CN109950556A - A kind of preparation method of the carbon fiber bipolar plates with three-dimensional porous structure - Google Patents
A kind of preparation method of the carbon fiber bipolar plates with three-dimensional porous structure Download PDFInfo
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- CN109950556A CN109950556A CN201910253019.XA CN201910253019A CN109950556A CN 109950556 A CN109950556 A CN 109950556A CN 201910253019 A CN201910253019 A CN 201910253019A CN 109950556 A CN109950556 A CN 109950556A
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- carbon fiber
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Abstract
A kind of preparation method of the carbon fiber bipolar plates with three-dimensional porous structure, using polypropylene cyano carbon fiber and graphite felt as conductive filler and reinforcement material, epoxy resin-base, paraffin is hole sealing agent, prepares polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and polypropylene cyano carbon fiber and graphite felt/paraffin prepreg using hot submersion method；Bipolar plates containing paraffin are prepared using hot press forming technology；The paraffin in bipolar plates is removed by later period dewaxing technique, finally obtains the two-sided bipolar plates containing carbon fiber porous structure.Preparation process of the present invention is simple, preparation cost is low, environmental pollution is small；Used epoxy resin-base and strong, the prepared carbon fiber bipolar plates high mechanical strength of the carbon fiber guiding electric material cohesive force in polypropylene cyano carbon fiber and graphite felt, have excellent electrochemical corrosion resistant and electric conductivity；Preparation process is easily controllable, is suitable for industrialized production.
Description
Technical field
The invention belongs to engineering material preparation technical fields, and in particular to a kind of carbon fiber with three-dimensional porous structure is double
The preparation method of pole plate.
Background technique
It is led in flow battery energy storage technical field, such as all-vanadium flow battery, lead flow battery redox flow batteries
Domain, bipolar plates are one of critical components of flow battery, it provides the anti-place of electrode.Since long-time is in charging and discharging state
Under, especially in a charging situation, electrochemical corrosion will lead to performance for bipolar plates serious corrosion to bipolar plates side of the positive electrode
Deteriorate, if electric conductivity, mechanical strength decline, shortens its service life.For this purpose, bipolar plates electrode material will have high antioxygen
The property changed, corrosion resistance, to ensure that the electrode material service life；Secondly, bipolar plates electrode material has excellent conduction
Property, the ohmic voltage drop in charge and discharge process is reduced, the voltage efficiency of battery is improved, while electric current can be reduced and passed in electrode plate
Energy loss when defeated improves the energy efficiency of battery；Finally, bipolar plates electrode material there will be good mechanical strength, meet
Intensity requirement of the battery in assembling process.
Currently, reported redox flow batteries such as all-vanadium flow battery, lead flow battery mainly use conductive filler/
Polymer matrix composite, wherein conductive filler is mainly based on carbon material, including carbon black, graphite powder and carbon fiber etc., polymerization
Object includes thermoplastic resin such as polypropylene, polyethylene, polytetrafluoroethylene (PTFE) etc. and thermosetting resin such as epoxy resin, phenolic resin
Deng.This kind of conducing composite material have the characteristics that light-weight, easy processing at, it is at low cost be widely adopted, conductivity be greater than 10S/
cm；Bending strength is greater than 40MPa；Electrochemical corrosion rate is less than 15 μ A/cm2.But it uses for a long time, due to side of the positive electrode electrification
It is easy to oxidize to learn oxidation carbon material such as carbon black, graphite powder, especially for the system of high oxidation electrode potential, electrochemical corrosion phenomenon
Seriously, the service life of battery is seriously constrained in this way.
Summary of the invention
The carbon fiber bipolar plates with three-dimensional porous structure that the object of the present invention is to provide a kind of have improvement existing compound
The electric conductivity and mechanical performance of material electrodes plate and the characteristics of effectively improving its electrochemical corrosion resistant.
The technical scheme adopted by the invention is that a kind of preparation side of the carbon fiber bipolar plates with three-dimensional porous structure
Method is specifically implemented according to the following steps:
Step 1 prepares epoxy resin adhesive liquid and vasoliniment；
Step 2 is presoaked with polypropylene cyano carbon fiber and graphite felt for polypropylene cyano carbon fiber and graphite felt/epoxy resin
Material；
Step 3, with two pieces of identical polypropylene cyano carbon fiber and graphite felts for two blocks of identical polypropylene cyano carbon fiber stones
Black felt/paraffin prepreg；
Step 4, with polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and two pieces of identical polypropylene cyano carbon fibers
Dimension graphite felt/paraffin prepreg suppresses the two-sided electrode plate containing paraffin；
The two-sided electrode plate containing paraffin obtained by step 5, step 4 removes Lasaxing Oilfield, and the two-sided carbon fiber in porous structure is made
Tie up bipolar plates.
The features of the present invention also characterized in that:
Step 1 is specifically implemented according to the following steps:
Step 1.1 mixes epoxy resin, crosslinking agent and catalyst, magnetic agitation 10-30 at a temperature of 50 DEG C -70 DEG C
Minute, obtain oxygen resin adhesive liquid；
Step 1.2, with 110-130 DEG C of silicone oil liquefied petrolatum, obtain vasoliniment.
Step 2 is specifically implemented according to the following steps:
Polypropylene cyano carbon fiber and graphite felt is completely infused in the resulting epoxy resin adhesive liquid of step 1 by step 2.1, leaching
Stain 1-5 minutes；
After the completion of step 2.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper is adhered on surface again, obtains polypropylene cyanogen
Base carbon fibre graphite/epoxy prepreg.
