CN109473694A - Solid oxide fuel cell stainless steel connector surface protection coating and its preparation - Google Patents
Solid oxide fuel cell stainless steel connector surface protection coating and its preparation Download PDFInfo
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- CN109473694A CN109473694A CN201811203615.9A CN201811203615A CN109473694A CN 109473694 A CN109473694 A CN 109473694A CN 201811203615 A CN201811203615 A CN 201811203615A CN 109473694 A CN109473694 A CN 109473694A
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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
- H01M8/0297—Arrangements for joining electrodes, reservoir layers, heat exchange units or bipolar separators to each other
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention belongs to high-temperature fuel cell technical fields, and in particular to a kind of solid oxide fuel cell stainless steel connector surface protection coating and preparation method thereof.In order to solve the problems, such as that stainless steel connector existing oxidation film during usage increases battery " poisoning of cathode " caused by caused resistivity increase and Cr volatilization, propose in stainless steel surface application copper oxide/cobalt-based spinelle duplex coating.In addition, propose using plating Cu-Co alloy, the then oxidation-treated method for preparing the coating, this method have the characteristics that simple process, it is at low cost, be easy to mass production.The present invention has theoretical and practical significance to the development of SOFC stainless steel connector surface conductance, antioxidant coating technology.
Description
Technical field
The invention belongs to high-temperature fuel cell technical fields, and in particular to a kind of solid oxide fuel cell stainless steel company
Junctor surface protection coating and preparation method thereof.
Background technique
Ferritic stainless steel is intermediate temperature solid oxide fuel cell (SOFC) metallic interconnection materials of most application prospect.So
And stainless steel connector is faced with high-temperature oxydation problem in SOFC environment (especially cathode environment).On the one hand, stainless steel watch
Look unfamiliar long chromium oxide film can in cathode atmosphere oxygen or vapor react, formed volatility Cr oxide,
Cause battery " poisoning of cathode "；On the other hand, the growth of chromium oxide film will increase resistance, and chromium oxide film cracking stripping can also occur
It falls, leads to SOFC performance degradation, applying conductive antioxidant coating is a kind of effective way to solve the above problems.Currently, Co3O4
Spinelle is considered as one of SOFC connector barrier material of most application prospect.However, under SOFC service condition,
Co3O4It is easy to generate Spinel containing Cr with the Cr element reaction spread in stainless steel base.Spinel containing Cr also can be with
Oxygen or vapor react, although the extent of reaction is much smaller compared with chromium oxide, can not avoid the shape of volatility Cr completely
At.
Summary of the invention
For the prior art under SOFC Service Environment Co3O4Coating can not be avoided caused by volatility Cr completely " in cathode
Poison " problem, it is an object of the invention to propose a kind of novel protective on solid oxide fuel cell stainless steel connector surface
Coating, and propose a kind of simple, efficient, energy-efficient method for preparing the coating, there is the SOFC of practical application foreground for developing
Stainless steel connector has positive effect with conductive antioxidant coating.
The technical scheme is that
A kind of solid oxide fuel cell stainless steel connector surface protection coating, the coating are made of double-layer structure,
Outer layer is continuous copper oxide, and internal layer is continuous cobalt-based spinel layer, and total coating thickness is not less than 3 μm.
The solid oxide fuel cell stainless steel connector surface protection coating, by atomic percentage, coating
In Cu/Co be 1:8~2:1.
The solid oxide fuel cell stainless steel connector surface protection coating, the general formula of internal layer cobalt-based spinelle
For Co3-xMxO4, 0≤x≤2.5；Wherein, the one or more of M Cr, Fe, Mn, Cu, Ni element.
The solid oxide fuel cell stainless steel connector surface protection coating, exist in cobalt-based spinel layer at
Point gradient, wherein M element content with the increase of coating/basal body interface distance and reduce.
The preparation method of the solid oxide fuel cell stainless steel connector surface protection coating, including walk as follows
It is rapid:
(1) preparation of plating solution: by mantoquita, cobalt salt and complexing agent by the mixing of required stoichiometric ratio and soluble in water, adjusting
The pH value of plating solution is 3~8, that is, plating solution needed for obtaining；
(2) using plating solution obtained by step (1), in stainless steel base surface electro-deposition Cu-Co coating, sedimentation time is 10~
120min, coating layer thickness are not less than 2 μm；
(3) the Cu-Co coating is subjected to high temperature oxidation process under the conditions of 500~900 DEG C in oxygen-containing atmosphere, that is, existed
Stainless steel base surface obtains copper oxide/cobalt-based spinelle coating.
