CN101593837B - Expanded graphite/phenolic resin composite bipolar plate and preparation method thereof - Google Patents
Expanded graphite/phenolic resin composite bipolar plate and preparation method thereof Download PDFInfo
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Abstract
膨胀石墨/酚醛树脂复合材料双极板及其制备方法，它涉及一种双极板及其制备方法。本发明解决了质子交换膜燃料电池双极板导电性差、机械性能差问题。本发明双极板由膨胀石墨、热塑性酚醛树脂和六次甲基四胺制成，方法如下：将膨胀石墨与热塑性酚醛树脂的水溶液混合、过滤，然后将滤渣干燥后与六次甲基四胺球磨混合，再加入模具中模压，然后减压、升温，再保温模压、脱模，即得膨胀石墨/酚醛树脂复合材料双极板。本发明方法所得双极板的导电率为105.8～159.2S/cm、抗弯强度为33.1～30.62MPa、抗压强度为82～76MPa、里氏硬度为645～625，孔隙率为0.078～0.118g/cm3，电化学腐蚀速度为6.146～5.172μA/cm2。An expanded graphite/phenolic resin composite material bipolar plate and a preparation method thereof relate to a bipolar plate and a preparation method thereof. The invention solves the problems of poor conductivity and poor mechanical properties of the bipolar plate of the proton exchange membrane fuel cell. The bipolar plate of the present invention is made of expanded graphite, thermoplastic phenolic resin and hexamethylenetetramine, and the method is as follows: the aqueous solution of expanded graphite and thermoplastic phenolic resin is mixed and filtered, and then the filter residue is dried and mixed with hexamethylenetetramine Mixed by ball milling, then put into a mold for molding, then depressurize, heat up, heat-preserve, mold, and demould to obtain a bipolar plate made of expanded graphite/phenolic resin composite material. The electrical conductivity of the bipolar plate obtained by the method of the present invention is 105.8-159.2 S/cm, the bending strength is 33.1-30.62 MPa, the compressive strength is 82-76 MPa, the Leeb hardness is 645-625, and the porosity is 0.078-0.118g /cm 3 , the electrochemical corrosion rate is 6.146～5.172μA/cm 2 .
Description
Technical field
The present invention relates to a kind of bipolar plates and preparation method thereof.
Background technology
Fuel cell (Fuel Cell) is as the supply unit of a kind of high-energy-density, high-energy conversion ratio, environment-friendly type and be subjected to the whole world and pay close attention to widely.Bipolar plates is the important component part of fuel cell, and it is battery-allocated fuel and oxidant, and the polyphone adjacent single cells.It is graphite or metal that present tradition is used to produce the dual polar plates of proton exchange membrane fuel cell material, big with Metal Production bipolar plate material weight, because the high corrosion-resistant of graphite and low-density character, the feasible bipolar plate material of producing with graphite is than using the in light weight of Metal Production bipolar plate material, but the thickness with the bipolar plate material of graphite production is several millimeters to tens millimeters, so difficulty is processed, (bending strength is 10～20MPa to bad mechanical property, compression strength is 50～70MPa, lee ' hardness is 400～500, and poorly conductive (conductance is 50S/cm).Existing bipolar plates account for fuel cell weight 60～80% and fuel cell total cost 40～50%, caused the problem that fuel cell weight is big, cost is high.
Summary of the invention
Technical problem to be solved by this invention is in order to solve dual polar plates of proton exchange membrane fuel cell poorly conductive, bad mechanical property problem, a kind of expanded graphite/phenolic resin composite bipolar plate and preparation method thereof to be provided.
Expanded graphite/phenolic resin composite bipolar plate of the present invention is made by expanded graphite, novolac resin and hexamethylenetetramine; Wherein the mass ratio of expanded graphite and novolac resin is 1: 3～3: 1, and the quality of hexamethylenetetramine is 5%～20% of a novolac resin quality, and the expansion multiple of described expanded graphite is 100～300ml/g.