Step 3 is specifically implemented according to the following steps:
Two pieces of identical polypropylene cyano carbon fiber and graphite felts are entirely put into vasoliniment by step 3.1, impregnate 1-
5 minutes；
After the completion of step 3.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper, the solidification of room temperature paraffin are adhered in surface again
Sealing of hole obtains two pieces of identical polypropylene cyano carbon fiber and graphite felt/paraffin prepregs.
Step 4 is specifically implemented according to the following steps:
Remove step 2, in 3 after the silicone oil paper on three prepreg surfaces of gained, three pieces of prepregs are sequentially placed into hot pressing
In mold, it is placed on intermediate polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and upper and lower layer polypropylene cyano carbon fiber
Dimension graphite felt/paraffin prepreg is not stacked with one side contacts of paraffin sealing of hole；
Step 4.2 closes grinding tool, is then warming up to 80 DEG C with the rate of 1-3 DEG C/min, keeps the temperature 120-180 minutes gels
Afterwards in 100-150kgf/cm2It is hot-forming；
After step 4.3, molding, then 130 DEG C are warming up to the rate of 1-3 DEG C/min and keeps the temperature 60-90 minutes, finally cool down
Pressure release is taken out after to room temperature, and the two-sided electrode plate containing paraffin is made.
Step 5 is specifically implemented according to the following steps:
The resulting two-sided electrode plate containing paraffin of step 4 is put into 120-150 DEG C of silicone oil and removes stone by step 5.1
Wax, being then placed in mass percent is that mass percent is in 40%NaOH aqueous solution, is impregnated at 80-90 DEG C 2-3 small
When；
It is immersion 2-3 small in 15% oxalic acid solution for taking out after step 5.2, immersion and moving into the mass percent of boiling
When；
Step 5.3, immersion terminate, and are finally successively cleaned by ultrasonic 8-10 minutes in acetone and deionized water, are made two-sided
In the carbon fiber bipolar plates of porous structure.
Epoxy resin adhesive liquid configures in step 1, it is desirable that the weight percent of each component is epoxy resin: crosslinking agent: catalysis
Agent=100:80-90:0.1-0.3.
Epoxy resin is bisphenol A-type, molecular weight 300-700 in step 1；Crosslinking agent is hexanedioic acid；Catalyst is benzyl
Dimethylamine；Paraffin is No. 90 microwaxes.
The beneficial effects of the present invention are:
1, method of the invention uses the polypropylene cyano carbon fiber and graphite felt with high conductivity for conductive material and increasing
Strong body material, epoxy resin are matrix, and paraffin is porous structure protective agent, and material source is abundant, low in cost.
2, polypropylene cyano carbon fiber and graphite felt prepreg is prepared by epoxy resin adhesive liquid and paraffin infiltration, used
Heat pressing process is pre- by polypropylene cyano carbon fiber and graphite felt/paraffin prepreg-polypropylene cyano carbon fiber and graphite felt/resin adhesive liquid
Leaching material-polypropylene cyano carbon fiber and graphite felt/paraffin prepreg prepares the two-sided electrode plate containing paraffin, and intermediate compacted zone is (poly-
Propylene cyano carbon fiber and graphite felt/epoxy resin composite material conductive layer) there is very high electric conductivity, mechanical performance and resistance to electrification
Learn corrosivity.
3, the bipolar plates with three-dimensional porous structure can be prepared by simple dewaxing technique, this material can be made
It can improve electrochemical corrosion resistant especially for lead flow battery for the double battery plates of redox flow batteries, improve battery
Efficiency extends the service life of battery.
Detailed description of the invention
Fig. 1 is a kind of process flow chart of the preparation method of the carbon fiber bipolar plates with three-dimensional porous structure of the present invention.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of the carbon fiber bipolar plates with three-dimensional porous structure of the present invention, it is specifically real according to the following steps
It applies:
Step 1 prepares epoxy resin adhesive liquid and vasoliniment；
Step 2 is presoaked with polypropylene cyano carbon fiber and graphite felt for polypropylene cyano carbon fiber and graphite felt/epoxy resin
Material；
Step 3, with two pieces of identical polypropylene cyano carbon fiber and graphite felts for two blocks of identical polypropylene cyano carbon fiber stones
Black felt/paraffin prepreg；
Step 4, with polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and two pieces of identical polypropylene cyano carbon fibers
Dimension graphite felt/paraffin prepreg suppresses the two-sided electrode plate containing paraffin；
The two-sided electrode plate containing paraffin obtained by step 5, step 4 removes Lasaxing Oilfield, and the two-sided carbon fiber in porous structure is made
Tie up bipolar plates.
Step 1 is specifically implemented according to the following steps:
Epoxy resin, crosslinking agent and catalyst are successively weighed and are added in beaker by step 1.1, in 50 DEG C of -70 DEG C of temperature
Lower magnetic agitation 10-30 minutes, mixes them thoroughly, and obtains flaxen epoxy resin adhesive liquid；
Step 1.2 pours into paraffin weighing in glass guide channel, is added to 110-130 DEG C using oil bath pan, makes its thorough liquid
Change, obtains the vasoliniment of the low viscosity with a thickness of 4mm high；
Epoxy resin adhesive liquid A is configured in step 1, it is desirable that the weight percent of each component is epoxy resin: crosslinking agent: catalysis
Agent=100:80-90:0.1-0.3.
