CN105239050B - A kind of preparation method of solid oxide fuel cell stainless steel connector spinel oxide protective coating - Google Patents
A kind of preparation method of solid oxide fuel cell stainless steel connector spinel oxide protective coating Download PDFInfo
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- CN105239050B CN105239050B CN201510771263.7A CN201510771263A CN105239050B CN 105239050 B CN105239050 B CN 105239050B CN 201510771263 A CN201510771263 A CN 201510771263A CN 105239050 B CN105239050 B CN 105239050B
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Abstract
A kind of preparation method of solid oxide fuel cell stainless steel connector spinel oxide protective coating, it is related to a kind of preparation method of solid oxide fuel cell stainless steel connector spinel oxide protective coating.The protective coating film hole for preparing the present invention is to solve conventional method is more, in conjunction with force difference, the problem of cannot preparing the spinel oxide film of suitable thickness.Method：One, it is cleaned by ultrasonic；Two, pre-sputtering is handled；Three, prepared by alloy firm；Four, prepared by protective coating.The film prepared through the present invention is fine and close, and binding force is good, and coating layer thickness is adjustable；High-temperature oxidation resistance is good, and interface resistance is low；It is good to hinder Cr performances, effectively prevent the poisoning of cathode.The present invention is used to apply on solid oxide fuel cell stainless steel connector surface plus protective layer.
Description
Technical field
The present invention relates to a kind of systems of solid oxide fuel cell stainless steel connector spinel oxide protective coating
Preparation Method.
Background technology
Solid oxide fuel cell (Solid Oxide Fuel Cell, SOFC) is that one kind can be directly by chemical energy
It is converted into the energy device of electric energy, as a kind of all solid state high-temperature fuel cell, the risk of electrolyte leakage, operation is not present
Temperature is high, and cheap metal oxide can be used and substitute noble metal as catalysis material, additionally have energy conversion efficiency high,
Suitability of fuel is wide, Environmental compatibility well equal remarkable advantages, in distributed power station, household cogeneration system, and as ship
The electrical source of power of oceangoing ship, vehicle etc. has a wide range of applications, and becomes the new energy technology that various countries competitively develop.
According to the operation principle of hydrogen-oxygen fuel cell, SOFC single batteries are only capable of the voltage of 0.7~0.8V of offer or so, are
The voltage request for meeting practical application, needing single battery being together in series constitutes battery pile.Between two single batteries, adopt
It is connected with fine and close connector, on the one hand connector plays a part of to conduct electric current, fuel gas and oxygen on the other hand can also be isolated
Change gas, and groove existing for surface plays the role of providing gas passage.Due to solid oxide fuel cell operating temperature
It is higher therefore more demanding for metallic interconnection materials, other than it is with good electric conductivity, it is also necessary to which there is stability, gas
Close property, thermal conductivity, and its coefficient of thermal expansion should match with the other components of battery, should additionally have preferable antioxygen
Change, chromium poison ability, have sufficiently high intensity and the performances such as creep-resistant property and plasticity are good at high temperature.
As SOFC operating temperatures are reduced to middle low temperature (600~800 DEG C) from high temperature (1000 DEG C), there is excellent conduction
Property, high intensity is inexpensive, and the stainless steel material of preferable processing performance causes extensive concern as metallic interconnection materials.Especially iron
The electricity of ferritic base stainless steel material (SUS430, SUS441, ZMG232L, ZMG232J3, ZMG232G10, APU22 etc.) and SOFC
Pole material, electrolyte and sealing material have good thermal matching and chemical stability, and its oxidation resistance compared with
Good, cost is relatively low, is the preferred material of SOFC connectors.But under SOFC operating temperatures, stainless steel connector oxidation rate
Higher, oxide layer is easy to fall off, and the Cr elements for playing antioxidation in stainless steel material can be sent out during the work time
Raw volatilization, causes cathode Cr intoxicating phenomenons occur, to affect the performance of battery pile.By in stainless steel connector surface system
Standby protective layer, can improve the oxidation resistance of stainless steel connector, additionally it is possible to reduce the interface electricity between connector and electrode
Resistance, and can stop the volatilization of Cr elements during the work time, it prevents cathode from poisoning, improves the steady in a long-term of battery pile
Property.