The preparation method of expanded graphite/phenolic resin composite bipolar plate of the present invention is as follows: will be that to join temperature be in 100 ℃ the aqueous solution of novolac resin for 1: 3～3: 1 expanded graphite with the novolac resin mass ratio one,, stir 10min～20min, be cooled to room temperature, filtration then, with filter residue dry 24h under 50 ℃～100 ℃ condition, obtain composite material again; Two, be the hexamethylenetetramine and composite material ball milling mixing 2h～12h of novolac resin quality 5%～20% with quality, obtain compound; Two, be the hexamethylenetetramine and composite material ball milling mixing 2h～12h of novolac resin quality 5%～20% with quality, obtain compound; Three, compound is joined in the mould, again mould is put into YSS-1 type double-speed manual hydraulic press, the pressure that is molding die 5～30min four under the condition of 20～50MPa at normal temperature, pressure then, is decompressed on the mould then is 10～40MPa, it is 120～250 ℃ that decompression time makes the temperature in the hot pressing furnace with the programming rate of 10～30 ℃/min, is that 120～250 ℃, pressure are insulation mold pressing 5～30min under the condition of 10～40MPa in temperature then; Five, then 50 ℃～150 ℃ temperature bottom knockout, be cooled to room temperature, can obtain expanded graphite/phenolic resin composite bipolar plate.
Above-mentioned Preparation of Expanded Graphite method is as follows: one, be that 50～120 purpose crystalline flake graphites, mass concentration are that 70%～72% perchloric acid, mass concentration are that 85% the SPA and the mixture of potassium bichromate stir 20～60min in 60 ℃ of waters bath with thermostatic control with fineness; Two, suction filtration then is neutral with distilled water washing filter residue to washing lotion in the time of suction filtration, stops suction filtration; Three, the filter residue that step 2 is obtained is put into crucible with filter residue then at 55 ℃ drying box inner drying 24h, crucible is placed in the microwave oven with the power microwave heating 10s of 800W again, promptly obtains the expanded graphite that expansion multiple is 100～300ml/g; Wherein the mass ratio of crystalline flake graphite and perchloric acid is 1: 1～2 in the step 1, and crystalline flake graphite is 1: 1～3 with the ratio of SPA, and the mass ratio of crystalline flake graphite and potassium bichromate is 5: 1～3.
The inventive method gained expanded graphite/phenolic resin composite bipolar plate has the advantage of good conductivity, good mechanical property; Its conductance is that 105.8～159.2S/cm, bending strength are that 33.1～30.62MPa, compression strength are that 82～76MPa, lee ' hardness are 645～625, and porosity is 0.078～0.118g/cm
3, electrochemical corrosion speed is 6.146～5.172 μ A/cm
2
Description of drawings
Fig. 1 is that 1000 times SEM figure is amplified on embodiment 11 gained expanded graphite/phenolic resin composite bipolar plates surface).Fig. 2 is that 10000 times SEM figure is amplified on embodiment 11 gained expanded graphite/phenolic resin composite bipolar plates surface.Fig. 3 is that embodiment 12 gained expanded graphite/phenolic resin composite bipolar plate sections amplify 1000 times SEM figure.Fig. 4 is that embodiment 12 gained expanded graphite/phenolic resin composite bipolar plate sections amplify 5000 times SEM figure.Fig. 5 is the steady-state polarization of the expanded graphite/phenolic resin composite bipolar plate of embodiment 13 gained.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: expanded graphite/phenolic resin composite bipolar plate is made by expanded graphite, novolac resin and hexamethylenetetramine in the present embodiment; Wherein the mass ratio of expanded graphite and novolac resin is 1: 3～3: 1, and the quality of hexamethylenetetramine is 5%～20% of a novolac resin quality, and the expansion multiple of described expanded graphite is 100～300ml/g.
Embodiment two: present embodiment and embodiment one are different is that the mass ratio of expanded graphite and novolac resin is 2: 1.Other is identical with embodiment one.
Embodiment three: present embodiment is different with embodiment one or two is that the addition of hexamethylenetetramine is 10% of a novolac resin quality.Other is identical with embodiment one or two.
