CN106887619B - A kind of preparation method and its water transport plate of hydrophilic porous graphite water transport plate - Google Patents
A kind of preparation method and its water transport plate of hydrophilic porous graphite water transport plate Download PDFInfo
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- CN106887619B CN106887619B CN201510933463.8A CN201510933463A CN106887619B CN 106887619 B CN106887619 B CN 106887619B CN 201510933463 A CN201510933463 A CN 201510933463A CN 106887619 B CN106887619 B CN 106887619B
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- transport plate
- porous graphite
- hydrophilic
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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
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
- H01M8/04082—Arrangements for control of reactant parameters, e.g. pressure or concentration
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses the preparation methods and its water transport plate of a kind of hydrophilic porous graphite water transport plate, this method is will to be placed in electric assistant depositing precursor liquid by pretreated hard porous graphite plate, and electricity consumption assisted deposition is in its inner hole deposition one layer of uniform hydrophilic layer of product.The porous graphite plate of the hydrophilicity-imparting treatment, which is used as solid polymer electrolyte fuel cell water transport plate, has the characteristics such as good permeable, choke, conductivity and compression strength, and can effectively alleviate battery water shortage and water logging situation, improve battery performance and stability.The deposition of graphite oxide is controllable in water transport plate manufacturing process of the invention.
Description
Technical field
The present invention relates to field of fuel cell technology, belong to the preparation method of the porous bipolar plates of fuel cell, specially one
Proton exchanging film fuel battery graphite porous hydrophilic plate and preparation method thereof.
Background technique
Fuel cell is hopeful to replace fossil energy generation mode to become master in the future with its high-energy density and of low pollution
Stream.And PEMFC has that room temperature starting is fast, electroless liquid stream is lost, low noise advantages, has as mobile power source, various portable
The potentiality of formula power supply and uninterruptible power supply.In PEMFC operational process, cathode can generate water, and generating water must be discharged from battery,
Otherwise the water logging that will cause cathode side influences the transmission of gas.And hydrogen ion can take away a part from anode electromigration to cathode
Hydrone necessarily will cause the drying of anode-side, it is necessary to provide supplement water to the anode-side of battery, the amount for supplementing water will be able to maintain
Anode side catalyst and proton exchange membrane are in wetting state.So guaranteeing that humidification and the balance of draining have important in battery
Meaning.Usual PEMFC is humidified to cell gas using external auxiliary humidification system, but auxiliary system increases the weight of battery
Amount, volume and complexity.For water logging, researchers are usually drained with the methods of impulse blowing, raising stoichiometric ratio,
But this strategy will lead to serious supplementary loss, so that fuel cell system is more complicated.Usual PEMFC is moved using complicated
State draining and humidification auxiliary system are drained and are humidified respectively to realize the management of water, but auxiliary system increases the weight of battery
Amount, volume and complexity, and it is easily reduced the stability in cell operation.Therefore research how to simplify system humidification and
Drainage Design has great importance.
The Konar of U.S.'s Institute of Gas Technology unit et al. [US 5942347] is hydrophilic inorganic
Oxide fine particle mixes compression molding with graphite powder, resin, and Lai Shixian bipolar plate runner side is hydrophilic, and it is raw that hydrophilic substance absorbs cathode
Cheng Shui is humidified to unsaturated gas.Wuhan University of Technology [CN 1004546450] uses perhafnate cement as bonding
Agent and conductive filler graphite carry out molding and form porous graphite plate, make in graphite plate because perhafnate is decomposed to form hydrophilic substance
It can achieve the water balance of humidification and draining containing gel capillary hole, and by adjusting hydraulic pressure." the water transmission of UTC company application
Electrically conductive graphite powder is enhanced carbon fiber, cellulose fibre (cork by plate and its application method " patent of invention [CN 11794280]
Slurry), thermosetting resin and solvent are sprayed on sieve after mixing, vacuum dried to go sieve, rolling curling, multi-laminate
It presses, high temperature graphitization process, obtains porous graphite plate after hydrophilicity-imparting treatment in hole.Though this method prepares resulting water transport plate
So have good pressure in bubbles, water penetration, planar resistor rate and compressive yield strength, but preparation process need 2000 DEG C with
On high temperature carry out graphitization processing.