Spinel oxide material (Co3O4, (Mn, Co) 3O4, (Cu, Mn) 3O4) has higher electric conductivity, with iron element
Body thermal expansion coefficient of stainless steel matches, and the diffusion of blocking Cr elements is can be very good under high temperature, cathode can be preferably protected, be
A kind of excellent SOFC stainless steel connector protective coating materials.Traditional protective coating preparation method has silk screen print method, spray
Coating, electrochemical co-deposition method etc..Protective coating hole prepared by silk-screen printing or spraying method is more, with basal body binding force
Difference is not easy to obtain film, and in the long-term test process of high temperature, the oxidation film layer of matrix surface is thicker, reduces membranous layer binding force, no
Conducive to the long-time stability of SOFC.The difficulty of electrochemical co-deposition is larger, can not prepare the protective coating film of suitable thickness.
Invention content
The present invention is to solve conventional method prepare protective coating film hole it is more, in conjunction with force difference, cannot prepare suitable
The problem of spinel oxide film of thickness, and a kind of solid oxide fuel cell stainless steel connector spinelle oxygen is provided
The preparation method of compound protective coating.
One, it is cleaned by ultrasonic：It is clear that ferrite base stainless steel is put into acetone ultrasound under conditions of supersonic frequency is 40kHz
It washes twice, it is 8min~15min, the ferrite base stainless steel after being ultrasonically treated to be cleaned by ultrasonic the time every time；
Two, pre-sputtering is handled：It is indoor that ferrite base stainless steel after supersound process that step 1 obtains is put into vacuum
On sample table, it is 1.0 × 10 to be evacuated to vacuum degree-4Pa~1.0 × 10-3Pa, in voltage be 100V~200V and air pressure is
Pre-sputter cleaning 10min~30min is carried out under conditions of 10Pa, obtains pre-sputtering treated ferrite base stainless steel；
Three, prepared by alloy firm：Alloy target material is fixed on target position, then uses high power pulsed source to step 2
Deposit alloy film on the surface of obtained pre-sputtering treated ferrite base stainless steel is 500V~700V, electricity in voltage
Stream be 10A~120A, the condition that ar pressure is 0.5~1.5Pa, pulsewidth is 50 μ of μ s~200 s and frequency 100Hz~500Hz
Under deposited, sedimentation time is 0.5h~5h, is cooled to room temperature after the completion of deposition, and obtaining surface deposition has the iron of alloy firm
Ferritic base stainless steel；
Four, prepared by protective coating：There is the ferrite base stainless steel of alloy firm to be placed in the surface deposition that step 3 obtains
In air furnace, under conditions of heating rate is 3 DEG C/min, by the temperature in air furnace from room temperature to keeping the temperature after 750 DEG C
1h, then rate of temperature fall be 3 DEG C/min under conditions of, the temperature in air furnace is cooled to 100 DEG C from 750 DEG C, then with
Stove is cooled to room temperature, and is obtained to surface and is covered with the ferrite base stainless steel of spinel oxide protective coating；The surface is covered with point
The thickness of the spinel oxide protective coating of the ferrite base stainless steel surface of spar oxide protective layer is 0.1 μm~10
μm。
The beneficial effects of the invention are as follows：
By the present invention in that preparing alloy film with the method for high-power impulse magnetron sputtering, and point is prepared by making annealing treatment
Spar oxide protective layer is prepared for densification, and binding force is good, the protective coating that thickness is adjustable (0.1 μm~10 μm).The present invention
It has the following advantages：
1, it is prepared for densification, binding force is good, the adjustable protective coating of coating layer thickness；Protective coating is fine and close, without hole, adopts
With different parameters, the film of different-thickness can be prepared, from nanoscale to micron order.
2, high-temperature oxidation resistance is good, and interface resistance is low.
3, resistance Cr performances are good, effectively prevent the poisoning of cathode；The film prepared through the invention, at 750 DEG C, work 500 is small
Shi Hou, film surface Cr contents are 0, and Cr is effectively prevent to volatilize, and protect cathode.
Description of the drawings
Fig. 1 is the surface for the ferrite base stainless steel that the surface that embodiment one obtains is covered with spinel oxide protective coating
Shape appearance figure.