Embodiment four: present embodiment is different with embodiment one or two is that the addition of hexamethylenetetramine is 8%～18% of a novolac resin quality.Other is identical with embodiment one or two.
Embodiment five: the preparation method of expanded graphite/phenolic resin composite bipolar plate is as follows in the present embodiment: will be that to join temperature be in 100 ℃ the aqueous solution of novolac resin for 1: 3～3: 1 expanded graphite with the novolac resin mass ratio one,, stir 10min～20min, be cooled to room temperature, filtration then, with filter residue dry 24h under 50 ℃～100 ℃ condition, obtain composite material again; Two, be the hexamethylenetetramine and composite material ball milling mixing 2h～12h of novolac resin quality 5%～20% with quality, obtain compound; Three, compound being joined in the mould, mould is put into YSS-1 type double-speed manual hydraulic press again, is molding die 5～30min under the condition of 20～50MPa at normal temperature, pressure then; Four, the pressure that is decompressed to then on the mould is 10～40MPa, it is 120～250 ℃ that decompression time makes the temperature in the hot pressing furnace with the programming rate of 10～30 ℃/min, is that 120～250 ℃, pressure are insulation mold pressing 5～30min under the condition of 10～40MPa in temperature then; Five, then 50 ℃～150 ℃ temperature bottom knockout, be cooled to room temperature, promptly get expanded graphite/phenolic resin composite bipolar plate.
The used novolac resin phenolic resins of present embodiment is water insoluble, and novolac resin will become oil supernatant on water shape material (phenolic resins) after directly putting in 100 ℃ of water, adds the phenolic resins of expanded graphite absorption oily then.
Ball milling balls grinding machine is that the model that Nanjing Univ. Instrument Factory produces is the planetary ball mill of QM-SB in the present embodiment step 2, and used abrading-ball is the big ball of 2cm and bead that diameter is 1cm according to 1: 1 number than forming by diameter; YSS-1 type double-speed manual hydraulic press described in the step 3 is produced by the state-run elegance and talent in Harbin instrument plant.
The conductance of the inventive method gained expanded graphite/phenolic resin composite bipolar plate is that 105.8～159.2S/cm, bending strength are that 33.1～30.62MPa, compression strength are that 82～76MPa, lee ' hardness are 645～625MPa, and porosity is 0.078～0.118g/cm
3, electrochemical corrosion speed is 6.146～5.172 μ A/cm
2
Embodiment six: what present embodiment and embodiment five were different is that the described Preparation of Expanded Graphite method of step 1 is as follows: one, be that 50～120 purpose crystalline flake graphites, mass concentration are that 70%～72% perchloric acid, mass concentration are that 85% the SPA and the mixture of potassium bichromate stir 20～60min in 60 ℃ of waters bath with thermostatic control with fineness; Two, suction filtration then is neutral with distilled water washing filter residue to washing lotion in the time of suction filtration, stops suction filtration; Three, the filter residue that step 2 is obtained is put into crucible with filter residue then at 55 ℃ drying box inner drying 24h, crucible is placed in the microwave oven with the power microwave heating 10s of 800W again, promptly obtains the expanded graphite that expansion multiple is 100～300ml/g; Wherein the mass ratio of crystalline flake graphite and perchloric acid is 1: 1～2 in the step 1, and crystalline flake graphite is 1: 1～3 with the ratio of SPA, and the mass ratio of crystalline flake graphite and potassium bichromate is 5: 1～3.Other is identical with embodiment five.
The expansion multiple of present embodiment gained expanded graphite is 100～300ml/g.
The expansion multiple of expanded graphite is the volume of gained expanded graphite and the ratio of expanded graphite quality in the present embodiment.
Embodiment seven: present embodiment is different with embodiment five or six is that to add in the step 1 with the novolac resin mass ratio be 2: 1 expanded graphite.Other is identical with embodiment five or six.
Embodiment eight: what present embodiment and embodiment seven were different is.In other and embodiment seven same steps as one that filter residue is dry under 80 ℃ condition.
