CN107275656A - SOFC spinelle/metal connector composite and preparation method thereof - Google Patents
SOFC spinelle/metal connector composite and preparation method thereof Download PDFInfo
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- CN107275656A CN107275656A CN201710426053.3A CN201710426053A CN107275656A CN 107275656 A CN107275656 A CN 107275656A CN 201710426053 A CN201710426053 A CN 201710426053A CN 107275656 A CN107275656 A CN 107275656A
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- metal connector
- sofc
- powder
- spinelle
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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
- H01M8/0223—Composites
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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
It is using stainless steel as matrix, in the Cu Mn Co alloy coats that surface plasma coating thickness is 10~25um the invention discloses a kind of SOFC spinelle/metal connector composite and preparation method thereof;Raw material is the mixture of Cu powder, Mn powder and Co powder;Before spraying, matrix surface is subjected to sandblasting roughening, pre-oxidation generation pre-oxidation layer, drying;Spray power is 25~30Kw, 80~85Lmin of primary air amount‑1, 4~10gmin of powder feeding rate‑1, spray away from 90~95mm.In 750~800 DEG C of 10~20h of pre-sintering after spraying.The Cu Mn Co spinelles coatings that the present invention is prepared can effectively improve metal connector high-temperature oxidation resistance and electric conductivity under SOFC oxidation working environment, suppress Cr and poison from the external diffusion generation negative electrode in base material.
Description
Technical field
The invention belongs to high temperature field of solid oxide fuel, particularly to one kind uses plasma spray
Apply the Cu-Mn-Co spinelles/metal connector composite with pyroconductivity and high-temperature oxidation resistance prepared, application
Metallic interconnection materials are used as in SOFC.
Background technology
SOFC (Solid oxide fuel cell, SOFC) is a kind of chemical energy by fuel
The electrochemical appliance of electric energy is converted directly into by electrode reaction.Due to no burning and mechanical process, SOFC chemistry-electric energy
Amount conversion efficiency is up to 85%, while the features such as having pollution-free and noiseless.In general, SOFC operating temperature is 800
DEG C~1000 DEG C, high operating temperature means that fuel can be reformed in fuel battery inside and avoid outside reformation, and
The high-quality byproduct produced is that heat energy can be used for cogeneration of heat and power;While different types of hydrocarbon fuels, such as oxygen, first
Institute, natural gas etc. can be used for cogeneration of heat and power.Another advantage that high operating temperature is brought is to substantially improve kinetics,
So that SOFC no longer needs metallic catalyst.With the development of middle low temperature SOFC technologies, the reduction of battery operating temperature to adopt
Prepared metal connector with high temperature resistant, Antioxidant alloy material and be possibly realized.With ceramic material LaCrO3Compare, metal alloy tool
There are good air-tightness, electrical conductivity and thermal conductivity height, bipolar plates uniformity of temperature profile, high mechanical strength and cost easy to process low aobvious
Write advantage.High-temperature oxidation resistant alloy is considered as that can be applied to one of most promising metallic interconnection materials of middle low temperature SOFC at present,
But, easily poison cell cathode etc. urgently there is also the Cr for mismatching and volatilizing with YSZ electrolyte thermal coefficient of expansion
The problem of solution.
In recent years, the coating material that can be applied to SOFC metal connectors barrier layer is widely studied, current coating material
Material is broadly divided into following four classes material:Active element oxide, RE perovskite oxide, spinel oxide and MAlCrYO
High-temperature resistant alloy material.Active element oxide refers mainly to the oxide of the elements such as Y, La, Ce, Hf, and this type oxide can have
Effect ground improves oxide layer and metallic matrix adhesion, reduces the thickness of oxide layer, it is possible to be effectively reduced the height of alloy substrate
Warm oxidation rate, main cause is that the affinity of Y, La, Ce, Hf isoreactivity element and oxygen is stronger, and they can be to oxygen activity highest
Superficial layer migration and in the grain boundaries segregation (active element ionic radius is relatively large) of oxide layer, so as to prevent other ions
(such as Cr) to external migration and reduction interface Lacking oxygen number.Elisabetta Tondo etc. are existed by galvanoplastic
AISI430 stainless steel surfaces prepare Y2O3、Y2O3/Au、Y2O3/Co3O4Deng composite coating, Y is found2O3It can be volatilized with matrix
The chromium gone out forms the perovskite structure oxide of conduction, and this layer of oxide can be effectively reduced the oxidation rate of matrix, reduces
Contact resistance, eliminates the cracking of oxide skin(coating).Perovskite structure oxide (ABO3) can be by adulterating (Sr, Fe, Cu etc.) at B
Adjust its electronic conductivity and thermal coefficient of expansion.Not only electrical conductivity is higher but also can be following point for RE perovskite type coating
Spar oxide skin(coating) provides active element (such as La, Mn), improves the oxidation behavior on barrier layer.Because perofskite type oxide
Belong to oxygen ion conductor and prepares coating is not fine and close enough, it is impossible to effectively stop Cr past external diffusion and the inside diffusion of oxygen.