Summary of the invention
The object of the present invention is to provide a kind of electric assisted depositions to prepare the hydrophilic porous graphite water transport plate of fuel cell,
Guarantee it with characteristics such as good permeable, choke, conductivity and compression strength.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of preparation method of hydrophilic porous graphite water transport plate the following steps are included:
(1) it is placed in porous graphite plate as working electrode in electric assistant depositing precursor liquid, electricity consumption assisted deposition is more
Hole graphite plate inner hole deposition accumulates one layer of hydrophilic film；
(2) by after the plate high-temperature roasting of above-mentioned hydrophilicity-imparting treatment up to hydrophilic porous graphite water transport plate.
The preparation method of step (1) the electric assistant depositing precursor liquid are as follows: electrolyte is added in hydrophilic substance presoma
Solution, and adjusting pH with acid solution is 2-6.Above-mentioned presoma is that ethyl orthosilicate, methyl orthosilicate, butyl titanate are therein
One or two or more kinds, the concentration of presoma are 0.1-1mol/L；Electrolyte solution is NaCl solution, NaNO3Solution, KCl are molten
Liquid, KNO3One of solution or two kinds or more, the total concentration of above-mentioned solute is 0.05-0.5mol/L in electrolyte solution；Acid
Solution is one of hydrochloric acid, sulfuric acid, perchloric acid solution or a variety of, and above-mentioned three kinds sour total concentration are 0.01- in acid solution
1mol/L。
Porous graphite panel aperture described in step (1) is 0.1-20 μm.
Electric assisted deposition described in step (1) is constant voltage method, galvanostatic method, pulse voltage deposits, pulse current sinks
Long-pending one kind.
When the electric assisted deposition is constant voltage method, voltage is (- 2)-(- 6) V, time 30-600s；Described
When electric assisted deposition is galvanostatic method, electric current is 10-500mA cm-2, time 10-300s；The electric assisted deposition
When depositing for pulse voltage, voltage range is (- 6) -0V, and pulse spacing 0.1-10ms, pulse number is 10-100 times；It is described
Electric assisted deposition be pulse current sedimentation when, current range be 10-500mA cm-2, pulse spacing 0.1-10ms, arteries and veins
Jig frequency number is 50-200 times.
The hydrophilic film is SiO2、TiO2It is one such or two kinds.
Step (2) the high-temperature roasting temperature is 300-700 DEG C, time 1-3h.
The hydrophilic porous graphite water transport plate prepared according to the method described above, planar resistor rate are 1-5m Ω cm, bending strength
For 10-50MPa, permeable pressure is 0-0.03MPa, and bubble point 0.05-0.2MPa, contact angle is 5 ° -85 °, average pore size 0.1-
20 μm, porosity 5%-50%, hydrophilic pores ratio is 50%-100%.
Presoma used in the present invention is the lesser organic matter of surface tension, and it is heavy can be effectively diffused into progress electricity auxiliary in hole
Long-pending, graphite oxide can be uniformly distributed in hole in the porous hydrophilic carbon plate of preparation, and electricity consumption assisted deposition can regulate and control
The deposition of hydrophilic substance.
Detailed description of the invention
Fig. 1 is the graphite water transport plate of electric assistant depositing preparation in embodiment 4 from moisturization figure；
Fig. 2 is the graphite water transport plate drainage performance figure of electric assistant depositing preparation in embodiment 5；
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1: 30min is mixed in 50ml sodium nitrate solution (0.1mol/L) and 5g ethyl orthosilicate.To TEOS
After being completely dissolved, hydrochloric acid solution (0.1mol/L) is slowly added dropwise, until pH value is close to 2, it is auxiliary to get electricity that 1h is stirred under greenhouse
Help deposition precursor liquid.The porous carbon sheet that average pore size is 7 μm is placed in electric assistant depositing precursor liquid, porous carbon sheet is as work
Electrode, closely knit smooth graphite plate apply a constant voltage-using constant voltage method as reference electrode and to electrode on the working electrode (s
3.5V carries out electric assistant depositing, time 120s, by 400 DEG C of high-temperature calcination 1h of porous carbon sheet of hydrophilicity-imparting treatment to get porous
Hydrophilic graphite water transport plate.
Embodiment 2: 30min is mixed in 50ml potassium nitrate solution (0.2mol/L) and 5g ethyl orthosilicate.To TEOS
After being completely dissolved, sulfuric acid solution (0.1mol/L) is slowly added dropwise, until pH value is close to 3, it is auxiliary to get electricity that 1h is stirred under greenhouse
Help deposition precursor liquid.The porous graphite plate that average pore size is 7 μm is placed in electric assistant depositing precursor liquid (electric assistant depositing forerunner
Liquid did not had porous graphite plate), porous graphite plate as working electrode, closely knit smooth graphite plate as reference electrode and to electrode,
Apply a constant current 200mA cm on the working electrode (s using galvanostatic method-2Electric assistant depositing is carried out, time 200s will be hydrophilic
Change 400 DEG C of high-temperature calcination 2h of porous graphite plate of processing to get porous hydrophilic graphite water transport plate.