Specific implementation mode
Specific implementation mode one：A kind of solid oxide fuel cell stainless steel connector spinelle oxidation of present embodiment
The preparation method of object protective coating is to carry out according to the following steps：
One, it is cleaned by ultrasonic：It is clear that ferrite base stainless steel is put into acetone ultrasound under conditions of supersonic frequency is 40kHz
It washes twice, it is 8min~15min, the ferrite base stainless steel after being ultrasonically treated to be cleaned by ultrasonic the time every time；
Two, pre-sputtering is handled：It is indoor that ferrite base stainless steel after supersound process that step 1 obtains is put into vacuum
On sample table, it is 1.0 × 10 to be evacuated to vacuum degree-4Pa~1.0 × 10-3Pa, in voltage be 100V~200V and air pressure is
Pre-sputter cleaning 10min~30min is carried out under conditions of 10Pa, obtains pre-sputtering treated ferrite base stainless steel；
Three, prepared by alloy firm：Alloy target material is fixed on target position, then uses high power pulsed source to step 2
Deposit alloy film on the surface of obtained pre-sputtering treated ferrite base stainless steel is 500V~700V, electricity in voltage
Stream be 10A~120A, the condition that ar pressure is 0.5~1.5Pa, pulsewidth is 50 μ of μ s~200 s and frequency 100Hz~500Hz
Under deposited, sedimentation time is 0.5h~5h, is cooled to room temperature after the completion of deposition, and obtaining surface deposition has the iron of alloy firm
Ferritic base stainless steel；
Four, prepared by protective coating：There is the ferrite base stainless steel of alloy firm to be placed in the surface deposition that step 3 obtains
In air furnace, under conditions of heating rate is 3 DEG C/min, by the temperature in air furnace from room temperature to keeping the temperature after 750 DEG C
1h, then rate of temperature fall be 3 DEG C/min under conditions of, the temperature in air furnace is cooled to 100 DEG C from 750 DEG C, then with
Stove is cooled to room temperature, and is obtained to surface and is covered with the ferrite base stainless steel of spinel oxide protective coating；The surface is covered with point
The thickness of the spinel oxide protective coating of the ferrite base stainless steel surface of spar oxide protective layer is 0.1 μm~10
μm。
Present embodiment prepares alloy film by using the method for high-power impulse magnetron sputtering, and is made by making annealing treatment
Standby spinel oxide protective coating, is prepared for densification, binding force is good, the protective coating that thickness is adjustable (0.1 μm~10 μm).This
Embodiment has the following advantages：
1, it is prepared for densification, binding force is good, the adjustable protective coating of coating layer thickness；Protective coating is fine and close, without hole, adopts
With different parameters, the film of different-thickness can be prepared, from nanoscale to micron order.
2, high-temperature oxidation resistance is good, and interface resistance is low.
3, resistance Cr performances are good, effectively prevent the poisoning of cathode；The film prepared through the invention, at 750 DEG C, work 500 is small
Shi Hou, film surface Cr contents are 0, and Cr is effectively prevent to volatilize, and protect cathode.
Specific implementation mode two：The present embodiment is different from the first embodiment in that：Ferrite described in step 1
Base stainless steel be SUS430 stainless steels, SUS441 stainless steels, ZMG232L stainless steels, ZMG232J3 stainless steels, ZMG232G10 not
Become rusty steel or APU22 stainless steels.Other are same as the specific embodiment one.
Specific implementation mode three：The present embodiment is different from the first and the second embodiment in that：In voltage in step 2
Pre-sputter cleaning 20min is carried out under conditions of being 10Pa for 100V~200V and air pressure.Other and specific implementation mode one or two
It is identical.
Specific implementation mode four：Unlike one of present embodiment and specific implementation mode one to three：Institute in step 3
It is CoMn alloys targets to state alloy target material, and it is 10%~90% that wherein Co constituent contents, which are 10%~90%, Mn constituent contents,.Other
It is identical as one of specific implementation mode one to three.
Specific implementation mode five：Unlike one of present embodiment and specific implementation mode one to four：Institute in step 3
It is CuMn alloys targets to state alloy target material, and it is 10%~90% that wherein Cu constituent contents, which are 10%~90%, Mn constituent contents,.Other
It is identical as one of specific implementation mode one to four.
Specific implementation mode six：Unlike one of present embodiment and specific implementation mode one to five：Institute in step 3
It is 67Co33Mn targets to state alloy target material.Other are identical as one of specific implementation mode one to five.
Specific implementation mode seven：Unlike one of present embodiment and specific implementation mode one to six：In step 3
Voltage is 600V, electric current 80A, under conditions of ar pressure 1Pa, pulsewidth are 100 μ s and frequency 200Hz.Other with it is specific
One of embodiment one to six is identical.
Specific implementation mode eight：Unlike one of present embodiment and specific implementation mode one to seven：It sinks in step 3
The product time is 3h.Other are identical as one of specific implementation mode one to seven.