Spinel oxides (AB2O4) coating has good electric conductivity, while the thermal expansion system with battery miscellaneous part
Count also comparison match.Above all spinelle coating is fine and close and with good absorption Cr ability, therefore is metal alloy
The quality material of surface barrier.(Mn,Co)3O4、(Cu,Mn)3O4、(Cu,Fe)3O4And Co3O4Deng spinel strucutre oxides
Calorifics and electric property are excellent, with the thermal coefficient of expansion close with metal alloy, therefore are suitable for being applied to metal connector
Coating for surface protection.
The content of the invention
Negative electrode is easily caused under solid oxidized fuel working environment in order to solve metal connector to poison and resistance to high temperature oxidation
It is the problem of scarce capacity, multiple with spinelle/metal connector it is an object of the invention to provide a kind of SOFC
Condensation material, with pyroconductivity and high-temperature oxidation resistance
Another object of the present invention is to provide a kind of SOFC spinelle/metal connector composite wood
The preparation method of material, is to prepare Cu-Mn-Co spinelle coatings using the method for plasma spraying, and pre- by 800 DEG C of high temperature
Oxidation generation Cr2O3Thermally grown layer, can suppress the external diffusion of Cr elements and the interior diffusion of O elements.
Addition element Cu can dramatically increase (Mn, Co) 3O4 spinelles stability and electric conductivity.The electric conductivity of spinelle by
Transition is produced between Mn3+ and Mn4+ of the electronics on octahedral site, and the size of electrical conductivity depends on Mn3+ and Mn4+ on B positions
Concentration and ratio.Cu doping, the cation on A or B positions is may replace according to addition concentration, and B have priority.Due to Cu
+ can exist simultaneously with Cu2+ ions, different valence state cation is conducive to increasing conductance in octahedral site, and improves composite wood
Expect performance, this has good application value.
SOFC spinelle/metal connector composite, is using stainless steel as matrix, on surface
Plasma spraying thickness is the thick Cu-Mn-Co alloy coats of 10~25um;
The preparation method of SOFC spinelle/metal connector composite, step is as follows:
(1), by Cu powder, Mn powder and Co powder in molar ratio (0.1~0.5):(0.9~0.5):2 mixing;Using lapping using star lapping machine
Machine ball milling mixing 3~7h of powder, is sufficiently mixed it;
(2) by metal connector matrix surface carry out sandblasting roughening treatment, sandblasting air pressure be 0.5~1Mpa, time 30s~
90s;Described metal connector matrix is stainless steel;
(3) after surface coarsening processing, matrix is pre-oxidized into 40~100h generations pre-oxidation layer in 750~800 DEG C and dried
It is dry;
(4) before spraying, mixed metal powder is put into 300 DEG C of drying 3h~5h of baking oven;
(5) plasma spray is used to be coated in matrix surface coating thickness for Cu-Mn-Co alloy coats thick 10~25um;Institute
It is that spray power is 25~30Kw, 80~85Lmin of primary air amount to state Plasma Spray Parameters-1, 4~10gmin of powder feeding rate-1, spray away from 90~95mm;
(6) in 750~800 DEG C of 10~20h of pre-sintering after spraying, obtain Cu-Mn-Co spinelles/metal connector and be combined
Material, thermal coefficient of expansion 11-12x10-6K, 800 DEG C of area specific resistance 10~30m Ω cm2。
Beneficial effect:(1) present invention prepares Cu-Mn-Co spinelle coatings, the coating of preparation using plasma spraying method
Thickness is 10~25um, has good high-temperature electric conduction performance and high temperature antioxygen under SOFC working environment
Change performance;Cr can effectively be suppressed2O3The growth of oxide layer, prevents Cr elements in matrix from poisoning to matrix external diffusion generation negative electrode;
(2) Cu-Mn-Co spinelles coating has the thermal coefficient of expansion and chemical compatibility that match with metal connector, is conducive to battery
Stability improve service life.(3) 800 DEG C of pre-oxidation generation Cr of high temperature are passed through2O3Thermally grown layer, can suppress Cr elements
External diffusion and the interior diffusion of O elements.
