CN102760890A - industrial production technology for novel direct sodium borohydride fuel battery cathode - Google Patents
industrial production technology for novel direct sodium borohydride fuel battery cathode Download PDFInfo
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- CN102760890A CN102760890A CN2012102637918A CN201210263791A CN102760890A CN 102760890 A CN102760890 A CN 102760890A CN 2012102637918 A CN2012102637918 A CN 2012102637918A CN 201210263791 A CN201210263791 A CN 201210263791A CN 102760890 A CN102760890 A CN 102760890A
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- nickel foam
- sodium borohydride
- fuel cell
- industrial production
- nitrogen
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- 239000000446 fuel Substances 0.000 title claims abstract description 34
- 238000005516 engineering process Methods 0.000 title claims abstract description 16
- 229910000033 sodium borohydride Inorganic materials 0.000 title claims abstract description 16
- 239000012279 sodium borohydride Substances 0.000 title claims abstract description 16
- 238000009776 industrial production Methods 0.000 title claims abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 87
- 239000006260 foam Substances 0.000 claims description 43
- 229910052759 nickel Inorganic materials 0.000 claims description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 229910021389 graphene Inorganic materials 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 14
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 7
- 238000009423 ventilation Methods 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 abstract 1
- 229910001385 heavy metal Inorganic materials 0.000 abstract 1
- 230000010354 integration Effects 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 210000004027 cell Anatomy 0.000 description 20
- 238000000034 method Methods 0.000 description 8
- 230000002209 hydrophobic effect Effects 0.000 description 7
- 238000011160 research Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 125000004355 nitrogen functional group Chemical group 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
Images
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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
-
- 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
Abstract
The invention discloses a large-scale industrial production technology for a novel direct sodium borohydride fuel battery cathode. In the technology, a carbon-nitrogen material not containing any heavy metal element is taken as a core catalyst, and preparation of a porous grapheme network carrier and nitrogen-doping integration treatment are performed. The prepared cathode has ultrahigh electrical conductivity, large surface specific area and superior catalytic activity. The technology has a simple and controllable cathode production process, and plays an important role in promoting direct practicability of a sodium borohydride fuel battery.
Description
Technical field
Present technique relates to the electrode preparation field, particularly direct sodium borohydride fuel cell negative electrode preparation field.
Background technology
Fuel cell is the generation technology that a kind of chemical energy that directly will be stored in the fuel is converted into electric energy; Because it has advantages such as the high and low discharging of energy conversion efficiency, pollution-free and noiselessness, the 4th kind of electricity-generating method outside be considered to continue firepower, waterpower, the nuclear energy.The exploitation non-precious metal catalyst is to reduce the fuel cell cost always, one of key issue of promotion fuel cell technology practicability [Michel Lefevre, Eric Proietti, Fr é d é ric Jaouen, et al., Science, 2009,
324: 71-74].
Graphene is that carbon atom is the individual layer two dimensional crystal material that the honeycomb lattice arrangement constitutes with the sp2 hybridized orbital, and it has unique physicochemical properties, like the theoretical specific area of height (about 2630 m
2g
-1), high chemical stability, high conductivity (106S cm
-1) and easy functionalization etc. [Dongsheng Geng, Songlan Yang, Yong Zhang, et al., Applied Surface Science, 2011,
257: 9193 – 9198], have important scientific research meaning and application prospects.The research synthetic and electrochemical properties of nitrogen-doped graphene recently receive extensive concern [Dongsheng Geng, Songlan Yang, Yong Zhang, et al., Applied Surface Science, 2011,
257: 9193 – 9198; Yuyan Shao, Sheng Zhang, Mark H, et al., Journal of Materials Chemistry, 2010,
20: 7491 – 7496; Liangti Qu, Yong Liu, Jong-Beom Baek, et al., Nano, 2010,
4: 1321 – 1326].Research shows, can effectively improve behind the nitrogen-doped graphene Graphene conductivity and corrosion resistance [Dongsheng Geng, Songlan Yang, Yong Zhang, et al., Applied Surface Science, 2011,
257: 9193 – 9198]; And people such as Shao research shows because the introducing of nitrogen functional group and surface texture defective, nitrogen-doped graphene to the catalytic activity of oxygen and hydrogen peroxide solution reduction reaction apparently higher than pure Graphene [Yuyan Shao; Sheng Zhang; Mark H, et al., Journal of Materials Chemistry; 2010
20: 7491 – 7496].This shows that nitrogen-doped graphene is a kind of very potential new material that is applied to fuel cell base metal cathod catalyst.The physical and chemical performance of Graphene and the number of plies of Graphene are closely related, and the Graphene of monoatomic layer has best physical and chemical performance in theory.Discover on the metallic nickel surface growth multi-layer graphene easily, and in growth course, be difficult to simply regulate and control the number of plies of Graphene through parameters such as control reaction constituent element, temperature.