The preparation method of the solid oxide fuel cell stainless steel connector surface protection coating, in step (1),
The molar concentration of mantoquita is 0.01~5mol/L, and the molar concentration of cobalt salt is 0.01~5mol/L.
The preparation method of the solid oxide fuel cell stainless steel connector surface protection coating, in step (1),
Complexing agent is citrate complexing agent, and molar concentration is 0~10mol/L.
The preparation method of the solid oxide fuel cell stainless steel connector surface protection coating, in step (1),
Plating solution composition is also comprising one or more of supporting electrolyte, buffer, anode activating agent and additive.
The preparation method of the solid oxide fuel cell stainless steel connector surface protection coating, in step (2):
Electrodeposition process is galvanostatic method, and current density is 1~20mAcm-2；Alternatively, electrodeposition process is potentiostatic method, plating current potential
For -0.8~-1.2VSCE。
The preparation method of the solid oxide fuel cell stainless steel connector surface protection coating, step (2) institute
After obtaining the progress high-temperature low-oxygen pressure processing of Cu-Co coating, then step (3) are carried out, the high-temperature low-oxygen presses treatment process are as follows: in inertia
It in atmosphere, vacuum atmosphere or reducing atmosphere, is heat-treated under the conditions of 300~900 DEG C, the processing time is 0.5~10h.
Design philosophy of the invention is:
The present invention proposes a kind of SOFC stainless steel connector copper oxide surface/cobalt-based spinelle Double-protection coating, outer layer
For continuous copper oxide, internal layer is continuous cobalt-based spinel layer.Copper oxide is higher than the conductivity of cobalt-based spinelle under high temperature
Several orders of magnitude will not reduce the electrical property of battery.Since copper oxide and the affinity of Cr are far below cobalt-based spinelle, never
The Cr spread in rust steel matrix is " captured " in internal layer spinelle, to be effectively isolated Spinel containing Cr and environment gas
Atmosphere avoids the formation of surface volatility Cr oxide.According to Cu-Co-O ternary phase diagrams (Phase Diagrams for
Ceramists 1975 Supplement.The American Ceramic Society, Columnus, 1975), in medium temperature
In SOFC service temperature section (600~800 DEG C), Cu is in Co3O4In solid solubility it is extremely low (solid solubility is less than 9% at 800 DEG C),
Extra Cu can exist in the form of copper oxide.As it can be seen that copper oxide/cobalt-based spinelle duplex coating has under SOFC Service Environment
There is higher thermodynamic stability, can achieve the purpose of long-lasting protection.
The present invention realizes growth in situ by carrying out high temperature oxidation process to Cu-Co deposition layer, in stainless steel surface
Copper oxide/cobalt-based spinelle duplex coating.This method is at low cost, it is high-efficient, be easy to mass production.Cu-Co coating can lead to
Peroxidating handles growth in situ and determines at relatively stable copper oxide/cobalt-based spinelle duplex coating there are three thermodynamics and kinetics
Determine factor: first is that thermodynamically copper oxide and cobalt-based spinelle can be stabilized；Second is that the equilibrium oxygen partial pres-sure of copper oxide is not low
In cobalt-based spinelle；Third is that the diffusion rate of Cu in the coating is much larger than Co.It is noted that not all ingredient is suitable
Preferably, uniformly, Cu-Co coating that is fine and close, being well combined with matrix can be obtained by reasonable high temperature oxidation process it is stable
Copper oxide/cobalt-based spinelle duplex coating.It is reported that in Co3O4The conductivity of cobalt-based spinelle can be improved in middle doping Cu
(Petric A,Ling H.J Am Ceram Soc 90(2007)1515-1520；Paknahad P et al.J Power
Sources 266(2014)79-87).In the case where obtaining the original intention of Co-Cu spinelle coating of high conductance, inventor once existed
Stainless steel surface prepares the Cu-Co coating that thickness is about 0.5 μm, after oxidation-treated 2h coating be changed into a thin layer CuO outer layer,
Thicker Cu0.92Co2.08O4Middle layer, a thin layer Co3O4Internal layer, but with the extension of oxidization time, coating is finally changed into list
One (Cr, Co, Cu, Mn, Fe)3O4Spinel layer (43 (2018) 3273- of X.Zhang, et al.Int J Hydrogen Energ
3279；Open corrosion science and the guard technologies such as snow, 30 (2018) 1-7).In fact, stable copper oxide/cobalt-based can be formed
One vital factor of spinelle duplex coating is thickness of coating.When thickness of coating is very thin, oxidation initial stage Cu and
Co is easier to come into full contact with, and forms unstable state mutually such as Cu0.92Co2.08O4, i.e. supersaturated solid solution of the Cu in cobalt-based spinelle, this
The presence of kind unstable state phase further increases the driving force that stainless steel base element is migrated into coating, and then ultimately forms
The single Spinel of high-Cr, the volatilization of Cr still can not avoid completely；When thickness of coating is thicker, CuO outer layer can be with
Be stabilized, thicker spinelle internal layer can also play better blocking effect, thus effectively completely cut off Spinel containing Cr and
The contact of cathode atmosphere.
