CN109728307A - A kind of preparation and bipolar plates and application of the metal double polar plates based on carbon film modification - Google Patents
A kind of preparation and bipolar plates and application of the metal double polar plates based on carbon film modification Download PDFInfo
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- CN109728307A CN109728307A CN201711026554.9A CN201711026554A CN109728307A CN 109728307 A CN109728307 A CN 109728307A CN 201711026554 A CN201711026554 A CN 201711026554A CN 109728307 A CN109728307 A CN 109728307A
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- 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
Abstract
The present invention relates to the surface modifying methods of novel metal bipolar plates a kind of in Proton Exchange Membrane Fuel Cells field.This modified bipolar plates are made of metallic matrix and surface reforming layer two parts, and modified layer passes through ion-plating deposition in matrix surface, and is divided into transition zone and outermost layer two parts.The present invention can further increase the corrosion resistance of metallic matrix, reduce the contact resistance of bipolar plates and gas diffusion layer material (carbon paper), bipolar plates can be processed using modes such as punching presses, to improve the quality specific power and volumetric specific power of fuel cell pile.
Description
Technical field
The present invention relates to the metal double polar plates based on carbon film modification in a proton exchanging film fuel battery technical field
Preparation and bipolar plates and application.
Background technique
Proton Exchange Membrane Fuel Cells (PEMFC) is a kind of energy conversion device for converting chemical energy to electric energy.Its with
Hydrogen and oxygen are raw material, and reaction generates water under the effect of the catalyst.Proton Exchange Membrane Fuel Cells is environmentally friendly, energy
High conversion efficiency, energy quick start, therefore, by global extensive concern.In addition, its in auto industry, spare answer urgent telegram
Source, the dispersion fields such as power station and military affairs have broad application prospects.
Bipolar plates are one of critical components of Proton Exchange Membrane Fuel Cells, have and connect single pond, support pile, provide gas
The effects of body flow field, collected current, heat dissipation, draining, it is therefore desirable to which the material as bipolar plates has high mechanical strength, permeation
Rate is low, conductivity is high, thermal conductivity is good, the properties such as corrosion-resistant, low with carbon paper contact resistance, inexpensive.
In electrical source of power application aspect, it is desirable that fuel cell pile quality specific power with higher and volumetric specific power,
But in traditional proton exchange film fuel cell electric piling, graphite is the main material for making bipolar plates, not due to graphite air-tightness
The good, reasons such as mechanical strength is low, brittleness is big, cause conventional bipolar plate thickness is big, quality weight, intolerant to mechanical shock, difficulty of processing
Greatly, at high cost, so that graphite is limited in the application of electrical source of power.Metal conductivity with higher, preferable mechanical strength,
Air penetrability is low, thermal conductivity is good, it is at low cost, the features such as punch process can be carried out, be make bipolar plates one of potential material, but gold
The contact resistance belonged between carbon paper is excessive, in turn results in the biggish ohmage of inside battery, this will significantly reduce metal conduct
When bipolar plates, the output performance of pile.Therefore, the bipolar plate surfaces of metal production must carry out modification appropriate.
Many researchers are in matrix stainless steel surface depositing TiN coating at present, this significantly reduces stainless steel and carbon paper it
Between contact resistance, but TiN coating stability is poor.Ho-Young Jung is prepared for 1 μm of gold plate on titanium plate surface, resistance
The formation of passivation layer is stopped, battery performance is preferable, but gold is expensive, it is difficult to realize large-scale commercial application.
B.Yang is prepared for the nitride of Cr by tropical resources in stainless steel surface, but film is discontinuous, poor to the protectiveness of matrix.?
Metal bipolar plate surface prepares fine and close, corrosion-resistant, good conductivity and the small carbon coating of contact resistance between carbon paper, then can mention
The corrosion resistance of high parent metal reduces the internal resistance of proton exchange film fuel cell electric piling, improves pile output performance.
The present invention is directed to the deficiency of existing dual polar plates of proton exchange membrane fuel cell process for modifying surface, provides one kind
The surface modifying method of dual polar plates of proton exchange membrane fuel cell improves its corrosion resistance, the contact between carbon paper
Resistance reduces, and meets the demand for development of proton exchange fuel cell high quality specific power and high volumetric specific power.
