CN101017903A - Dual-electrode plate for Ti3SiC2/graphite proton exchange film fuel battery and its preparing method - Google Patents
Dual-electrode plate for Ti3SiC2/graphite proton exchange film fuel battery and its preparing method Download PDFInfo
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- CN101017903A CN101017903A CNA2007100512688A CN200710051268A CN101017903A CN 101017903 A CN101017903 A CN 101017903A CN A2007100512688 A CNA2007100512688 A CN A2007100512688A CN 200710051268 A CN200710051268 A CN 200710051268A CN 101017903 A CN101017903 A CN 101017903A
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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
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Abstract
The related TiSiC/graphite proton exchange film fuel cell bi-pole plate comprises: selecting Ti powder, Si powder, TiC power, Al power and graphite powder by mole ratio as: 1:(0.85-1.15):2: (0.1-0.2), wherein, graphite powder is 10-30vt%; every kind of powder has purity more than 98wt%, while partical fineness less than 15 mu m, except graphite powder less then 30 mu m. This product has high conductivity, well mechanical and anti-corrosivity performance, and fit to be applies in PEMFC.
Description
Technical field
The present invention relates to a kind of bipolar plates that is used for Proton Exchange Membrane Fuel Cells and preparation method thereof.
Background technology
Proton Exchange Membrane Fuel Cells (PEMFC) is a kind of Blast Furnace Top Gas Recovery Turbine Unit (TRT) that hydrogen and airborne combination with oxygen can be generated water and discharge electric energy.It has high power density, high-energy conversion ratio, cold-starting, advantage such as pollution-free.Its research has been become a focus in electrochemistry and the energy science field, caused the great attention of many developed countries and company, and invest heavily in this technology.At present, the major obstacle that hinders the PEMFC commercialized development is the price and the performance of its assembled material, comprises proton exchange membrane, catalyst and bipolar plates etc.Bipolar plates is the main support material of pemfc stack, and specifically, the function of bipolar plates and effect are as follows: (1) separates oxidant (oxygen or air) and reducing agent (hydrogen), has the choke function; (2) have collected current and drain function; (3) guarantee that battery pack temperature evenly distributes and the heat extraction scheme implementation good conductor of heat; (4) has resistance to corrosion (acid corrosion and oxide etch); (5) its flow field, both sides can make reacting gas evenly distribute in entire electrode everywhere.So the material that can be used for preparing bipolar plates is had following requirement: (1) material price is low, and the processing technology cost is low; (2) in light weight, plate is thin; (3) good mechanical performance (enough bending strengths and pliability, anti-vibration and impact); (4) high surface and volume conductance, low contact resistance; (5) low gas permeability and corrosion-resistant (poisoning film and catalyst); (6) high pyroconductivity.
The machine work graphite bi-polar plate owing to have function such as favorable conductive, thermal conductivity and corrosion resistance by generally as the bipolar plates of PEMFC, but because its complicated manufacturing process causes machine work graphite cake price high, there is reported in literature machine work graphite cake to account for the 40-60% of PEMFC cost greatly, becomes problem anxious to be solved in the PEMFC commercialization process.So the bipolar plate material that seek to substitute the machine work graphite bi-polar plate is in very among the active research, mainly contains two kinds of research thinkings at present: (1) metal and surface modifying material always; (2) polymer/conductive filler composite material.Though metal double polar plates has high conductivity, good mechanical strength, price is not high, and production technology is various, as coming processing gas flow field and cooling water flow field by punching press or etching, and can be processed into thin plate, reduce the battery volume, but under the sour environment of the high temperature of fuel cell and the about 2-3 of PH, dissolving and corrosion are unavoidably, particularly metal ion infiltrates and causes ionic conductivity decline and corrosion layer can increase contact resistance in the proton exchange membrane, reduces fuel battery performance.So, must modify the surface of metal double polar plates, improve its surface quality, but also do not find reasonable coating of durability and surface modification method at present.By graphite or powdered carbon filler and the compound bipolar plates of making of fluoropolymer resin is the another one research direction.Though the content of polymer very low (have less than 30wt%), but graphite/polymer composites has partly kept the processing characteristics of polymer basically, therefore, it can be by the typical plastics process technology as the goods of extruding, the materialize shape is done in mold pressing or injection.The flow field can be formed by the direct pressing mold of composite material, and needn't consider independent this step of expensive machine work.But bipolar plates mechanical strength and conductivity by this material are difficult to get both, and particularly conductivity is too low, and thermal conductivity is also bad, thereby lower by the pile power output of this class bipolar plates assembling.