Compared with the prior art, advantages of the present invention and beneficial effect are:
1, under SOFC running environment, prior art Co3O4The long-term usage rear surface of coating not can avoid volatility Cr's still
It is formed, the present invention proposes a kind of stainless steel connector copper oxide surface/cobalt-based spinelle duplex coating, using poor with Cr affinity
Copper oxide outer layer can completely isolated Spinel containing Cr and cathode atmosphere contact, so that volatility Cr be avoided to cause completely
" poisoning of cathode " problem.
2, the present invention proposes a kind of in stainless steel base surface preparation Cu-Co coating, is aoxidized through high temperature oxidation process
Copper/cobalt-based spinelle duplex coating preparation method.This method is upper complicated, ingenious in theory design, both needs at component selections
The problems such as considering conductivity, thermal matching considers thermodynamics and kinetics factor again.In addition, this method also has technique
Simply, high-efficient, the features such as being easy to mass production, is at low cost.
Detailed description of the invention
Fig. 1 (a)-(b) is coating Cross Section Morphology figure and constituency energy spectrum diagram prepared by embodiment 1.Wherein, Fig. 1 (a) is plating
Layer cross section shape appearance figure, Fig. 1 (b) are constituency energy spectrum diagram.
Fig. 2 be aoxidize 48h in 750 DEG C of humid airs, respectively with painting prepared by uncoated sample (a) and embodiment 1
Layer sample (b) stacks the constituent analysis spectrogram on the strontium lanthanum manganese oxide piece surface placed.
Fig. 3 is copper oxide/cobalt-based spinelle duplex coating sample prepared by embodiment 3 in the case where simulating sofc cathode environment
Cross Section Morphology figure after aoxidizing 500h.
Specific embodiment
In the specific implementation process, solid oxide fuel cell stainless steel connector copper oxide surface/cobalt-based of the present invention
Spinelle duplex coating, the coating are made of double-layer structure, and outer layer is continuous copper oxide, and internal layer is that continuous cobalt-based point is brilliant
Rock layers；Total coating thickness is not less than 3 μm, and preferred copper oxide is with a thickness of 1~2.5 μm, preferred cobalt-based spinel layer thickness
It is 4~12 μm, the preparation method of the coating includes the following steps:
(1) preparation of plating solution: by mantoquita, cobalt salt and complexing agent by the mixing of required stoichiometric ratio and soluble in water, adjusting
The pH value of plating solution is 3~8, that is, plating solution needed for obtaining；
(2) using plating solution obtained by step (1), in stainless steel base surface electro-deposition Cu-Co coating, sedimentation time is 10~
120min, coating layer thickness are not less than 2 μm；
(3) the Cu-Co coating is subjected to high temperature oxidation process under the conditions of 500~900 DEG C in oxygen-containing atmosphere, that is, existed
Stainless steel base surface obtains copper oxide/cobalt-based spinelle coating.
The present invention is described in detail with reference to the accompanying drawings and embodiments.