Embodiment 3: 30min is mixed in 100ml sodium nitrate solution (0.2mol/L) and 5g butyl titanate.It is complete to TEOS
After fully dissolved, hydrochloric acid solution (0.1mol/L) is slowly added dropwise, until pH value is close to 4, is stirred for 1h under greenhouse to get electricity auxiliary
Deposition precursor liquid.The porous graphite plate that average pore size is 5 μm is placed in electric assistant depositing precursor liquid (electric assistant depositing precursor liquid
Do not cross porous graphite plate), porous graphite plate is adopted as working electrode, closely knit smooth graphite plate as reference electrode and to electrode
Apply a pulse voltage on the working electrode (s with impulse-voltage method, pulsating sphere is that (- 3) -0V carries out electric assistant depositing, when pulse
Between between be divided into 1ms, pulse number is 200 times, by 450 DEG C of high-temperature calcination 2h of porous graphite plate of hydrophilicity-imparting treatment to get porous
Hydrophilic graphite water transport plate.
Embodiment 4: 50ml potassium nitrate solution (0.2mol/L) is added to 3g ethyl orthosilicate and 2g butyl titanate mixes
30min is stirred in liquid.After ethyl orthosilicate and butyl titanate are completely dissolved, perchloric acid solution is slowly added dropwise, until pH value connects
3,1h is stirred under greenhouse to get electric assistant depositing precursor liquid.The porous graphite plate that average pore size is 3 μm is placed in electric auxiliary
In deposition precursor liquid (electric assistant depositing precursor liquid did not had porous graphite plate), porous carbon sheet is as working electrode, closely knit smooth stone
It is heavy to apply pulse current progress electricity auxiliary using pulse current method as reference electrode and to electrode on the working electrode (s for black plate
Product, pulse current range are 0-200mA cm-2, pulse spacing 1ms, pulse number is 200 times, by the porous of hydrophilicity-imparting treatment
450 DEG C of high-temperature calcination 2h of graphite plate are to get hydrophilic porous graphite water transport plate.As anode current collector plate, soft graphite is made
For cathode collector plate, and the performance evaluation under the conditions of monocell carries out low-humidification is dressed up with membrane electrode assembly.It is not humidified in anode-side
In the case of, as seen from Figure 1, using hydrophilic porous graphite water transport plate in 800mA cm-23000min is run under current density
Substantially do not decay, and with fluid-tight bipolar plates, it cannot be in 800mA cm-2Lower operation.
Embodiment 5: 30min is mixed in 50ml sodium nitrate solution (0.1mol/L) and 5g TEOS.It is completely molten to TEOS
Hydrochloric acid solution is slowly added dropwise in Xie Hou, until pH value is close to 3, is stirred for 1h under greenhouse to get electric assistant depositing precursor liquid.It will
Average pore size is that 1 μm of porous graphite plate is placed in precursor liquid (electric assistant depositing precursor liquid did not had porous graphite plate), porous stone
Black plate applies a constant voltage-as reference electrode and to electrode as working electrode, closely knit smooth graphite plate on the working electrode (s
3.5V carries out electric assistant depositing, time 120s, by 500 DEG C of high-temperature calcination 2h of porous graphite plate of hydrophilicity-imparting treatment to get parent
Water porous graphite water transport plate.As cathode collector plate, soft graphite is dressed up as anode current collector plate, and with membrane electrode assembly
Monocell carries out performance evaluation in the case of being humidified entirely.As seen from Figure 2, for fluid-tight bipolar plates, using parent
Battery performance decline is slower after water porous graphite water transport plate, and battery water logging problem in the case of high electric density is effectively relieved, improves
Battery performance.
Table 1 is the physical property of the porous hydrophilic graphite plate of each embodiment.
Quantitative measurement is carried out to the hydrophilic porous graphite water transport plate of embodiment 1-5 preparation, the results are shown in Table 1.Table 1
Test condition are as follows: when permeable pressure test, the side of plate is added water to, when water side is pressurizeed, and water droplet occurs in the other side of plate
Pressure is permeable pressure；When pressure in bubbles is tested, the side of plate is added water to, is pressurizeed in the other side with nitrogen, water surface has
Pressure when bubble occurs is pressure in bubbles；When permeable amount is tested, the side of plate is added water to, and be pressurized to water cavity
0.02MPa, water, that is, water penetration amount of pressure side reduction.