Summary of the invention
A kind of preparation method of the metal double polar plates based on carbon film modification, comprising the following steps:
1) in advance to metal base carry out surface clean, the process of cleaning include pickling, alkali cleaning, deionization washing, it is described
Metal base can be sheet metal prepared by stainless steel, titanium and its alloy, aluminium and its alloy, magnesium alloy, thickness exists
0.01mm~1mm；
2) using ion plating metallic substrate surface deposit transition zone, the transition zone be Cr, Ti, Nb, Ta, Ni, Cu,
One of Al, V, Co, Au, Ag etc. or a variety of, transition zone can be metal simple-substance, be also possible to the nitride or carbon of metal
Compound, the vacuum degree of the ion plating are 1 × 10-2Pa~50Pa, working gas He, Ar, N2, methane, in the gases such as acetylene
One or several kinds of gases mixed gas, deposition current is 1A~300A, and time of deposition is 10min~300min, institute
The thickness of the transition zone of preparation is in 10nm~30 μm；
3) using ion plating in the surface depositing carbon film of transition zone, the vacuum degree of the ion plating is 1 × 10-2Pa~
50Pa, working gas are the mixed gas of one of Ar, He gas or two kinds of gases, and deposition current is 1A~300A, are sunk
The long-pending time is 10min~300min, and the thickness of prepared carbon film is in 10nm~30 μm.
The metal base that the present invention selects with a thickness of 0.01mm~1mm, more mature metal board machining process can be used
Carry out the processing of the components such as flow field.Transition metal has resistance to local corrosion ability strong, plays a part of to obstruct Corrosion developing, outermost
The carbon film of layer has the characteristic that resistivity is low, the corrosion-resistant contact resistance between carbon paper is small, therefore, the presence of modified layer, so that
140N cm-2Pressing force under, 459m Ω cm of the contact resistance by most2It is reduced to 5.17m Ω cm2, 0.5mol L-1Sulphur
177.8 μ A cms of the corrosion current by most in acid solution-2It is reduced to 0.12 μ A cm-2, modified layer significantly reduces bipolar plates
The mass ratio of Proton Exchange Membrane Fuel Cells can be improved in contact resistance and corrosion current between carbon paper, modified bipolar plates
Power and volumetric specific power.Modified layer price is lower, can reduce the cost of Proton Exchange Membrane Fuel Cells, is suitble to answer on a large scale
With.
Detailed description of the invention
Fig. 1 be between the modified 316L stainless steel in 1 surface of embodiment and carbon paper contact resistance with pressure change schematic diagram.
Fig. 2 is the modified 316L stainless steel in 1 surface of embodiment in 0.5mol L-1Polarization curve signal in sulfuric acid solution
Figure.
Fig. 3 is the scanning electron microscope diagram of the modified 316L stainless steel in 1 surface of embodiment.
Specific embodiment
Elaborate with reference to the accompanying drawing to the embodiment of the present invention: the present embodiment before being with technical solution of the present invention
It puts and is implemented, but the contents of the present invention are not limited solely to the following examples.
Embodiment 1:
The 316L stainless steel substrates for taking 0.1mm thickness are polished step by step with 600 mesh~2000 mesh sand paper, clear with acetone and water ultrasound
30min is washed, is evacuated to 1 × 10-3Pa~1 × 10-2Pa is filled with argon gas, pressure is adjusted between 1Pa~10Pa, in stainless steel
Piece surface deposits CrC/C composite coating:
(1) Cr bottom is deposited, chromium target sputtering current increases to 5A from 0A, sputters 5min；
(2) CrC transition zone is deposited, chromium target current drops to 2A, and graphite target electric current gradually rises to 6A, and preparation CrC is applied
Layer；
(3) electric current of chromium target and graphite target is respectively maintained at 2A and 6A, sputters 60min, generates fine and close C:Cr coating；
(4) chromium target current is gradually decrease to close, and 45min is deposited under 5A sputtering current, forms carbon film.