Wherein, it is a kind of thermosetting resin that epoxy resin, which is bisphenol A type epoxy resin, has good adhesive strength and resistance to
Chemical property, molecular weight are advisable for 300-700, and commercial grades have E-42, E-44, E-51, and softening point is less than 30 DEG C；
Crosslinking agent is hexanedioic acid, and hexanedioic acid is a kind of Dicarboxylic Acids, and organo-functional group carboxylic acid can be with epoxy resin
In epoxy group occur that esterification is anti-, generate the macromolecular with reticular structure；
Catalyst is benzyl dimethylamine, and benzyl dimethylamine is a kind of trimethylamine, being capable of the offer of cross-linking catalyst ethanedioic acid
Anion activated centre promotes epoxy resin and crosslinking agent anionic polymerisation is counter occurs；
Sealing of hole protective of the paraffin as porous carbon fiber polypropylene cyano carbon fiber and graphite felt is No. 90 microwaxes,
Feature is odorless, tasteless white-amorphous amorphous solid wax, close containing a small amount of ring-type, straight-chain hydrocarbons based on branched-chain saturated hydrocarbon
Degree is 0.9g/mL or so, and fusing point is greater than 90 DEG C, can be retained by techniques such as high temperature infiltration-low-temperature setting-high temperature dewaxings poly-
The porous structure of propylene cyano carbon fiber and graphite felt；
After the mixed glue solution hot setting of above-mentioned epoxy resin, crosslinking agent and catalyst, elasticity modulus is greater than 3GPa, energy
Carbon fiber tight bond in enough and polypropylene cyano carbon fiber and graphite felt, is prepared into certain mechanical performance, conducting function
With the plate of electrochemical corrosion resistant.
Step 2 is specifically implemented according to the following steps:
Polypropylene cyano carbon fiber and graphite felt is completely infused in that step 1 is resulting to fill epoxy resin adhesive liquid by step 2.1
Glass in, impregnate 1-5 minutes；
After the completion of step 2.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper is adhered on surface again, obtains polypropylene cyanogen
Base carbon fibre graphite felt/epoxy prepreg.
Polypropylene cyano carbon fiber and graphite felt in step 2, volume density 0.1-0.15g/cm3, carbon content be greater than 99%, gather
Polypropylene cyano electric conduction of carbon fiber rate in propylene cyano carbon fiber and graphite felt is greater than 1 × 102S/cm.Polypropylene cyano carbon fiber
Graphite felt is capable of providing three-dimensional porous structure as conductive filler, provides a large amount of active site for electrode is counter, improves battery effect
Rate；It can simultaneously serve as reinforcement, improve plate bending strength；In addition polypropylene cyano carbon fiber has very high resistance to electrochemistry
Corrosivity and good chemical stability, can improve the service life of bipolar plates.
Resin using polypropylene cyano carbon fiber and graphite felt as conductive material, the length of polypropylene cyano carbon fiber and graphite felt ×
Width × thickness size is 10cm × 10cm × 0.5cm.
Step 3 is specifically implemented according to the following steps:
Two pieces of identical polypropylene cyano carbon fiber and graphite felts are entirely put into step 2 and fill vasoliniment by step 3.1
Glass guide channel in, impregnate 1-5 minutes；
After the completion of step 3.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper, the solidification of room temperature paraffin are adhered in surface again
Sealing of hole obtains two pieces of identical polypropylene cyano carbon fiber and graphite felt/paraffin prepregs.
Paraffin sealing of hole thickness is in 4-5mm in step 3.2.
Polypropylene cyano carbon fiber and graphite felt is conductive material in step 3, and the size of length x width x thickness is
10cm×10cm×1cm。
Step 4 is as shown in Figure 1, be specifically implemented according to the following steps:
Step 4.1 removes step 2, in 3 after the silicone oil paper on three prepreg surfaces of gained, and three pieces of prepregs are successively put
Enter into hot pressing die, is placed on intermediate polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and upper and lower layer polypropylene
Cyano carbon fiber and graphite felt/paraffin prepreg is not stacked with one side contacts of paraffin sealing of hole；
Step 4.2 closes grinding tool, is then warming up to 80 DEG C with the rate of 1-3 DEG C/min, keeps the temperature 120-180 minutes gels
Afterwards in 100-150kgf/cm2It is hot-forming；
After step 4.3, molding, then 130 DEG C are warming up to the rate of 1-3 DEG C/min and keeps the temperature 60-90 minutes, finally with furnace
It is cooled to room temperature rear pressure release to take out, the two-sided electrode plate containing paraffin is made.
Step 5 is specifically implemented according to the following steps:
Except deparaffnize, then the two-sided electrode plate containing paraffin of step 4 is put into 120-150 DEG C of silicone oil by step 5.1
Being put into mass percent is that 2-3 hour is impregnated at 80-90 DEG C in 40%NaOH aqueous solution；
It is immersion 2-3 small in 15% oxalic acid solution for taking out after step 5.2, immersion and moving into the mass percent of boiling
When；
Step 5.3, immersion terminate, and are finally successively cleaned by ultrasonic 8-10 minutes in acetone and deionized water, are made two-sided
In the bipolar plates of porous structure.