Specific implementation mode nine：Unlike one of present embodiment and specific implementation mode one to eight：It sinks in step 3
The product time is 4h.Other are identical as one of specific implementation mode one to eight.
Specific implementation mode ten：Unlike one of present embodiment and specific implementation mode one to nine：It covers on the surface
It is 5 μm to have the thickness of the spinel oxide protective coating of the ferrite base stainless steel surface of spinel oxide protective coating.
Other are identical as one of specific implementation mode one to nine.
Beneficial effects of the present invention are verified using following embodiment：
Embodiment one：A kind of preparation of solid oxide fuel cell stainless steel connector spinel oxide protective coating
Method is to carry out according to the following steps：
One, it is cleaned by ultrasonic：SUS430 stainless steels are put into acetone and are cleaned by ultrasonic under conditions of supersonic frequency is 40kHz
Twice, it is 10min, the SUS430 stainless steels after being ultrasonically treated to be cleaned by ultrasonic the time every time；
Two, pre-sputtering is handled：SUS430 stainless steels after supersound process that step 1 obtains are put into the indoor examination of vacuum
On sample platform, it is 1.0 × 10 to be evacuated to vacuum degree-4Pa~1.0 × 10-3Pa, in voltage be 100V~200V and air pressure is 10Pa
Under conditions of carry out pre-sputter cleaning 10min~30min, obtain pre-sputtering treated SUS430 stainless steels；
Three, prepared by alloy firm：Alloy target material is fixed on target position, then uses high power pulsed source to step 2
Deposit alloy film on the surface of obtained pre-sputtering treated SUS430 stainless steels is 500V~700V, electric current in voltage
For 10A~120A, under conditions of ar pressure is 0.5~1.5Pa, pulsewidth is 50 μ of μ s~200 s and frequency 100Hz~500Hz
It is deposited, sedimentation time is 0.5h~1.5h, is cooled to room temperature after the completion of deposition, and obtaining surface deposition has alloy firm
SUS430 stainless steels；
Four, prepared by protective coating：There are the SUS430 stainless steels of alloy firm to be placed in sky the surface deposition that step 3 obtains
In steam stove, under conditions of heating rate is 3 DEG C/min, by the temperature in air furnace from room temperature to keeping the temperature 1h after 750 DEG C,
Then under conditions of rate of temperature fall is 3 DEG C/min, the temperature in air furnace is cooled to 100 DEG C from 750 DEG C, then with furnace cooling
But it to room temperature, obtains to surface and is covered with the SUS430 stainless steels of spinel oxide protective coating；The surface is covered with spinelle oxygen
The thickness of the spinel oxide protective coating of the SUS430 stainless steel surfaces of compound protective coating is 0.1 μm~10 μm.
Fig. 1 is the surface for the ferrite base stainless steel that the surface that embodiment one obtains is covered with spinel oxide protective coating
Shape appearance figure；The present invention is prepared for densification as can be seen from Figure 1, and binding force is good, the adjustable protective coating of coating layer thickness；Protective coating
Densification, without hole.
The surface that embodiment one obtains is covered with the SUS430 stainless steels of spinel oxide protective coating in oxidation 500h
Afterwards, spinel oxide protective coating resistance value at 800 DEG C is 0.022ohm/cm2, surface is covered with spinel oxide protection and applies
The SUS430 stainless steels of layer resistance value at 800 DEG C is 0.088ohm/cm2。
Claims (6)
1. a kind of preparation method of solid oxide fuel cell stainless steel connector spinel oxide protective coating, feature
It is that a kind of preparation method of solid oxide fuel cell stainless steel connector spinel oxide protective coating is by following
Step carries out：
One, it is cleaned by ultrasonic：SUS430 stainless steels are put into acetone and are cleaned by ultrasonic two under conditions of supersonic frequency is 40kHz
Secondary, it is 8min~15min, the SUS430 stainless steels after being ultrasonically treated to be cleaned by ultrasonic the time every time；
Two, pre-sputtering is handled：SUS430 stainless steels after supersound process that step 1 obtains are put into the indoor sample table of vacuum
On, it is 1.0 × 10 to be evacuated to vacuum degree-4Pa~1.0 × 10-3Pa, in the item that voltage is 100V~200V and air pressure is 10Pa
Pre-sputter cleaning 10min~30min is carried out under part, obtains pre-sputtering treated SUS430 stainless steels；