It is prepared based on the bipolar plate of stainless steel of carbon film in 140N cm-2Pressing force under, contact resistance is by most
459mΩcm2It is reduced to 5.17m Ω cm2, 0.5mol L-1Sulfuric acid solution in 177.8 μ A cms of the corrosion current by most-2
It is reduced to 0.12 μ A cm-2。
Embodiment 2:
The 316L stainless steel substrates for taking 0.2mm thickness are polished step by step with 600 mesh~2000 mesh sand paper, clear with acetone and water ultrasound
30min is washed, is evacuated to 1 × 10-3Pa~1 × 10-2Pa adjusts pressure between 1Pa~10Pa, heavy on stainless steel substrates surface
Product CrN/C composite coating:
(1) it is passed through Ar gas into cavity, deposits Cr bottom, chromium target sputtering current increases to 5A from 0A, sputters 5min；
(2) it is filled with Ar/N2(Ar gas, N2The flow-rate ratio of gas is 1:2), CrN transition zone is deposited, chromium target current drops to 2A, makes
Standby CrN coating；
(3) chromium target current is gradually decrease to close, and 45min is deposited under 5A sputtering current, forms carbon film.
It is prepared based on the bipolar plate of stainless steel of carbon film in 140N cm-2Pressing force under, contact resistance is by most
459mΩcm2It is reduced to 6.5m Ω cm2, 0.5mol L-1Sulfuric acid solution in 177.8 μ A cms of the corrosion current by most-2Drop
Low is 0.18 μ A cm-2。
Embodiment 3:
The titanium sheet for taking 0.1mm thickness carries out pickling with 1% HF, is cleaned by ultrasonic 30min with acetone and water, it is evacuated to 1 ×
10-3Pa~1 × 10-2Pa adjusts pressure between 1Pa~10Pa, in titanium plate surface depositing TiN/C composite coating:
(1) Ar gas, depositing Ti bottom are passed through into cavity, titanium target sputtering current increases to 5A from 0A, sputters 5min；
(2) it is filled with Ar/N2(Ar gas, N2The flow-rate ratio of gas is 1:2), depositing TiN transition zone, titanium target electric current drops to 2A, system
Standby TiN coating；
(3) titanium target electric current is gradually decrease to close, and 45min is deposited under 5A sputtering current, forms carbon film.
The prepared titanium alloy bipolar plates based on carbon film are in 140N cm-2Pressing force under, contact resistance is by most
516mΩcm2It is reduced to 5.5m Ω cm2, 0.5mol L-1Sulfuric acid solution in 468.2 μ A cms of the corrosion current by most-2Drop
Low is 0.19 μ A cm-2。
Embodiment 4:
The titanium sheet for taking 0.1mm thickness carries out pickling with 1% HF, is cleaned by ultrasonic 30min with acetone and water, it is evacuated to 1 ×
10-3Pa~1 × 10-2Pa is filled with argon gas, pressure is adjusted between 1Pa~10Pa, in the compound painting of titanium plate surface depositing Ti C/C
Layer:
(1) depositing Ti bottom, titanium target sputtering current increase to 5A from 0A, sputter 5min；
(2) depositing Ti C transition zone, titanium target electric current drop to 3A, and graphite target electric current gradually rises to 6A, and preparation TiC is applied
Layer；
(3) electric current of titanium target and graphite target is respectively maintained at 3A and 6A, sputters 60min, generates fine and close C:Ti coating；
(4) titanium target electric current is gradually decrease to close, and 45min is deposited under 5A sputtering current, forms carbon film.