Bipolar plates obtained are tested for the property, need exist for for the bipolar plates performance test with porous structure into
Row explanation, according to the literature, polypropylene cyano electric conduction of carbon fiber rate is greater than 1 × 102S/cm, electrochemical corrosion resistant meet liquid
The needs of galvanic battery, here mainly for compacted zone among bipolar plates, i.e. polypropylene cyano carbon fiber and graphite felt/epoxy resin derivative
Electric layer is tested for the property.After removing bipolar plates two sides porous polypropylene cyano carbon fiber and graphite felt, measured using four probe method
Intermediate compacted zone conductivity, conductivity are greater than 1 × 102S/cm；According to GB standard GB1449-2005-T, three-point bending method is used
The bending strength for measuring intermediate compacted zone is greater than 59MPa；With the H of 3M2SO4For electrolyte, using electrochemistry linear polarization method,
Intermediate compacted zone corrosion rate can be obtained less than 1 μ A/cm2。
Embodiment 1
Step 1 prepares epoxy resin solution and vasoliniment；
Step 1.1, using epoxy resin as matrix, so that weight percent is met epoxy resin: crosslinking agent: catalyst=100:
Epoxy resin, crosslinking agent and catalyst are successively weighed and are added in beaker by 80:0.1, and magnetic agitation 10 is divided at 50 °C
Clock mixes them thoroughly, and obtains flaxen epoxy resin adhesive liquid；
Step 1.2 pours into the weighing of edible paraffin in glass guide channel, is added to 110 DEG C using oil bath pan, makes its thorough liquid
Change, obtains the vasoliniment of the low viscosity with a thickness of 4mm high；
Step 2 is presoaked with polypropylene cyano carbon fiber and graphite felt for polypropylene cyano carbon fiber and graphite felt/epoxy resin
Material；
Polypropylene cyano carbon fiber and graphite felt is completely infused in that step 1 is resulting to fill epoxy resin adhesive liquid by step 2.1
Glass in, impregnate 1 minute, polypropylene cyano carbon fiber and graphite felt specification: the size of length x width x thickness be 10cm
×10cm×0.5cm；
After the completion of step 2.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper is adhered on surface again, obtains polypropylene cyanogen
Base carbon fibre graphite felt/epoxy prepreg.
Step 3, with two pieces of identical polypropylene cyano carbon fiber and graphite felts for two blocks of identical polypropylene cyano carbon fiber stones
Black felt/paraffin prepreg；
Step 3.1, by the identical polypropylene cyano carbon fiber and graphite felt with material in two pieces of same steps 2, entirely
It is put into step 2 to fill in the glass guide channel of vasoliniment, impregnate 1 minute, polypropylene cyano carbon fiber and graphite felt specification: length ×
Width × thickness size is 10cm × 10cm × 1cm；
After the completion of step 3.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper, the solidification of room temperature paraffin are adhered in surface again
Sealing of hole obtains two pieces of identical polypropylene cyano carbon fiber and graphite felt/paraffin prepregs, and paraffin sealing of hole thickness is in 4mm.
Step 4, with polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and two pieces of identical polypropylene cyano carbon fibers
Dimension graphite felt/paraffin prepreg suppresses the two-sided electrode plate containing paraffin；
Step 4.1 removes step 2, in 3 after the silicone oil paper on three prepreg surfaces of gained, and three pieces of prepregs are successively put
Enter into hot pressing die, is placed on intermediate polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and upper and lower layer polypropylene
Cyano carbon fiber and graphite felt/paraffin prepreg is not stacked with one side contacts of paraffin sealing of hole；
Step 4.2 closes grinding tool, is then warming up to 80 DEG C with the rate of 1 DEG C/min, keep the temperature after 120 minutes gels
100kgf/cm2It is hot-forming；
After step 4.3, molding, then 130 DEG C are warming up to the rate of 1 DEG C/min and keeps the temperature 60 minutes, last furnace cooling
Pressure release is taken out after to room temperature, and the two-sided electrode plate containing paraffin is made.
The two-sided electrode plate containing paraffin obtained by step 5, step 4 removes Lasaxing Oilfield, and the two-sided carbon fiber in porous structure is made
Tie up bipolar plates；
The resulting two-sided electrode plate containing paraffin of step 4 is put into 120 DEG C of silicone oil except deparaffnize, so by step 5.1
After be put into mass percent be 40%NaOH aqueous solution in, at 80 DEG C impregnate 2 hours；
Taking out after step 5.2, immersion and moving into the mass percent of boiling is that immersion is 2 small in 15% oxalic acid solution
When；
Step 5.3, immersion terminate, and are finally successively cleaned by ultrasonic 8 minutes in acetone and deionized water, are made two-sided in more
The bipolar plates of pore structure.
Polypropylene cyano carbon fiber and graphite felt/epoxy resin compacted zone among bipolar plates obtained is tested for the property,
Conductive plate conductivity is 2.3 × 102S/cm；Bending strength is 64MPa；Corrosion rate is 0.2 μ A/cm2。
Embodiment 2
Step 1 prepares epoxy resin solution and vasoliniment；
Step 1.1, using epoxy resin as matrix, so that weight percent is met epoxy resin: crosslinking agent: catalyst=100:
Epoxy resin, crosslinking agent and catalyst are successively weighed and are added in beaker by 80:0.2, and magnetic agitation 14 is divided at a temperature of 54 DEG C
Clock mixes them thoroughly, and obtains flaxen epoxy resin adhesive liquid；
Step 1.2 pours into the weighing of edible paraffin in glass guide channel, is added to 120 DEG C using oil bath pan, makes its thorough liquid
Change, obtains the vasoliniment of the low viscosity with a thickness of 4mm high.