Brief description of the drawings
Fig. 1 is Cu-Mn-Co alloy coat shape appearance figures after the thermal spraying of embodiment 5;
Fig. 2 is that Cu-Mn-Co alloy coats are heat-treated 20h shape appearance figures at 800 DEG C after the thermal spraying of embodiment 5.
Embodiment
Illustrate technical scheme below with reference to specific embodiment:
Cu powder, Mn powder, Co powder employed in embodiment are 100 mesh;The matrix used is SUS304 stainless steel base;
During plasma spraying, spray gun sweeps lateral separation 400mm once, and spray gun is vertically moved apart from 1mm, and spray gun sweeps speed and is
200mm·min-1.Before dusty spray, plasma gun is opened, base material is preheated.
Embodiment 1
SOFC metal connector surface C u-Mn-Co spinelle coatings are prepared using plasma spraying:
(1) by 100 mesh Cu powder, 100 mesh Mn powder and 100 mesh Co powder in molar ratio 0.1:0.9:2 mixing.Using lapping using star lapping machine
Machine ball milling mixing powder 3h.
(2) by SUS304 stainless steel base wire cuttings, surface carries out sandblasting roughening treatment, and sandblasting air pressure is 0.5Mpa, when
Between 90s;
(3) after surface coarsening processing, sample is put into 800 DEG C of pre-oxidation 100h of chamber type electric resistance furnace;
(4) before spraying, mixed metal powder is put into 300 DEG C of drying 3h of baking oven.Plasma Spray Parameters, spray power is
25Kw, primary air amount 80Lmin-1, powder feeding rate 4gmin-1, spray away from 90mm.Spray gun running parameter, spray gun sweeps horizontal stroke once
To apart from 400mm, spray gun is vertically moved apart from 1mm, and it is 200mmmin that spray gun, which sweeps speed,-1.Before dusty spray, open etc. from
Sub- spray-painting gun, base material is preheated.By spraying, it is Cu- thick 10um to prepare thickness in SUS304 stainless steel surfaces
Mn-Co alloy coats;
(5) after spraying, sample is put into 800 DEG C of sintering 10h in chamber type electric resistance furnace, and dense uniform is generated in matrix surface
Cu-Mn-Co spinelle coatings.
Cu-Mn-Co spinelles coating is combined closely with stainless steel base, and the effective external diffusion for inhibiting Cr elements,
Cr2O3The thickness of thermally grown layer is less than 1um.Area specific resistance of the Cu-Mn-Co spinelles coating under 800~900 DEG C of operating temperatures
Scope is 13.9~17.60m Ω cm2。
Embodiment 1-5 technological parameter is as shown in table 1, other guide be the same as Example 1:
Table 1
Wherein, area specific resistance (unit m Ω cm when area specific resistance is 800~900 DEG C2), thermal coefficient of expansion is 800~
Thermal coefficient of expansion (unit K under 900 DEG C of operating temperatures-1)。
Embodiment 1-5 is generating the Cu-Mn-Co spinelle coatings of dense uniform in matrix surface, with stainless steel base
Combine closely, and effectively inhibit the external diffusion of Cr elements;The gained Cu-Mn-Co spinelles coating of embodiment 3 is at 800 DEG C
1000h is aoxidized, the thickness of rich Cr oxide layers only has 0.75um, shows that Cu-Mn-Co spinelle coatings have fabulous high temperature resistance oxygen
Change performance, it is effective to prevent poisoning effect of the Cr elements external diffusion to cell cathode in matrix.
Claims (5)
1. SOFC spinelle/metal connector composite, it is characterised in that be using stainless steel as base
Body, is the thick Cu-Mn-Co alloy coats of 10~25um in surface plasma coating thickness.