Three, prepared by alloy firm：Alloy target material is fixed on target position, then step 2 is obtained using high power pulsed source
Pre-sputtering treated SUS430 stainless steels surface on deposit alloy film, voltage be 500V~700V, electric current 10A
~120A, ar pressure are 0.5~1.5Pa, pulsewidth is sunk under conditions of being 50 μ of μ s~200 s and frequency 100Hz~500Hz
Product, sedimentation time are 0.5h~5h, are cooled to room temperature after the completion of deposition, and obtaining surface deposition has the SUS430 of alloy firm stainless
Steel；The alloy target material is CuMn alloys targets, wherein Cu constituent contents be 10%~90%, Mn constituent contents be 10%~
90%；
Four, prepared by protective coating：There are the SUS430 stainless steels of alloy firm to be placed in air furnace the surface deposition that step 3 obtains
In, under conditions of heating rate is 3 DEG C/min, by the temperature in air furnace from room temperature to 1h is kept the temperature after 750 DEG C, then
Under conditions of rate of temperature fall is 3 DEG C/min, the temperature in air furnace is cooled to 100 DEG C from 750 DEG C, is then cooled to the furnace
Room temperature obtains to surface and is covered with the SUS430 stainless steels of spinel oxide protective coating；The surface is covered with spinel oxide
The thickness of the spinel oxide protective coating of the SUS430 stainless steel surfaces of protective coating is 0.1 μm~10 μm；Obtained table
Face is covered with the SUS430 stainless steels of spinel oxide protective coating after aoxidizing 500h, and spinel oxide protective coating exists
Resistance value is 0.022ohm/cm at 800 DEG C2, surface is covered with the SUS430 stainless steels of spinel oxide protective coating at 800 DEG C
Resistance value is 0.088ohm/cm2。
2. a kind of solid oxide fuel cell stainless steel connector spinel oxide protection according to claim 1 applies
The preparation method of layer, it is characterised in that splashed in advance under conditions of voltage is 100V~200V and air pressure is 10Pa in step 2
Penetrate cleaning 20min.
3. a kind of solid oxide fuel cell stainless steel connector spinel oxide protection according to claim 1 applies
Layer preparation method, it is characterised in that in step 3 voltage be 600V, electric current 80A, ar pressure 1Pa, pulsewidth 100
Under conditions of μ s and frequency 200Hz.
4. a kind of solid oxide fuel cell stainless steel connector spinel oxide protection according to claim 1 applies
The preparation method of layer, it is characterised in that sedimentation time is 3h in step 3.
5. a kind of solid oxide fuel cell stainless steel connector spinel oxide protection according to claim 1 applies
The preparation method of layer, it is characterised in that sedimentation time is 4h in step 3.
6. a kind of solid oxide fuel cell stainless steel connector spinel oxide protection according to claim 1 applies
The preparation method of layer, it is characterised in that the surface is covered with the ferrite base stainless steel surface of spinel oxide protective coating
The thickness of spinel oxide protective coating is 5 μm.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US11374231B2 (en) * | 2017-10-20 | 2022-06-28 | Lg Chem, Ltd. | Connecting material for solid oxide fuel cell, manufacturing method therefor, and solid oxide fuel cell |
| CN112195444A (en) * | 2020-08-17 | 2021-01-08 | 徐州华清智能装备有限公司 | Preparation method of solid oxide fuel cell stack connector protective coating |
| CN112331893B (en) * | 2020-10-28 | 2022-02-15 | 华中科技大学 | Flat-plate type solid oxide fuel cell and sealing method thereof |
| CN114318248A (en) * | 2021-12-17 | 2022-04-12 | 国家能源集团新能源有限责任公司 | Preparation method and application of manganese-cobalt spinel coating |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101068678A (en) * | 2004-11-30 | 2007-11-07 | 山特维克知识产权股份有限公司 | Fuel cell component comprising a complex oxide forming coating |
| CN102653858A (en) * | 2012-05-28 | 2012-09-05 | 哈尔滨工业大学深圳研究生院 | Method for preparing MnCo spinel protecting film by magnetron sputtering and subsequent oxidation |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009017841A2 (en) * | 2007-08-02 | 2009-02-05 | Trustees Of Boston University | Protective oxide coatings for sofc interconnections |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101068678A (en) * | 2004-11-30 | 2007-11-07 | 山特维克知识产权股份有限公司 | Fuel cell component comprising a complex oxide forming coating |
| CN102653858A (en) * | 2012-05-28 | 2012-09-05 | 哈尔滨工业大学深圳研究生院 | Method for preparing MnCo spinel protecting film by magnetron sputtering and subsequent oxidation |
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