Step 2 is presoaked with polypropylene cyano carbon fiber and graphite felt for polypropylene cyano carbon fiber and graphite felt/epoxy resin
Material；
Polypropylene cyano carbon fiber and graphite felt is completely infused in that step 1 is resulting to fill epoxy resin adhesive liquid by step 2.1
Glass in, impregnate 3 minutes, polypropylene cyano carbon fiber and graphite felt specification: the size of length x width x thickness be 10cm
×10cm×0.5cm；
After the completion of step 2.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper is adhered on surface again, obtains polypropylene cyanogen
Base carbon fibre graphite felt/epoxy prepreg.
Step 3, with two pieces of identical polypropylene cyano carbon fiber and graphite felts for two blocks of identical polypropylene cyano carbon fiber stones
Black felt/paraffin prepreg；
Step 3.1, by the identical polypropylene cyano carbon fiber and graphite felt with material in two pieces of same steps 2, entirely
It is put into step 2 to fill in the glass guide channel of vasoliniment, impregnate 4 minutes, polypropylene cyano carbon fiber and graphite felt specification: length ×
Width × thickness size is 10cm × 10cm × 1cm；
After the completion of step 3.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper, the solidification of room temperature paraffin are adhered in surface again
Sealing of hole obtains two pieces of identical polypropylene cyano carbon fiber and graphite felt/paraffin prepregs, and paraffin sealing of hole thickness is in 5mm.
Step 4, with polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and two pieces of identical polypropylene cyano carbon fibers
Dimension graphite felt/paraffin prepreg suppresses the two-sided electrode plate containing paraffin；
Step 4.1 removes step 2, in 3 after the silicone oil paper on three prepreg surfaces of gained, and three pieces of prepregs are successively put
Enter into hot pressing die, is placed on intermediate polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and upper and lower layer polypropylene
Cyano carbon fiber and graphite felt/paraffin prepreg is not stacked with one side contacts of paraffin sealing of hole；
Step 4.2 closes grinding tool, is then warming up to 80 DEG C with the rate of 3 DEG C/min, keep the temperature after 170 minutes gels
120kgf/cm2It is hot-forming；
After step 4.3, molding, then 130 DEG C are warming up to the rate of 2 DEG C/min and keeps the temperature 70 minutes, last furnace cooling
Pressure release is taken out after to room temperature, and the two-sided electrode plate containing paraffin is made.
The two-sided electrode plate containing paraffin obtained by step 5, step 4 removes Lasaxing Oilfield, and the two-sided carbon fiber in porous structure is made
Tie up bipolar plates；
The resulting two-sided electrode plate containing paraffin of step 4 is put into 150 DEG C of silicone oil except deparaffnize, so by step 5.1
After be put into mass percent be 40%NaOH aqueous solution in, at 80 DEG C impregnate 2 hours；
Taking out after step 5.2, immersion and moving into the mass percent of boiling is that immersion is 2 small in 15% oxalic acid solution
When；
Step 5.3, immersion terminate, and are finally successively cleaned by ultrasonic 9 minutes in acetone and deionized water, are made two-sided in more
The bipolar plates of pore structure.
Polypropylene cyano carbon fiber and graphite felt/epoxy resin compacted zone among bipolar plates obtained is tested for the property,
Conductive plate conductivity is 1.9 × 102S/cm；Bending strength is 63MPa；Corrosion rate is 0.44 μ A/cm2。
Embodiment 3
Step 1 prepares epoxy resin solution and vasoliniment；
Step 1.1, using epoxy resin as matrix, so that weight percent is met epoxy resin: crosslinking agent: catalyst=100:
Epoxy resin, crosslinking agent and catalyst are successively weighed and are added in beaker by 85:0.2, and magnetic agitation 20 is divided at a temperature of 60 DEG C
Clock mixes them thoroughly, and obtains flaxen epoxy resin adhesive liquid；
Step 1.2 pours into the weighing of edible paraffin in glass guide channel, is added to 118 DEG C using oil bath pan, makes its thorough liquid
Change, obtains the vasoliniment of the low viscosity with a thickness of 4mm high.
Step 2 is presoaked with polypropylene cyano carbon fiber and graphite felt for polypropylene cyano carbon fiber and graphite felt/epoxy resin
Material；
Polypropylene cyano carbon fiber and graphite felt is completely infused in that step 1 is resulting to fill epoxy resin adhesive liquid by step 2.1
Glass in, impregnate 4 minutes, polypropylene cyano carbon fiber and graphite felt specification: the size of length x width x thickness be 10cm
×10cm×0.5cm；
After the completion of step 2.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper is adhered on surface again, obtains polypropylene cyanogen
Base carbon fibre graphite felt/epoxy prepreg.
Step 3, with two pieces of identical polypropylene cyano carbon fiber and graphite felts for two blocks of identical polypropylene cyano carbon fiber stones
Black felt/paraffin prepreg；
Step 3.1, by the identical polypropylene cyano carbon fiber and graphite felt with material in two pieces of same steps 2, entirely
It is put into step 2 to fill in the glass guide channel of vasoliniment, impregnate 3 minutes, polypropylene cyano carbon fiber and graphite felt specification: length ×
Width × thickness size is 10cm × 10cm × 1cm；
After the completion of step 3.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper, the solidification of room temperature paraffin are adhered in surface again
Sealing of hole obtains two pieces of identical polypropylene cyano carbon fiber and graphite felt/paraffin prepregs, and paraffin sealing of hole thickness is in 4.5mm.