Embodiment nine: present embodiment and embodiment five, six or eight are different is that the addition of hexamethylenetetramine described in the step 2 is 10% of a novolac resin quality.Other is identical with embodiment five, six or eight.
Embodiment ten: present embodiment and embodiment nine are different is to be molding die under the condition of 30MPa at pressure in the step 3.Other is identical with embodiment nine.
Embodiment 11: the method for expanded graphite/phenolic resin composite bipolar plate in the present embodiment, the preparation method who it is characterized in that expanded graphite/phenolic resin composite bipolar plate is as follows: will be that to join temperature be in 100 ℃ the aqueous solution of novolac resin for 1: 1 expanded graphite with the novolac resin mass ratio one,, stir 15min, be cooled to room temperature, filtration then, with filter residue dry 24h under 90 ℃ condition, obtain composite material again; Two, be the hexamethylenetetramine and composite material ball milling mixing 10h of novolac resin quality 15% with quality, obtain compound; Three, compound being joined in the mould, mould is put into YSS-1 type double-speed manual hydraulic press again, is molding die 25min under the condition of 20MPa at normal temperature, pressure then; Four, the pressure that is decompressed to then on the mould is 30MPa, and making the temperature in the hot pressing furnace with the programming rate of 10 ℃/min in the time of decompression is 250 ℃, is that 250 ℃, pressure are insulation mold pressing 30min under the condition of 40MPa in temperature then; Five, then 100 ℃ temperature bottom knockout, be cooled to room temperature, promptly get expanded graphite/phenolic resin composite bipolar plate.
Can see that by Fig. 1 (1000 times SEM figure is amplified on present embodiment gained expanded graphite/phenolic resin composite bipolar plate surface) and Fig. 2 (10000 times SEM figure is amplified on present embodiment gained expanded graphite/phenolic resin composite bipolar plate surface) present embodiment gained expanded graphite/phenolic resin composite bipolar plate surface is smoother, compactness is better, thereby improved the mechanical strength of present embodiment gained expanded graphite/phenolic resin composite bipolar plate, reduced the porosity of present embodiment gained expanded graphite/phenolic resin composite bipolar plate.
The conductance of present embodiment gained expanded graphite/phenolic resin composite bipolar plate is that 105.8S/cm, bending strength are that 33.1MPa, compression strength are that 82MPa, lee ' hardness are 645MPa, and porosity is 0.078g/cm
3, electrochemical corrosion speed is 6.146 μ A/cm
2
Embodiment 12: the method for expanded graphite/phenolic resin composite bipolar plate in the present embodiment, the preparation method who it is characterized in that expanded graphite/phenolic resin composite bipolar plate is as follows: will be that to join temperature be in 100 ℃ the aqueous solution of novolac resin for 1.5: 1 expanded graphite with the novolac resin mass ratio one,, stir 20min, be cooled to room temperature, filtration then, with filter residue dry 24h under 80 ℃ condition, obtain composite material again; Two, be the hexamethylenetetramine and composite material ball milling mixing 8h of novolac resin quality 18% with quality, obtain compound; Three, compound being joined in the mould, mould is put into YSS-1 type double-speed manual hydraulic press again, is molding die 20min under the condition of 40MPa at normal temperature, pressure then; Four, the pressure that is decompressed to then on the mould is 20MPa, and making the temperature in the hot pressing furnace with the programming rate of 25 ℃/min in the time of decompression is 200 ℃, is that 200 ℃, pressure are insulation mold pressing 25min under the condition of 30MPa in temperature then; Five, then 90 ℃ temperature bottom knockout, be cooled to room temperature, promptly get expanded graphite/phenolic resin composite bipolar plate.
Find out that by Fig. 3 (present embodiment gained expanded graphite/phenolic resin composite bipolar plate section amplifies 1000 times SEM figure) expanded graphite in the expanded graphite/phenolic resin composite bipolar plate that present embodiment obtains and phenolic resins are in conjunction with closely, resin disperses more even between expanded graphite particles, from Fig. 4 (present embodiment gained expanded graphite/phenolic resin composite bipolar plate section amplifies 5000 times SEM figure), can see that phenolic resins is filled between the laminar sheet of expanded graphite, combine closelyr between phenolic resins and the expanded graphite stratiform thin slice, promptly present embodiment gained expanded graphite/phenolic resin composite compactness is better.