On the other hand, since the fuel cell technology development, the preparation method of two kinds of the most frequently used fuel cell membrane electrodes is still in the low-temperature fuel cell: 1) catalyst layer is applied to gas diffusion layers, then increases film; 2) catalyst layer is applied to film, then increases gas diffusion layers [Ma Xin, Wang Shengkai, Chen Guoshun etc. are translated, fuel cell design and manufacturing, Electronic Industry Press, 2008 years].More than all add hydrophobic material (polytetrafluoroethylene) in the preparation of catalyst layer of two kinds of methods and realize three-phase reaction interface; Yet the variation of hydrophobic material addition directly has influence on the generating efficiency of the rate of catalysis reaction and the fuel cell of catalyst layer, has influenced the actual serviceability of battery to a certain extent.The hydrophobic processing procedure has increased the battery electrode preparation flow simultaneously, has improved the battery production cost.The electrode hydrophobic is handled and the negative electrode of development of new high catalytic activity in order to solve simultaneously, the invention provides a kind of large-scale industrial production technology of negative electrode of novel high catalytic activity.
Summary of the invention
High for the exploitation catalytic activity, can large-scale industrial production and can simplify the cathode preparation method of hydrophobic processing procedure; The present invention uses following thinking to address the above problem: utilize a cover reaction unit to realize that the growth of Graphene and the one-step method that nitrogen mixes prepare continuously; And this growing method can be through its number of plies of growth time regulation and control of Graphene; Utilize Graphene itself to have the hydrophobic processing that good hydrophobicity is exempted conventional negative electrode; Utilize Graphene good electrical conductivity and porous breathable property to serve as gas diffusion layers and conductive layer; Carry out nitrogen simultaneously on the Graphene surface and mix, the C-N active sites catalytic oxygen reduction of utilizing the nitrogen doping to form is served as catalyst layer, realizes the operate as normal of battery.Practical implementation process of the present invention is following: in the reactor that electronic rolling unwinding device is installed of airtight vacuum-pumping and ventilation atmosphere, the nickel foam volume is placed on the left side rotating shaft, one of nickel foam of extraction is passed the intermediate reaction district and is fixed in the right side rolling-up mechanism.Reactor is evacuated to 10
-2Pa and inflated with nitrogen vacuumize again, make the interior oxygen residual volume of reactor less than 10 repeatedly for several times
-4Pa.Intermediate reaction district temperature is risen to 1000
oC begins to feed methane, ammonia and nitrogen mixture body, starts right side transmission rolling-up mechanism simultaneously and makes nickel foam continuously through the intermediate reaction district.When the complete rolling of nickel foam stops heating and ventilation behind the right side, make reactor temperature be reduced to 100
oOpen reactor after below the C and take out the nickel foam volume.The fuel cell flow field area, the nickel foam of cutting appropriate size from the nickel foam volume, and ironed to 1 mm.Ironed nickel foam and carbon felt, PEM, anode groups are dressed up membrane electrode (MEA), be assembled into direct sodium borohydride fuel cell with flow field plate afterwards.
Beneficial effect of the present invention: realized that the nitrogen-doped graphene original position is applied to direct sodium borohydride fuel cell negative electrode integratedly and makes battery obtain high power generation performance; Remove hydrophobic operation rambunctious from, greatly simplified the technology of preparing of cell cathode; Realize big batch of large-scale industrial production of negative electrode, raising battery production rate also reduces production costs.