Embodiment 1
In the present embodiment, sample selects 430 ferritic stainless steels, stainless steel sample is polishing to 1000# step by step, and through clear
Water rinses, acetone ultrasonic cleaning dries up.First by sample in 20vol.%H before plating2SO4Soaking time 30s is in solution to remove not
The oxidation film for steel surface of becoming rusty, carries out electro-deposition at once after then successively being cleaned with clear water, deionized water.Using bipolar electrode system into
Row Cu-Co alloy electrodeposition, working electrode are 430 stainless steel samples, and anode is graphite plate.Plating solution composition are as follows: 0.04M
CuSO4, 0.02~0.4M CoSO4, 0.02~0.2M C6H8O7、0.5M Na2SO4With the water of surplus.Bath pH value is 4~6,
Current density is 2~10mAcm-2, sedimentation time 30min, experimental temperature is 25 DEG C.The Cross Section Morphology figure and energy spectrum diagram of coating
As shown in Fig. 1 (a)-(b), it is seen that coating is uniform, fine and close, is well combined with matrix, and Coating composition is Cu and Co.Cu-Co is plated
Layer carries out destressing in 400~800 DEG C of vacuum drying ovens and handles 2h, then the oxidation processes 2h in 700~900 DEG C of air, obtains oxygen
Change copper/cobalt-based spinelle duplex coating, copper oxide is with a thickness of 1.5 μm, and cobalt-based spinel layer is with a thickness of 5 μm.By coating sample
With uncoated sample respectively with cathode material strontium lanthanum manganese oxide (La0.8Sr0.2MnO3) piece stacking, it is placed in (mould in 750 DEG C of humid airs
Quasi- sofc cathode atmosphere) oxidation 48h, the energy spectrum analysis on the strontium lanthanum manganese oxide surface stacked with sample as shown in Fig. 2, with coating sample
The strontium lanthanum manganese oxide piece surface that product stack does not detect Cr element, and then examines on the strontium lanthanum manganese oxide piece surface stacked with uncoated sample
Cr element is measured, illustrates that copper oxide/cobalt-based spinelle duplex coating can be effectively avoided caused by volatility Cr " in cathode
Poison " problem.
Embodiment 2
In the present embodiment, sample selects 430 ferritic stainless steels, stainless steel sample is polishing to 1000# step by step, and through clear
Water rinses, acetone ultrasonic cleaning dries up.First by sample in 20vol.%H before plating2SO4Soaking time 20s is in solution to remove not
The oxidation film for steel surface of becoming rusty, carries out electro-deposition at once after then successively being cleaned with clear water, deionized water.Using three-electrode system into
Row Cu-Co alloy electrodeposition, working electrode are 430 stainless steel samples, and anode is Pt piece, and reference electrode is saturated calomel electrode.
Plating solution composition are as follows: 0.5M CuSO4、4M CoCl2, 0.5~8M Na3C6H5O7With the water of surplus.Bath pH value is 5, plating current potential
For -0.8~-1.4VSCE, sedimentation time 20min, experimental temperature is 20~40 DEG C.By Cu-Co coating in 700~900 DEG C of skies
Oxidation processes 20h in gas, obtains copper oxide/cobalt-based spinelle duplex coating, and copper oxide is with a thickness of 2 μm, cobalt-based spinel layer
With a thickness of 7 μm.
Embodiment 3
In the present embodiment, sample selects 430 ferritic stainless steels, stainless steel sample is polishing to 800# step by step, and through clear
Water rinses, EtOH Sonicate cleaning dries up.First by sample in 15vol.%HCl+5vol.%HNO before plating3Soaking time in solution
10s carries out electro-deposition to remove the oxidation film of stainless steel surface at once after then successively being cleaned with clear water, deionized water.Using
Three-electrode system carries out Cu-Co alloy electrodeposition, and working electrode is stainless steel sample, and anode is Pt piece, and reference electrode is saturation
Calomel electrode.Plating solution composition are as follows: 0.02~0.2M CuSO4、0.3M CoSO4, 0.03~0.5M Na3C6H5O7、0.4M NaCl、
0.2M Na2SO4With the water of surplus.Bath pH value is 4~7, and current density is 3~12mAcm-2, sedimentation time 35min, in fact
Testing temperature is 20~40 DEG C.By Cu-Co coating in 700~900 DEG C of air oxidation processes 10h, it is brilliant to obtain copper oxide/cobalt-based point
Stone duplex coating, copper oxide is with a thickness of 2.5 μm, and cobalt-based spinel layer is with a thickness of 8 μm.By coating sample in simulation sofc cathode
(800 DEG C of air atmospheres) aoxidizes 500h under environment, and coating cross sections pattern is as shown in Figure 3, it is seen that aoxidizes 500h in 800 DEG C of air
Copper oxide/cobalt-based spinelle duplex coating is still able to maintain good structural stability afterwards, i.e. outer layer is continuous copper oxide, internal layer
For cobalt-based spinelle.