The prepared titanium alloy bipolar plates based on carbon film are in 140N cm-2Pressing force under, contact resistance is by most
516mΩcm2It is reduced to 6.5m Ω cm2, 0.5mol L-1Sulfuric acid solution in 468.2 μ A cms of the corrosion current by most-2Drop
Low is 0.20 μ A cm-2。
Embodiment 5:
The aluminum alloy flake for taking 0.1mm thickness carries out pickling with 1% HCl, is cleaned by ultrasonic 30min with acetone and water, takes out true
Sky is to 1 × 10-3Pa~1 × 10-2Pa is filled with argon gas, adjusts pressure between 1Pa~10Pa, deposits on aluminum alloy flake surface
TiC/C composite coating:
(1) depositing Ti bottom, titanium target sputtering current increase to 5A from 0A, sputter 5min；
(2) depositing Ti C transition zone, titanium target electric current drop to 3A, and graphite target electric current gradually rises to 6A, and preparation TiC is applied
Layer；
(3) electric current of titanium target and graphite target is respectively maintained at 3A and 6A, sputters 60min, generates fine and close C:Ti coating；
(4) titanium target electric current is gradually decrease to close, and 45min is deposited under 5A sputtering current, forms carbon film.
The prepared aluminium alloy bipolar plates based on carbon film are in 140N cm-2Pressing force under, contact resistance is by most
495mΩcm2It is reduced to 6.5m Ω cm2, 0.5mol L-1Sulfuric acid solution in 698.7 μ A cms of the corrosion current by most-2Drop
Low is 0.19 μ A cm-2。
Embodiment 6:
The magnesium alloy thin slice for taking 0.5mm thickness, with 1% HClO4Pickling is carried out, is cleaned by ultrasonic 30min with acetone and water, takes out
Vacuum is to 1 × 10-3Pa~1 × 10-2Pa is filled with argon gas, adjusts pressure between 1Pa~10Pa, heavy in magnesium alloy sheet surface
Product TiC/C composite coating:
(1) depositing Ti bottom, titanium target sputtering current increase to 5A from 0A, sputter 5min；
(2) depositing Ti C transition zone, titanium target electric current drop to 3A, and graphite target electric current gradually rises to 6A, and preparation TiC is applied
Layer；
(3) electric current of titanium target and graphite target is respectively maintained at 3A and 6A, sputters 60min, generates fine and close C:Ti coating；
(4) titanium target electric current is gradually decrease to close, and 45min is deposited under 5A sputtering current, forms carbon film.
The prepared magnesium alloy bipolar plates based on carbon film are in 140N cm-2Pressing force under, contact resistance is by most
625mΩcm2It is reduced to 4.5m Ω cm2, 0.5mol L-1Sulfuric acid solution in 861.7 μ A cms of the corrosion current by most-2Drop
Low is 0.25 μ A cm-2。
Embodiment 7:
The aluminum alloy flake for taking 0.1mm thickness carries out pickling with 1% HCl, is cleaned by ultrasonic 30min with acetone and water, takes out true
Sky is to 1 × 10-3Pa~1 × 10-2Pa adjusts pressure between 1Pa~10Pa, in the unilateral compound painting of deposition NbN/C of aluminum alloy thin
Layer:
(1) Ar gas, depositing Ti bottom are passed through into cavity, niobium target sputtering current increases to 5A from 0A, sputters 5min；
(2) it is filled with Ar/N2(Ar gas, N2The flow-rate ratio of gas is 1:5), NbN transition zone is deposited, titanium target electric current drops to 2A, makes
Standby NbN coating；
(3) niobium target current is gradually decrease to close, and 45min is deposited under 5A sputtering current, forms carbon film.
The prepared aluminium alloy bipolar plates based on carbon film are in 140N cm-2Pressing force under, contact resistance is by most
495mΩcm2It is reduced to 7.2m Ω cm2, 0.5mol L-1Sulfuric acid solution in 698.7 μ A cms of the corrosion current by most-2Drop
Low is 0.19 μ A cm-2。
Embodiment 8:
The titanium alloy thin slice for taking 0.1mm thickness carries out pickling with 1% HF, is cleaned by ultrasonic 30min with acetone and water, takes out true
Sky is to 1 × 10-3Pa~1 × 10-2Pa is passed through Ar gas, adjusts pressure between 1Pa~10Pa, deposits in titanium alloy sheet plane
Ag/C composite coating:
(1) Ag bottom is deposited, silver target sputtering electric current increases to 5A from 0A, sputters 5min；
(2) Ag/C transition zone is deposited, silver-colored target current drops to 2A, and graphite target electric current gradually rises to 6A, prepares Ag/C
Coating；
(3) silver-colored target current is gradually decrease to close, and the electric current of graphite target maintains 5A, deposits 45min, forms carbon film.