Description of drawings
Fig. 1 reaction in-situ device sketch map
Fig. 2 MEA structure chart
Embodiment
Embodiment 1:
In reactor as shown in Figure 1, the nickel foam volume is placed on the left side rotating shaft, one of nickel foam of extraction is passed the intermediate reaction district and is fixed in the right side rolling-up mechanism.Reactor is evacuated to 10
-2Pa and inflated with nitrogen vacuumize again, make the interior oxygen residual volume of reactor less than 10 repeatedly for several times
-4Pa.Intermediate reaction district temperature is risen to 1050
oC begins to feed methane, ammonia and nitrogen mixture body (three's volume ratio is 10:30:60), starts right side transmission rolling-up mechanism simultaneously and makes nickel foam pass through the intermediate reaction district continuously with the speed of 1 mm/min.When the complete rolling of nickel foam stops heating and ventilation behind the right side, make reactor temperature be reduced to 100
oOpen reactor after below the C and take out the nickel foam volume.The fuel cell flow field area, the nickel foam of cutting appropriate size from the nickel foam volume, and ironed to 1 mm.Ironed nickel foam and carbon felt, PEM, Ni-Pd anode are dressed up MEA by Fig. 2 structural group, be assembled into direct sodium borohydride fuel cell with flow field plate afterwards.This battery is with 10wt.%NaOH-5wt.%NaBH
4For fuel 80
oThe peak power output density of C can reach 240 mW/cm
2
Embodiment 2:
In reactor as shown in Figure 1, the nickel foam volume is placed on the left side rotating shaft, one of nickel foam of extraction is passed the intermediate reaction district and is fixed in the right side rolling-up mechanism.Reactor is evacuated to 10
-2Pa and inflated with nitrogen vacuumize again, make the interior oxygen residual volume of reactor less than 10 repeatedly for several times
-4Pa.Intermediate reaction district temperature is risen to 1050
oC begins to feed methane, ammonia and nitrogen mixture body (three's volume ratio is 20:40:40), starts right side transmission rolling-up mechanism simultaneously and makes nickel foam pass through the intermediate reaction district continuously with the speed of 10 mm/min.When the complete rolling of nickel foam stops heating and ventilation behind the right side, make reactor temperature be reduced to 100
oOpen reactor after below the C and take out the nickel foam volume.The fuel cell flow field area, the nickel foam of cutting appropriate size from the nickel foam volume, and ironed to 1 mm.Ironed nickel foam and carbon felt, PEM, Ni-Pd anode are dressed up MEA by Fig. 2 structural group, be assembled into direct sodium borohydride fuel cell with flow field plate afterwards.This battery is with 10wt.%NaOH-5wt.%NaBH
4For fuel 80
oThe peak power output density of C can reach 280 mW/cm
2
Embodiment 3:
In reactor as shown in Figure 1, the nickel foam volume is placed on the left side rotating shaft, one of nickel foam of extraction is passed the intermediate reaction district and is fixed in the right side rolling-up mechanism.Reactor is evacuated to 10
-2Pa and inflated with nitrogen vacuumize again, make the interior oxygen residual volume of reactor less than 10 repeatedly for several times
-4Pa.Intermediate reaction district temperature is risen to 1050
oC begins to feed methane, ammonia and nitrogen mixture body (three's volume ratio is 40:20:40), starts right side transmission rolling-up mechanism simultaneously and makes nickel foam pass through the intermediate reaction district continuously with the speed of 100 mm/min.When the complete rolling of nickel foam stops heating and ventilation behind the right side, make reactor temperature be reduced to 100
oOpen reactor after below the C and take out the nickel foam volume.The fuel cell flow field area, the nickel foam of cutting appropriate size from the nickel foam volume, and ironed to 1 mm.Ironed nickel foam and carbon felt, PEM, Ni-Pd anode are dressed up MEA by Fig. 2 structural group, be assembled into direct sodium borohydride fuel cell with flow field plate afterwards.This battery is with 10wt.%NaOH-5wt.%NaBH
4For fuel 80
oThe peak power output density of C can reach 300 mW/cm
2
Do not depart from the scope of the present invention and principle, different changes of the present invention and variation are conspicuous for those of ordinary skills, are to be understood that the illustrative embodiments that the invention is not restricted in the preceding text proposition.