Embodiment the result shows that, it is double-deck that the present invention on the stainless steel connector surface SOFC applies copper oxide/cobalt-based spinelle
Coating utilizes the contact with the copper oxide outer layer of Cr affinity difference to completely isolated Spinel containing Cr and cathode atmosphere.This
Outside, by the way that rationally, cleverly design concept, the present invention propose that a kind of SOFC stainless steel connector copper oxide surface/cobalt-based point is brilliant
The preparation method of stone duplex coating, it is then oxidation-treated to prepare the protective coating using plating Cu-Co alloy.To effectively
It solves stainless steel connector existing oxidation film during usage and increases electricity caused by caused resistivity increase and Cr volatilization
Pond " poisoning of cathode " problem has the development of SOFC stainless steel connector surface conductance, antioxidant coating technology theoretical and real
Border meaning.
Claims (10)
1. a kind of solid oxide fuel cell stainless steel connector surface protection coating, which is characterized in that the coating is by bilayer
Structure composition, outer layer are continuous copper oxide, and internal layer is continuous cobalt-based spinel layer, and total coating thickness is not less than 3 μm.
2. solid oxide fuel cell stainless steel connector surface protection coating as described in claim 1, which is characterized in that
By atomic percentage, the Cu/Co in coating is 1:8~2:1.
3. solid oxide fuel cell stainless steel connector surface protection coating as described in claim 1, which is characterized in that
The general formula of internal layer cobalt-based spinelle is Co3-xMxO4, 0≤x≤2.5；Wherein, M Cr, one kind of Fe, Mn, Cu, Ni element or two
Kind or more.
4. solid oxide fuel cell stainless steel connector surface protection coating as claimed in claim 1 or 3, feature exist
In there are component gradients in cobalt-based spinel layer, and wherein M element content subtracts with the increase of coating/basal body interface distance
It is few.
5. a kind of solid oxide fuel cell stainless steel connector surfacecti proteon as described in any one of claims 1 to 4
The preparation method of coating, which comprises the steps of:
(1) preparation of plating solution: by mantoquita, cobalt salt and complexing agent by the mixing of required stoichiometric ratio and soluble in water, adjusting plating solution
PH value be 3~8, that is, obtain needed for plating solution；
(2) using plating solution obtained by step (1), in stainless steel base surface electro-deposition Cu-Co coating, sedimentation time is 10~
120min, coating layer thickness are not less than 2 μm；
(3) the Cu-Co coating is subjected to high temperature oxidation process under the conditions of 500~900 DEG C in oxygen-containing atmosphere, i.e., stainless
Steel matrix surface obtains copper oxide/cobalt-based spinelle coating.
6. the preparation method of solid oxide fuel cell stainless steel connector surface protection coating as claimed in claim 5,
It is characterized in that, the molar concentration of mantoquita is 0.01~5mol/L in step (1), the molar concentration of cobalt salt is 0.01~5mol/
L。
7. the preparation method of solid oxide fuel cell stainless steel connector surface protection coating as claimed in claim 5,
It is characterized in that, complexing agent is citrate complexing agent in step (1), molar concentration is 0~10mol/L.
8. the preparation method of solid oxide fuel cell stainless steel connector surface protection coating as claimed in claim 5,
It is characterized in that, plating solution composition is also comprising one in supporting electrolyte, buffer, anode activating agent and additive in step (1)
Kind is two or more.
9. the preparation method of solid oxide fuel cell stainless steel connector surface protection coating as claimed in claim 5,
It is characterized in that, in step (2): electrodeposition process is galvanostatic method, and current density is 1~20mAcm-2；Alternatively, electrodeposition process
For potentiostatic method, plating current potential is -0.8~-1.2VSCE。
10. the preparation method of solid oxide fuel cell stainless steel connector surface protection coating as claimed in claim 5,
It is characterized in that, after Cu-Co coating obtained by step (2) carries out the processing of high-temperature low-oxygen pressure, then step (3) are carried out, the high temperature is low
Oxygen pressure treatment process are as follows: in inert atmosphere, vacuum atmosphere or reducing atmosphere, hot place is carried out under the conditions of 300~900 DEG C
Reason, processing time are 0.5~10h.
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