The conductance of present embodiment gained expanded graphite/phenolic resin composite bipolar plate is that 159.2S/cm, bending strength are that 30.62MPa, compression strength are that 76MPa, lee ' hardness are 625MPa, and porosity is 0.118g/cm
3, electrochemical corrosion speed is 5.172 μ A/cm
2
Embodiment 13: the method for expanded graphite/phenolic resin composite bipolar plate in the execution mode, the preparation method who it is characterized in that expanded graphite/phenolic resin composite bipolar plate is as follows: will be that to join temperature be in 100 ℃ the aqueous solution of novolac resin for 1.8: 1 expanded graphite with the novolac resin mass ratio one,, stir 12min, be cooled to room temperature, filtration then, with filter residue dry 24h under 70 ℃ condition, obtain composite material again; Two, be the hexamethylenetetramine and composite material ball milling mixing 3h of novolac resin quality 8% with quality, obtain compound; Three, compound being joined in the mould, mould is put into YSS-1 type double-speed manual hydraulic press again, is molding die 19min under the condition of 30MPa at normal temperature, pressure then; Four, the pressure that is decompressed to then on the mould is 15MPa, and making the temperature in the hot pressing furnace with the programming rate of 15 ℃/min in the time of decompression is 180 ℃, is that 180 ℃, pressure are insulation mold pressing 10min under the condition of 15MPa in temperature then; Five, then 120 ℃ temperature bottom knockout, be cooled to room temperature, promptly get expanded graphite/phenolic resin composite bipolar plate.
The corrosion electric current density that can draw the expanded graphite/phenolic resin composite bipolar plate of present embodiment gained through the CHI660A computed in software according to curve among the figure among Fig. 5 (steady-state polarization of the expanded graphite/phenolic resin composite bipolar plate of present embodiment gained) is 5.17 * 10
-6A/cm
2, corrosion electric current density is less, and the expanded graphite/phenolic resin composite bipolar plate corrosion resistance of present embodiment gained is better.
The conductance of the inventive method gained expanded graphite/phenolic resin composite bipolar plate is that 115.8S/cm, bending strength are that 32.1MPa, compression strength are that 80MPa, lee ' hardness are 635, and porosity is 0.078～0.118g/cm
3
Claims (10)
1. expanded graphite/phenolic resin composite bipolar plate is characterized in that expanded graphite/phenolic resin composite bipolar plate made by expanded graphite, novolac resin and hexamethylenetetramine; Wherein the mass ratio of expanded graphite and novolac resin is 1: 3～3: 1, and the quality of hexamethylenetetramine is 5%～20% of a novolac resin quality, and the expansion multiple of described expanded graphite is 100～300ml/g.
2. expanded graphite/phenolic resin composite bipolar plate according to claim 1, the mass ratio that it is characterized in that expanded graphite and novolac resin is 2: 1.
3. expanded graphite/phenolic resin composite bipolar plate according to claim 1 and 2, the addition that it is characterized in that hexamethylenetetramine is 8%～18% of a novolac resin quality.
4. expanded graphite/phenolic resin composite bipolar plate according to claim 1 and 2, the addition that it is characterized in that hexamethylenetetramine is 10% of a novolac resin quality.