Claims (5)
1. a kind of preparation method of hydrophilic porous graphite water transport plate, it is characterised in that: the following steps are included:
(1) it is placed in porous graphite plate as working electrode in electric assistant depositing precursor liquid, electricity consumption assisted deposition is in porous stone
One layer of hydrophilic film is deposited in black plate hole；
(2) by the plate high-temperature roasting of above-mentioned hydrophilicity-imparting treatment up to hydrophilic porous graphite water transport plate；
The preparation method of step (1) the electric assistant depositing precursor liquid are as follows: electrolyte solution is added in hydrophilic substance presoma,
And adjusting pH value with acid solution is 2-6；
The acid solution is one of hydrochloric acid, sulfuric acid, perchloric acid solution or a variety of, and concentration is 0.01-1 mol/L；
Presoma is one of ethyl orthosilicate, methyl orthosilicate, butyl titanate or two kinds or more in the precursor liquid, preceding
The concentration for driving body is 0.1-1mol/L；The electrolyte solution is NaCl solution, NaNO3Solution, KCl solution, KNO3Solution
One of or two kinds or more, concentration be 0.05-0.5 mol/L；
The electric assisted deposition is one kind of constant voltage method, galvanostatic method, pulse voltage deposition, pulse current deposition；
The hydrophilic film is SiO2、TiO2It is one such or two kinds.
2. preparation method according to claim 1, it is characterised in that: porous graphite panel aperture described in step (1) is
0.1-20 μm。
3. preparation method according to claim 1, it is characterised in that: when the electric assisted deposition is constant voltage method,
Voltage is -2~-6 V, and the time is 30-600 s；When the electric assisted deposition is galvanostatic method, electric current 10-500
mA·cm-2, the time is 10-300 s；When the electric assisted deposition is that pulse voltage deposits, voltage range is -6~0 V,
Pulse spacing is 0.1-10 ms, and pulse number is 10-100 times；When the electric assisted deposition is pulse current sedimentation,
Current range is 10-500 mAcm-2, the pulse spacing is 0.1-10 ms, and pulse number is 50-200 times.
4. preparation method according to claim 1, it is characterised in that: step (2) the high-temperature roasting temperature is 300-
700 DEG C, the time is 1-3 h.
5. a kind of hydrophilic porous graphite water transport plate of any the method preparation of claim 1-4, it is characterised in that: plane
Resistivity is 1-5 m Ω cm, and bending strength is 10-50 MPa, and permeable pressure is 0-0.03 Mpa, pressure in bubbles 0.05-
0.2 Mpa, contact angle 5o-85o, average pore size is 0.1-20 μm, porosity 5%-50%, and hydrophilic pores account for the ratio of all holes
Example is 50%-100%；
The test method of permeable pressure is to introduce the water into the side of water transport plate, and the exposure of the other side of plate is in air, so
It pressurizes afterwards to water side, the pressure when water droplet occurs in the air side of plate is permeable pressure；The test method of pressure in bubbles
To be pressurizeed in the side of the above-mentioned water transport plate by permeable pressure test with nitrogen, when the other side of plate has bubble to occur
Pressure is pressure in bubbles.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102034990A (en) * | 2009-09-25 | 2011-04-27 | 北京有色金属研究总院 | Metallic bipolar plate of proton exchange membrane fuel cell and surface modification method thereof |
| CN102191499A (en) * | 2010-03-19 | 2011-09-21 | 通用汽车环球科技运作有限责任公司 | Method of coating a substrate with nanoparticles including a metal oxide |
| CN101901914B (en) * | 2009-04-23 | 2014-12-17 | 通用汽车环球科技运作公司 | Method of coating a surface of a fuel cell plate |
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2015
- 2015-12-15 CN CN201510933463.8A patent/CN106887619B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101901914B (en) * | 2009-04-23 | 2014-12-17 | 通用汽车环球科技运作公司 | Method of coating a surface of a fuel cell plate |
| CN102034990A (en) * | 2009-09-25 | 2011-04-27 | 北京有色金属研究总院 | Metallic bipolar plate of proton exchange membrane fuel cell and surface modification method thereof |
| CN102191499A (en) * | 2010-03-19 | 2011-09-21 | 通用汽车环球科技运作有限责任公司 | Method of coating a substrate with nanoparticles including a metal oxide |
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