Step 4, with polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and two pieces of identical polypropylene cyano carbon fibers
Dimension graphite felt/paraffin prepreg suppresses the two-sided electrode plate containing paraffin；
Step 4.1 removes step 2, in 3 after the silicone oil paper on three prepreg surfaces of gained, and three pieces of prepregs are successively put
Enter into hot pressing die, is placed on intermediate polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and upper and lower layer polypropylene
Cyano carbon fiber and graphite felt/paraffin prepreg is not stacked with one side contacts of paraffin sealing of hole；
Step 4.2 closes grinding tool, is then warming up to 80 DEG C with the rate of 2 DEG C/min, keep the temperature after 160 minutes gels
140kgf/cm2It is hot-forming；
After step 4.3, molding, then 130 DEG C are warming up to the rate of 2.5 DEG C/min and keeps the temperature 80 minutes, it is finally cold with furnace
But it is taken out to pressure release after room temperature, the two-sided electrode plate containing paraffin is made.
The two-sided electrode plate containing paraffin obtained by step 5, step 4 removes Lasaxing Oilfield, and the two-sided carbon fiber in porous structure is made
Tie up bipolar plates；
The resulting two-sided electrode plate containing paraffin of step 4 is put into 140 DEG C of silicone oil except deparaffnize, so by step 5.1
After be put into mass percent be 40%NaOH aqueous solution in, at 80 DEG C impregnate 2.5 hours；
Taking out after step 5.2, immersion and moving into the mass percent of boiling is that immersion is 2.5 small in 15% oxalic acid solution
When；
Step 5.3, immersion terminate, and are finally successively cleaned by ultrasonic 8.5 minutes in acetone and deionized water, being made two-sided is in
The bipolar plates of porous structure.
Polypropylene cyano carbon fiber and graphite felt/epoxy resin compacted zone among bipolar plates obtained is tested for the property,
Conductive plate conductivity is 2.1 × 102S/cm；Bending strength is 66MPa；Corrosion rate is 0.17 μ A/cm2。
Embodiment 4
Step 1 prepares epoxy resin solution and vasoliniment；
Step 1.1, using epoxy resin as matrix, so that weight percent is met epoxy resin: crosslinking agent: catalyst=100:
Epoxy resin, crosslinking agent and catalyst are successively weighed and are added in beaker by 80:0.3, and magnetic agitation 17 is divided at a temperature of 66 DEG C
Clock mixes them thoroughly, and obtains flaxen epoxy resin adhesive liquid；
Step 1.2 pours into the weighing of edible paraffin in glass guide channel, is added to 127 DEG C using oil bath pan, makes its thorough liquid
Change, obtains the vasoliniment of the low viscosity with a thickness of 4mm high；
Step 2 is presoaked with polypropylene cyano carbon fiber and graphite felt for polypropylene cyano carbon fiber and graphite felt/epoxy resin
Material；
Polypropylene cyano carbon fiber and graphite felt is completely infused in that step 1 is resulting to fill epoxy resin adhesive liquid by step 2.1
Glass in, impregnate 2 minutes, polypropylene cyano carbon fiber and graphite felt specification: the size of length x width x thickness be 10cm
×10cm×0.5cm；
After the completion of step 2.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper is adhered on surface again, obtains polypropylene cyanogen
Base carbon fibre graphite felt/epoxy prepreg.
Step 3, with two pieces of identical polypropylene cyano carbon fiber and graphite felts for two blocks of identical polypropylene cyano carbon fiber stones
Black felt/paraffin prepreg；
Step 3.1, by the identical polypropylene cyano carbon fiber and graphite felt with material in two pieces of same steps 2, entirely
It is put into step 2 to fill in the glass guide channel of vasoliniment, impregnate 2 minutes, polypropylene cyano carbon fiber and graphite felt specification: length ×
Width × thickness size is 10cm × 10cm × 1cm；
After the completion of step 3.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper, the solidification of room temperature paraffin are adhered in surface again
Sealing of hole obtains two pieces of identical polypropylene cyano carbon fiber and graphite felt/paraffin prepregs, and paraffin sealing of hole thickness is in 4.5mm.
Step 4, with polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and two pieces of identical polypropylene cyano carbon fibers
Dimension graphite felt/paraffin prepreg suppresses the two-sided electrode plate containing paraffin；
Step 4.1 removes step 2, in 3 after the silicone oil paper on three prepreg surfaces of gained, and three pieces of prepregs are successively put
Enter into hot pressing die, is placed on intermediate polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and upper and lower layer polypropylene
Cyano carbon fiber and graphite felt/paraffin prepreg is not stacked with one side contacts of paraffin sealing of hole；
Step 4.2 closes grinding tool, is then warming up to 80 DEG C with the rate of 2.5 DEG C/min, keep the temperature after 150 minutes gels
130kgf/cm2It is hot-forming；
After step 4.3, molding, then 130 DEG C are warming up to the rate of 3 DEG C/min and keeps the temperature 75 minutes, last furnace cooling
Pressure release is taken out after to room temperature, and the two-sided electrode plate containing paraffin is made.
The two-sided electrode plate containing paraffin obtained by step 5, step 4 removes Lasaxing Oilfield, and the two-sided carbon fiber in porous structure is made
Tie up bipolar plates；
The resulting two-sided electrode plate containing paraffin of step 4 is put into 150 DEG C of silicone oil except deparaffnize, so by step 5.1
After be put into mass percent be 40%NaOH aqueous solution in, at 80 DEG C impregnate 2.5 hours；
Taking out after step 5.2, immersion and moving into the mass percent of boiling is that immersion is 2.5 small in 15% oxalic acid solution
When；
Step 5.3, immersion terminate, and are finally successively cleaned by ultrasonic 8.5 minutes in acetone and deionized water, being made two-sided is in
The bipolar plates of porous structure.