5. the method for preparing the described expanded graphite/phenolic resin composite bipolar plate of claim 1, the preparation method who it is characterized in that expanded graphite/phenolic resin composite bipolar plate is as follows: will be that to join temperature be in 100 ℃ the aqueous solution of novolac resin for 1: 3～3: 1 expanded graphite with the novolac resin mass ratio one,, stir 10min～20min, be cooled to room temperature, filtration then, with filter residue dry 24h under 50 ℃～100 ℃ condition, obtain composite material again; Two, be the hexamethylenetetramine and composite material ball milling mixing 2h～12h of novolac resin quality 5%～20% with quality, obtain compound; Three, compound being joined in the mould, mould is put into YSS-1 type double-speed manual hydraulic press again, is molding die 5～30min under the condition of 20～50MPa at normal temperature, pressure then; Four, the pressure that is decompressed to then on the mould is 10～40MPa, it is 120～250 ℃ that decompression time makes the temperature in the hot pressing furnace with the programming rate of 10～30 ℃/min, is that 120～250 ℃, pressure are insulation mold pressing 5～30min under the condition of 10～40MPa in temperature then; Five, then 50～150 ℃ temperature bottom knockout, be cooled to room temperature, promptly get expanded graphite/phenolic resin composite bipolar plate.
6. the preparation method of expanded graphite/phenolic resin composite bipolar plate according to claim 5 is characterized in that the described Preparation of Expanded Graphite method of step 1 is as follows: one, be that 50～120 purpose crystalline flake graphites, mass concentration are that 70%～72% perchloric acid, mass concentration are that 85% the SPA and the mixture of potassium bichromate stir 20～60min in 60 ℃ of waters bath with thermostatic control with fineness; Two, suction filtration then is neutral with distilled water washing filter residue to washing lotion in the time of suction filtration, stops suction filtration; Three, the filter residue that step 2 is obtained is put into crucible with filter residue then at 55 ℃ drying box inner drying 24h, crucible is placed in the microwave oven with the power microwave heating 10s of 800W again, promptly obtains the expanded graphite that expansion multiple is 100～300ml/g; Wherein the mass ratio of crystalline flake graphite and perchloric acid is 1: 1～2 in the step 1, and crystalline flake graphite is 1: 1～3 with the ratio of SPA, and the mass ratio of crystalline flake graphite and potassium bichromate is 5: 1～3.
7. according to the preparation method of claim 5 or 6 described expanded graphite/phenolic resin composite bipolar plates, it is characterized in that adding in the step 1 with the novolac resin mass ratio is 2: 1 expanded graphite.
8. the preparation method of expanded graphite/phenolic resin composite bipolar plate according to claim 7 is characterized in that in the step 1 filter residue is dry under 80 ℃ condition.
9. according to the preparation method of claim 5,6 or 8 described expanded graphite/phenolic resin composite bipolar plates, the addition that it is characterized in that hexamethylenetetramine described in the step 2 is 10% of a novolac resin quality.
10. the preparation method of expanded graphite/phenolic resin composite bipolar plate according to claim 9 is characterized in that in the step 3 that at pressure be molding die under the condition of 30MPa.
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| CN101859905B (en) * | 2010-06-23 | 2012-06-20 | 湖南大学 | Method for preparing graphite/resin compound bipolar plate for fuel cell |
| CN103811778B (en) * | 2011-06-01 | 2016-03-09 | 南通大学 | The dual polar plates of proton exchange membrane fuel cell that mechanical property, conduction and thermal conductivity are good |
| CN103159481B (en) * | 2013-03-12 | 2014-07-30 | 武汉科技大学 | Composite carbon raw material for carbon-containing refractory material and preparation method thereof |
| CN103633340B (en) * | 2013-12-17 | 2016-06-08 | 哈尔滨工业大学 | A kind of modified expanded graphite base composite material double pole plate and preparation method thereof |
| CN106189058A (en) * | 2016-07-18 | 2016-12-07 | 宜昌新成石墨有限责任公司 | A kind of soft graphite composite board and preparation method thereof |
| CN106189228A (en) * | 2016-07-20 | 2016-12-07 | 周荣 | A kind of preparation method of modified graphite base composite material double pole plate |
| CN115347208B (en) * | 2022-10-17 | 2023-01-03 | 江苏金亚隆科技有限公司 | Preparation process of graphite polar plate |
| CN119252960B (en) * | 2024-12-06 | 2025-03-11 | 唐山金湾特碳石墨有限公司 | Preparation method of fuel cell graphite composite board and graphite composite board prepared by same |
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