2. the preparation method of SOFC spinelle/metal connector composite described in claim 1,
Characterized in that, step is as follows:
(1), by Cu powder, Mn powder and Co powder in molar ratio (0.1~0.5):(0.9~0.5):2 mixing;
(2) metal connector matrix surface is subjected to sandblasting roughening treatment, described metal connector matrix is stainless steel;
(3) after surface coarsening processing, matrix is pre-oxidized into 40~100h generations pre-oxidation layer and drying in 750~800 DEG C;
(4) plasma spray is used to be coated in Cu-Mn-Co alloy coat of the matrix surface coating thickness for 10~25um;Parameter is spray
Painting power is 25~30Kw, 80~85Lmin of primary air amount-1, 4~10gmin of powder feeding rate-1, spray away from 90~95mm;
(5) in 750~800 DEG C of 10~20h of pre-sintering after spraying, Cu-Mn-Co spinelles/metal connector composite is obtained,
Thermal coefficient of expansion 11-12x10-6K, 800 DEG C of area specific resistance 10~30m Ω cm2。
3. the preparation method of SOFC spinelle/metal connector composite described in claim 2,
Characterized in that, hybrid mode makes to use 3~7h of star lapping machine ball milling mixing powder in step (1).
4. the preparation method of SOFC spinelle/metal connector composite described in claim 2,
Characterized in that, blasting craft is in step (2):Air pressure is 0.5~1Mpa, time 30s~90s.
5. the preparation method of SOFC spinelle/metal connector composite described in claim 2,
Characterized in that, the stoving process of step (3) is 300 DEG C of drying 3h~5h.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108998789A (en) * | 2018-07-23 | 2018-12-14 | 景德镇陶瓷大学 | A kind of alloy connector and preparation method thereof of surface cladding Mn-Co spinelle coating |
CN112204781A (en) * | 2018-06-20 | 2021-01-08 | 株式会社Lg化学 | Connecting material for solid oxide fuel cell, method of manufacturing the same, and solid oxide fuel cell including the same |
CN112331893A (en) * | 2020-10-28 | 2021-02-05 | 华中科技大学 | Flat-plate type solid oxide fuel cell and sealing method thereof |
CN113328113A (en) * | 2021-05-28 | 2021-08-31 | 广东省科学院新材料研究所 | Preparation method of solid oxide fuel cell/electrolytic cell connector |
CN114243047A (en) * | 2021-12-14 | 2022-03-25 | 中国科学院大连化学物理研究所 | Method for preparing metal surface coating at low temperature |
CN116121701A (en) * | 2023-03-03 | 2023-05-16 | 青岛大学 | Modified composite three-layer coating of fuel cell metal connector and preparation method thereof |
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CN106571476A (en) * | 2016-11-14 | 2017-04-19 | 江苏科技大学 | Coating material of metallic interconnector for high-temperature fuel cells and preparation method thereof |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112204781A (en) * | 2018-06-20 | 2021-01-08 | 株式会社Lg化学 | Connecting material for solid oxide fuel cell, method of manufacturing the same, and solid oxide fuel cell including the same |
CN108998789A (en) * | 2018-07-23 | 2018-12-14 | 景德镇陶瓷大学 | A kind of alloy connector and preparation method thereof of surface cladding Mn-Co spinelle coating |
CN108998789B (en) * | 2018-07-23 | 2020-04-28 | 景德镇陶瓷大学 | Alloy connector with surface coated with Mn-Co spinel coating and preparation method thereof |
CN112331893A (en) * | 2020-10-28 | 2021-02-05 | 华中科技大学 | Flat-plate type solid oxide fuel cell and sealing method thereof |
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 |
CN113328113A (en) * | 2021-05-28 | 2021-08-31 | 广东省科学院新材料研究所 | Preparation method of solid oxide fuel cell/electrolytic cell connector |
CN113328113B (en) * | 2021-05-28 | 2022-07-12 | 广东省科学院新材料研究所 | Preparation method of solid oxide fuel cell/electrolytic cell connector |
CN114243047A (en) * | 2021-12-14 | 2022-03-25 | 中国科学院大连化学物理研究所 | Method for preparing metal surface coating at low temperature |
CN114243047B (en) * | 2021-12-14 | 2023-11-10 | 中国科学院大连化学物理研究所 | Method for preparing metal surface coating at low temperature |
CN116121701A (en) * | 2023-03-03 | 2023-05-16 | 青岛大学 | Modified composite three-layer coating of fuel cell metal connector and preparation method thereof |
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Effective date of registration: 20201218 Address after: 214500 East head of Dunyi bridge, Jingjiang City, Taizhou City, Jiangsu Province Patentee after: JIANGSU YONGHAO HIGH-STRENGTH BOLT Co.,Ltd. Address before: 212003, No. 2, Mengxi Road, Zhenjiang, Jiangsu Patentee before: JIANGSU University OF SCIENCE AND TECHNOLOGY |