The prepared titanium alloy bipolar plates based on carbon film are in 140N cm-2Pressing force under, contact resistance is by most
516mΩcm2It is reduced to 5.1m Ω cm2, 0.5mol L-1Sulfuric acid solution in 468.2 μ A cms of the corrosion current by most-2Drop
Low is 0.18 μ A cm-2。
Present invention process parameter bound value can all be able to achieve the present invention, embodiment numerous to list herein.
Claims (8)
1. a kind of preparation method of the metal double polar plates based on carbon film modification, it is characterised in that: using ion electroplating method in metal
Substrate surface prepares modified layer, obtains modified metal double polar plates, the modified layer is by the intermediate metal close to substrate surface
It is formed with outermost layer.
2. a kind of preparation method of metal double polar plates based on carbon film modification according to claim 1, it is characterised in that: institute
The metal base stated can be one of stainless steel, titanium and its alloy, aluminium and its alloy, magnesium alloy materials or two kinds or more
Sheet metal, thickness is in 0.01mm~1mm.
3. the preparation method of the metal double polar plates according to claim 1 based on carbon film modification, it is characterised in that: the gold
Belong to transition zone be between substrate surface and outermost layer, one of metal Cr, Ti, Ni, Cu, Al, V, Co, Au, Ag or
Two kinds or more metals, buffer layer material can be one of above-mentioned metal simple-substance, the carbide of metal or nitride or two
Kind or more, the thickness of transition zone is in 10nm~30 μm.
4. the preparation method of the metal double polar plates according to claim 1 based on carbon film modification, it is characterised in that: described
Outermost layer coating is C film, and the thickness of C film is in 10nm~30 μm.
5. the preparation method of transition zone according to claim 1, it is characterized in that: the working gas that the ion plating uses
It is He, Ar, N2, methane, one of gases such as acetylene or two kinds or more gas mixed gas, operating pressure is 1 × 10-2
~50Pa, the deposition current of ion plating are 1A~300A, and sedimentation time is 1min~300min.
6. preparation method according to claim 1 or 5, it is characterised in that: the work gas that the ion plating process uses
Body is the mixed gas of one of Ar, He gas or two kinds of gases, and operating pressure is 1 × 10-2~50Pa, ion plating are sunk
Product electric current is 1A~300A, and sedimentation time is 1min~300min.
7. a kind of bipolar plates that any preparation method of claim 1-6 prepares.
8. a kind of application of the bipolar plates described in claim 7 in Proton Exchange Membrane Fuel Cells.
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Cited By (6)
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| CN110265668A (en) * | 2019-06-19 | 2019-09-20 | 上海大学 | Hydrogen fuel battery metal bi-polar plate and preparation method thereof |
| CN112111721A (en) * | 2020-09-25 | 2020-12-22 | 中国科学院兰州化学物理研究所 | Preparation method of CrCuC gradient CrCu composite carbon film bipolar plate |
| CN112795886A (en) * | 2020-12-24 | 2021-05-14 | 上海治臻新能源装备有限公司 | Conductive corrosion-resistant precoating for forming metal bipolar plate and preparation method thereof |
| CN112993276A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Metal bipolar plate for Nb-Cr-C coating modified fuel cell and preparation method thereof |
| CN113373469A (en) * | 2021-05-31 | 2021-09-10 | 宝武清洁能源有限公司 | Bipolar plate of water electrolysis hydrogen production system and preparation method and application thereof |
| CN114231925A (en) * | 2021-12-14 | 2022-03-25 | 中国科学院大连化学物理研究所 | Fuel cell metal bipolar plate composite coating and preparation method thereof |
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| CN113373469A (en) * | 2021-05-31 | 2021-09-10 | 宝武清洁能源有限公司 | Bipolar plate of water electrolysis hydrogen production system and preparation method and application thereof |
| CN114231925A (en) * | 2021-12-14 | 2022-03-25 | 中国科学院大连化学物理研究所 | Fuel cell metal bipolar plate composite coating and preparation method thereof |
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Application publication date: 20190507 |