furnace, the reaction is carried out, the reaction temperature is 600 ℃, the reaction time is 2 hours, the molten salt system contains molten salt and a titanium source, the molten salt is ternary salt, namely LiCl, KCl and NaCl, the titanium source is Ti and K, and the titanium source is 2 TiF 6 Comprises LiCl, KCl and NaCl in a molar ratio of LiCl to KCl to NaCl =55 to 33 to 12, ti and K 2 TiF 6 According to the mass ratio of Ti to K 2 TiF 6 = 3: 2; the mass ratio of the molten salt to the titanium source is 8.
After the experiment is completed, a uniform and compact carbide coating can be obtained on the surface of 316L stainless steel, fig. 5 is a Raman scanning image of the carbide coating, fig. 6 is a surface scanning electron microscope image of the carbide coating, fig. 7 is a cross-sectional scanning electron microscope image of the carbide coating, fig. 8 is an element distribution diagram in the EDS scanning coating, and the TiC coating on the surface of 316L can be obtained by combining the Raman spectrum and the element distribution analysis result.
Watch 1
By the method, the titanium carbide composite coating can be prepared on the surface of 316L stainless steel by using organic carbon, so that more choices are provided for the preparation method of the titanium carbide coating on the surface of the metal bipolar plate, and the method is simpler and more convenient.
Claims (5)
1. A preparation method of a titanium carbide coating used on the surface of a metal bipolar plate of a proton exchange membrane fuel cell is characterized by comprising the following operation steps:
1) Pretreatment of a base material: selecting stainless steel as a base material, and carrying out polishing and water washing pretreatment on the surface of the stainless steel to obtain a continuous flat and rough base material surface;
2) Preparing an organic carbon solution: firstly, mixing an organic carbon source of perylene-3, 4,9, 10-tetracarboxylic dianhydride (PTCDA) and N-methylpyrrolidone (NMP) serving as a solvent, uniformly dispersing the mixture by ultrasonic treatment, adding an epoxy resin and a methyl tetrahydrophthalic anhydride serving as a curing agent, and performing ultrasonic treatment again, wherein the perylene-3, 4,9, 10-tetracarboxylic dianhydride (PTCDA), the N-methylpyrrolidone (NMP), the epoxy resin and the methyl tetrahydrophthalic anhydride are configured according to a mass ratio of 1: 4: 2, and uniformly mixing the mixture by ultrasonic treatment to obtain an organic carbon solution;
3) And (3) heat treatment: putting the stainless steel substrate treated in the step 1) into the organic carbon solution in the step 2), then putting the stainless steel substrate into an oven for heat treatment at the temperature of 140 ℃ for 35min, then putting the stainless steel substrate into a tubular furnace for segmented heat treatment, wherein inert gas is continuously introduced into the tubular furnace for reaction, and the operation of the segmented heat treatment is as follows: treating at 600 deg.C for 60min, and treating at 800 deg.C for 60min to obtain stainless steel substrate with organic carbon film formed on surface;
4) Preparing a TiC coating: putting the stainless steel substrate obtained in the step 3) into a molten salt system in a molten salt crucible, then putting the stainless steel substrate into a well type furnace, continuously introducing inert gas for reaction, wherein the reaction temperature is 600 ℃, the reaction time is 2 hours, and a TiC coating grows on the surface of the substrate in the reaction process, so that the titanium carbide coating for the surface of the metal bipolar plate of the proton exchange membrane fuel cell is obtained.
2. The method of claim 1, wherein the molten salt system of step 4) comprises a mixture of LiCl, KCl, and NaCl at a molar ratio of LiCl to KCl to NaCl =55 to 33 to 12, and a titanium source comprising Ti and K 2 TiF 6 According to the mass ratio of Ti to K 2 TiF 6 And the molten salt is 8:5 in mass ratio to the titanium source.
3. The method for preparing the titanium carbide coating on the surface of the metal bipolar plate of the proton exchange membrane fuel cell according to the claim 1 or 2, wherein in the step 3) and the step 4), the inert gas is high-purity argon.
4. The method for preparing the titanium carbide coating on the surface of the metal bipolar plate of the proton exchange membrane fuel cell according to claim 1 or 2, wherein in the step 1), the stainless steel is 316L stainless steel or 304 stainless steel, and is cut into thin slices with the length x the width x the height =10mm x 2 mm.
5. The method for preparing the titanium carbide coating on the surface of the metal bipolar plate of the proton exchange membrane fuel cell according to the claim 1 or 2, wherein in the step 1), the grinding in the pretreatment of the base material is performed by 600-mesh sand paper.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102130341A (en) * | 2011-01-18 | 2011-07-20 | 大连理工大学 | Bipolar plate of fuel cell and method for preparing carbon titanium nanocomposite film on surface thereof |
| CN103014793A (en) * | 2012-12-11 | 2013-04-03 | 广东电网公司电力科学研究院 | Method for preparing titanium carbide coating through pulse electrodeposition |
| CN105322184A (en) * | 2014-07-07 | 2016-02-10 | 江苏冰城电材股份有限公司 | Production technology of metal bipolar plate for proton exchange membrane fuel cell |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102130341A (en) * | 2011-01-18 | 2011-07-20 | 大连理工大学 | Bipolar plate of fuel cell and method for preparing carbon titanium nanocomposite film on surface thereof |
| CN103014793A (en) * | 2012-12-11 | 2013-04-03 | 广东电网公司电力科学研究院 | Method for preparing titanium carbide coating through pulse electrodeposition |
| CN105322184A (en) * | 2014-07-07 | 2016-02-10 | 江苏冰城电材股份有限公司 | Production technology of metal bipolar plate for proton exchange membrane fuel cell |
Non-Patent Citations (1)
| Title |
|---|
| 李伟;李争显;刘林涛;王浩楠;: "质子交换膜燃料电池金属双极板表面改性研究进展", 表面技术, no. 10, pages 92 - 100 * |
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