Polypropylene cyano carbon fiber and graphite felt/epoxy resin compacted zone among bipolar plates obtained is tested for the property,
Conductive plate conductivity is 1.6 × 102S/cm；Bending strength is 64MPa；Corrosion rate is 0.11 μ A/cm2。
Embodiment 5
Step 1 prepares epoxy resin solution and vasoliniment；
Step 1.1, using epoxy resin as matrix, so that weight percent is met epoxy resin: crosslinking agent: catalyst=100:
Epoxy resin, crosslinking agent and catalyst are successively weighed and are added in beaker by 90:0.3, and magnetic agitation 30 is divided at a temperature of 70 DEG C
Clock mixes them thoroughly, and obtains flaxen epoxy resin adhesive liquid；
Step 1.2 pours into the weighing of edible paraffin in glass guide channel, is added to 130 DEG C using oil bath pan, makes its thorough liquid
Change, obtains the vasoliniment of the low viscosity with a thickness of 4mm high；
Step 2 is presoaked with polypropylene cyano carbon fiber and graphite felt for polypropylene cyano carbon fiber and graphite felt/epoxy resin
Material；
Polypropylene cyano carbon fiber and graphite felt is completely infused in that step 1 is resulting to fill epoxy resin adhesive liquid by step 2.1
Glass in, impregnate 5 minutes, polypropylene cyano carbon fiber and graphite felt specification: the size of length x width x thickness be 10cm
×10cm×0.5cm；
After the completion of step 2.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper is adhered on surface again, obtains polypropylene cyanogen
Base carbon fibre graphite felt/epoxy prepreg.
Step 3, with two pieces of identical polypropylene cyano carbon fiber and graphite felts for two blocks of identical polypropylene cyano carbon fiber stones
Black felt/paraffin prepreg；
Step 3.1, by the identical polypropylene cyano carbon fiber and graphite felt with material in two pieces of same steps 2, entirely
It is put into step 2 to fill in the glass guide channel of vasoliniment, impregnate 5 minutes, polypropylene cyano carbon fiber and graphite felt specification: length ×
Width × thickness size is 10cm × 10cm × 1cm；
After the completion of step 3.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper, the solidification of room temperature paraffin are adhered in surface again
Sealing of hole obtains two pieces of identical polypropylene cyano carbon fiber and graphite felt/paraffin prepregs, and paraffin sealing of hole thickness is in 4.5mm.
Step 4, with polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and two pieces of identical polypropylene cyano carbon fibers
Dimension graphite felt/paraffin prepreg suppresses the two-sided electrode plate containing paraffin；
Step 4.1 removes step 2, in 3 after the silicone oil paper on three prepreg surfaces of gained, and three pieces of prepregs are successively put
Enter into hot pressing die, is placed on intermediate polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and upper and lower layer polypropylene
Cyano carbon fiber and graphite felt/paraffin prepreg is not stacked with one side contacts of paraffin sealing of hole；
Step 4.2 closes grinding tool, is then warming up to 80 DEG C with the rate of 2.5 DEG C/min, keep the temperature after 180 minutes gels
150kgf/cm2It is hot-forming；
After step 4.3, molding, then 130 DEG C are warming up to the rate of 3 DEG C/min and keeps the temperature 90 minutes, last furnace cooling
Pressure release is taken out after to room temperature, and the two-sided electrode plate containing paraffin is made.
The two-sided electrode plate containing paraffin obtained by step 5, step 4 removes Lasaxing Oilfield, and the two-sided carbon fiber in porous structure is made
Tie up bipolar plates；
The resulting two-sided electrode plate containing paraffin of step 4 is put into 150 DEG C of silicone oil except deparaffnize, so by step 5.1
After be put into mass percent be 40%NaOH aqueous solution in, at 80 DEG C impregnate 3 hours；
Taking out after step 5.2, immersion and moving into the mass percent of boiling is that immersion is 3 small in 15% oxalic acid solution
When；
Step 5.3, immersion terminate, and are finally successively cleaned by ultrasonic 10 minutes in acetone and deionized water, being made two-sided is in
The bipolar plates of porous structure.
Polypropylene cyano carbon fiber and graphite felt/epoxy resin compacted zone among bipolar plates obtained is tested for the property,
Conductive plate conductivity is 2.4 × 102S/cm；Bending strength is 61MPa；Corrosion rate is 0.3 μ A/cm2。
| Conductivity (S/cm) | Bending strength (MPa) | Corrosion rate (μ A/cm2) | |
| Embodiment 1 | 2.3×102 | 64 | 0.2 |
| Embodiment 2 | 1.9×102 | 63 | 0.44 |
| Embodiment 3 | 2.1×102 | 66 | 0.17 |
| Embodiment 4 | 1.6×102 | 64 | 0.11 |
| Embodiment 5 | 2.4×102 | 61 | 0.3 |
Table 1
As can be seen from Table 1: polypropylene cyano carbon fiber and graphite felt/epoxy resin compacted zone conductive plate of embodiment 1-5
Conductivity, bending strength and corrosion rate reach and are better than U.S. Department of Energy bipolar plates performance standard, i.e. conductivity is greater than 100S/
Cm, bending strength are greater than 59MPa, and corrosion rate is less than 1 μ A/cm2。
Claims (8)
1. a kind of preparation method of the carbon fiber bipolar plates with three-dimensional porous structure, which is characterized in that specifically according to following step
It is rapid to implement:
Step 1 prepares epoxy resin adhesive liquid and vasoliniment；
Step 2, with polypropylene cyano carbon fiber and graphite felt for polypropylene cyano carbon fiber and graphite felt/epoxy prepreg；
Step 3, with two pieces of identical polypropylene cyano carbon fiber and graphite felts for two pieces of identical polypropylene cyano carbon fiber and graphite felts/
Paraffin prepreg；
Step 4, with polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and two blocks of identical polypropylene cyano carbon fiber stones
Black felt/paraffin prepreg suppresses the two-sided electrode plate containing paraffin；
The two-sided electrode plate containing paraffin obtained by step 5, step 4 removes Lasaxing Oilfield, and it is double that the two-sided carbon fiber in porous structure is made
Pole plate.