Claims (6)
1. the industrial production technology of a direct sodium borohydride fuel cell negative electrode comprises the steps:
1) in the container that electronic rolling unwinding device is installed of airtight vacuum-pumping and ventilation atmosphere, the nickel foam volume is placed on the left side rotating shaft, one of nickel foam of extraction is passed the intermediate reaction district and is fixed in the right side rolling-up mechanism, and reaction unit is evacuated to 10
-2Pa and inflated with nitrogen vacuumize again, make the interior oxygen residual volume of reactor less than 10 repeatedly for several times
-4Pa; Intermediate reaction district temperature is risen to 1050
oC begins to feed methane, ammonia and nitrogen mixture body, starts right side transmission rolling-up mechanism simultaneously and makes nickel foam continuously through the intermediate reaction district, when the complete rolling of nickel foam stops heating and ventilation behind the right side, makes reactor temperature be reduced to 100
oOpen reactor after below the C and take out the nickel foam volume;
2) fuel cell flow field area, the nickel foam of cutting appropriate size from the nickel foam volume, and ironed to 1 mm; Ironed nickel foam and carbon felt, PEM, anode groups are dressed up membrane electrode.
2. the industrial production technology of a kind of direct sodium borohydride fuel cell negative electrode as claimed in claim 1, it is characterized in that the volume ratio of methane, ammonia and nitrogen mixture body is: methane is 10% ~ 40%; Ammonia is 20% ~ 40%; Nitrogen is 40% ~ 60%.
3. the industrial production technology of a kind of direct sodium borohydride fuel cell negative electrode as claimed in claim 1 is characterized in that nickel foam is 1 ~ 100 mm/min through the speed in intermediate reaction district.
4. the industrial production technology of a kind of direct sodium borohydride fuel cell negative electrode as claimed in claim 1; It is characterized in that prepared nickel foam top layer fully covers Graphene; And the number of plies of Graphene is 1 ~ 50; Be doped with the nitrogen element in the graphene-structured, nitrogen element content is not less than 0.005% (atomic percent).
5. the industrial production technology of a kind of direct sodium borohydride fuel cell negative electrode as claimed in claim 1 is characterized in that the carbon felt is between nickel foam and PEM.
6. direct sodium borohydride fuel cell, it is characterized in that: it possesses each described negative electrode in the claim 1 ~ 5.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210263791.8A CN102760890B (en) | 2012-07-29 | 2012-07-29 | Industrial production technology for novel direct sodium borohydride fuel battery cathode |
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|---|---|---|---|
| CN201210263791.8A CN102760890B (en) | 2012-07-29 | 2012-07-29 | Industrial production technology for novel direct sodium borohydride fuel battery cathode |
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| CN102760890A true CN102760890A (en) | 2012-10-31 |
| CN102760890B CN102760890B (en) | 2014-09-03 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289181A (en) * | 2008-05-29 | 2008-10-22 | 中国科学院化学研究所 | Doped graphene and method for preparing same |
| CN102502593A (en) * | 2011-10-11 | 2012-06-20 | 中国石油大学(北京) | Preparation method of grapheme or doped graphene or graphene complex |
-
2012
- 2012-07-29 CN CN201210263791.8A patent/CN102760890B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289181A (en) * | 2008-05-29 | 2008-10-22 | 中国科学院化学研究所 | Doped graphene and method for preparing same |
| CN102502593A (en) * | 2011-10-11 | 2012-06-20 | 中国石油大学(北京) | Preparation method of grapheme or doped graphene or graphene complex |
Non-Patent Citations (1)
| Title |
|---|
| LIANGTI QU ET.AL: "Nitrogen-Doped Graphene as Efficient Metal-free Electrocatalyst for Oxygen Reduction in Fuel Cells", 《ASC NANO》 * |
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| CN102760890B (en) | 2014-09-03 |
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