2. a kind of preparation method of carbon fiber bipolar plates with three-dimensional porous structure according to claim 1, feature
It is, the step 1 is specifically implemented according to the following steps:
Step 1.1 mixes epoxy resin, crosslinking agent and catalyst, magnetic agitation 10-30 minutes at a temperature of 50 DEG C -70 DEG C,
Obtain oxygen resin adhesive liquid；
Step 1.2, with 110-130 DEG C of silicone oil liquefied petrolatum, obtain vasoliniment.
3. a kind of preparation method of carbon fiber bipolar plates with three-dimensional porous structure according to claim 1, feature
It is, the step 2 is specifically implemented according to the following steps:
Polypropylene cyano carbon fiber and graphite felt is completely infused in the resulting epoxy resin adhesive liquid of step 1 by step 2.1, impregnates 1-5
Minute；
After the completion of step 2.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper is adhered on surface again, obtains polypropylene cyano carbon
Graphite fiber/epoxy prepreg.
4. a kind of preparation method of carbon fiber bipolar plates with three-dimensional porous structure according to claim 1, feature
It is, the step 3 is specifically implemented according to the following steps:
Two pieces of identical polypropylene cyano carbon fiber and graphite felts are entirely put into vasoliniment by step 3.1, and 1-5 points of dipping
Clock；
After the completion of step 3.2, dipping, taking-up is placed in silicone oil paper, and one layer of silicone oil paper, room temperature paraffin solidification envelope are adhered in surface again
Hole obtains two pieces of identical polypropylene cyano carbon fiber and graphite felt/paraffin prepregs.
5. a kind of preparation method of carbon fiber bipolar plates with three-dimensional porous structure according to claim 1, feature
It is, the step 4 is specifically implemented according to the following steps:
Step 4.1 removes step 2, in 3 after the silicone oil paper on three prepreg surfaces of gained, and three pieces of prepregs are sequentially placed into
In hot pressing die, it is placed on intermediate polypropylene cyano carbon fiber and graphite felt/epoxy prepreg and upper and lower layer polypropylene cyano
Carbon fiber and graphite felt/paraffin prepreg is not stacked with one side contacts of paraffin sealing of hole；
Step 4.2 closes grinding tool, is then warming up to 80 DEG C with the rate of 1-3 DEG C/min, keep the temperature after 120-180 minutes gels
100-150kgf/cm2It is hot-forming；
After step 4.3, molding, then 130 DEG C are warming up to the rate of 1-3 DEG C/min and keeps the temperature 60-90 minutes, be finally cooled to room
Pressure release is taken out after temperature, and the two-sided electrode plate containing paraffin is made.
6. a kind of preparation method of carbon fiber bipolar plates with three-dimensional porous structure according to claim 1, feature
It is, the step 5 is specifically implemented according to the following steps:
The resulting two-sided electrode plate containing paraffin of step 4 is put into 120-150 DEG C of silicone oil except deparaffnize, so by step 5.1
After to be put into mass percent be that mass percent is in 40%NaOH aqueous solution, 2-3 hour is impregnated at 80-90 DEG C；
It is that immersion 2-3 is a small in 15% oxalic acid solution that immigration is taken out after step 5.2, immersion in the mass percent of boiling
When；
Step 5.3, immersion terminate, and are finally successively cleaned by ultrasonic 8-10 minutes in acetone and deionized water, are made two-sided in more
The carbon fiber bipolar plates of pore structure.
7. a kind of preparation method of carbon fiber bipolar plates with three-dimensional porous structure according to claim 2, feature
It is, epoxy resin adhesive liquid configures in step 1, it is desirable that the weight percent of each component is epoxy resin: crosslinking agent: catalyst=
100:80-90:0.1-0.3。
8. a kind of preparation method of carbon fiber bipolar plates with three-dimensional porous structure according to claim 7, feature
It is, epoxy resin is bisphenol A-type, molecular weight 300-700 in the step 1；Crosslinking agent is hexanedioic acid；Catalyst is benzyl
Dimethylamine；Paraffin is No. 90 microwaxes.
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| CN111171518A (en) * | 2020-01-21 | 2020-05-19 | 西安理工大学 | Preparation method of carbon fiber composite electrode plate with thickness of 1mm |
| CN113388240A (en) * | 2021-06-15 | 2021-09-14 | 威驰腾(福建)汽车有限公司 | Graphite felt composite material and forming method thereof |
| CN114335584A (en) * | 2021-12-29 | 2022-04-12 | 深圳市贝特瑞新能源技术研究院有限公司 | Bipolar plate preform and preparation method thereof, bipolar plate and preparation method thereof, and fuel cell |
| CN117117229A (en) * | 2023-09-11 | 2023-11-24 | 苏州林森新能源材料科技有限公司 | Manufacturing process of impregnated graphite bipolar plate |
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