At present, a kind of novel conducting ceramic material is arranged in the ceramic material family, as titanium silicon-carbon (Ti
3SiC
2), it is a kind of ceramic layered material, layer with layer between combine the graphite that feature class is similar to stratiform.It has the premium properties of metal and pottery simultaneously.The same with metal, good electric conductivity is arranged at normal temperatures, and (conductivity can reach 10
6S/cm) and heat conductivility (conductive coefficient 40W/m.K), relatively low Vickers hardness and higher modulus of elasticity have ductility at normal temperatures, can carry out machining as metal and graphite; Simultaneously, it has the performance of ceramic material again, and high yield strength is arranged, high-melting-point, high thermal stability and excellent corrosion resistance; And can prepare the very high block conductivity ceramics of purity by traditional sintering process, can be used to prepare turbine blade and stator, ceramic engine, bearing material, electrode material etc. utilize titanium silicon-carbon (Ti
3SiC
2) make the PEMFC bipolar plates and also do not appear in the newspapers.Although titanium silicon-carbon (Ti
3SiC
2) the various physical properties of conductivity ceramics can both satisfy the requirement of making the PEMFC bipolar plates, but this conductivity ceramics price comparison height, and than great, if directly adopt them to do the PEMFC bipolar plates, do not have very big competitive advantage, be unfavorable for promoting the commercialization of PEMFC.
Summary of the invention
The purpose of this invention is to provide a kind of titanium silicon-carbon/graphite used in proton exchange membrane fuel cell bipolar plates, its bipolar plates has high conductivity, good mechanical property and excellent corrosion resistance; Another object of the present invention provides the method for this bipolar plates of preparation, price and proportion that this method preparation technology is simple, reduced bipolar plates.
To achieve these goals, technical scheme of the present invention is: a kind of titanium silicon-carbon/graphite used in proton exchange membrane fuel cell bipolar plates, it is characterized in that it is mixed after hot pressed sintering forms by Ti powder, Si powder, TiC powder, Al powder and graphite powder raw material, the mol ratio of Ti powder, Si powder, TiC powder, Al powder raw material is n (Ti): n (Si): n (TiC): n (Al)=1: (0.85-1.15): 2: (0.1-0.2), the percent by volume that graphite powder accounts for whole raw material components is 10-30%; The purity of described Ti powder, Si powder, TiC powder, Al powder is all greater than 98wt%, and grain fineness is all less than 15 μ m; Described graphite powder is artificial graphite powder, and purity is greater than 98wt%, and grain fineness is less than 30 μ m.
The preparation method of above-mentioned a kind of titanium silicon-carbon/graphite used in proton exchange membrane fuel cell bipolar plates is characterized in that it comprises the steps:
1) mol ratio by Ti powder, Si powder, TiC powder, Al powder raw material is n (Ti): n (Si): n (TiC): n (Al)=1: (0.85-1.15): 2: (0.1-0.2) take by weighing Ti powder, Si powder, TiC powder and Al powder and mix, get compound, the percent by volume that compound accounts for whole raw material components is 70-90%; Compound is added ball grinder, and mill ball adopts stainless steel or carbide alloy, and the weight ratio of ball and compound is 10: 1-100: 1, and ball grinder vacuumizes, and drum's speed of rotation is 150-350r/min, room-temperature ball-milling 1-4 hour; The purity of described Ti powder, Si powder, TiC powder, Al powder is all greater than 98wt%, and grain fineness is less than 15 μ m;
2) take by weighing graphite powder, the percent by volume that graphite powder accounts for whole raw material components is 10-30%; Adopt the mechanical agitation mode fully to mix the compound behind graphite powder and the above-mentioned ball milling, mixed powder; Described graphite powder is artificial graphite powder, and purity is greater than 98wt%, and grain fineness is less than 30 μ m;
3) above-mentioned mixed powder is packed in the graphite jig, the graphite jig inwall scribbles boron nitride (BN) coating, puts into the vacuum heating-press sintering stove and carries out hot pressed sintering; At first be pre-stressed to 3-5MPa during sintering, heat up then, heating rate 20-60 ℃/min, temperature is pressurized to 30-60MPa after being raised to sintering temperature 1300-1800 ℃ immediately, and heat-insulation pressure keeping 1hr, and feeding argon gas in the whole sintering process is protective gas;
4) naturally cool to room temperature under the pressurize, depanning also promptly gets tabula rasa with the sand papering sample surfaces then;
5) adopt conventional process for machining to make gas flowfield, get titanium silicon-carbon/graphite used in proton exchange membrane fuel cell bipolar plates on the tabula rasa surface.
The present invention has overcome the preparation technology of traditional machine work graphite bi-polar plate complexity, a kind of titanium silicon-carbon/graphite used in proton exchange membrane fuel cell bipolar plates has been proposed, compound with a certain amount of graphite in the synthetic preparation process of titanium silicon-carbon sintering, reduced the price and the proportion of bipolar plates, can adopt conventional process for machining to make gas flowfield on the tabula rasa surface.
Cost of manufacture of the present invention is low, and when having overcome the composite material moulded moulding of polymer/conductive filler and making bipolar plates, the difficult problem that conductivity and mechanical property can not get both has simultaneously overcome the not corrosion-resistant problem of metal and surface modifying material bipolar plates.
The present invention and existing method relatively have following advantage:
1) the present invention adopts in the synthetic preparation process of titanium silicon-carbon sintering and the compound bipolar plates of making of a certain amount of graphite, and the bipolar plates volume conductance can reach 10
3-10
4S/cm, the twin shaft bending strength can reach 50-100MPa, has high conductivity, good mechanical property, considerably beyond the performance requirement that USDOE proposed.
2) bipolar plates of the present invention's making has excellent decay resistance and antioxygenic property, by the pem fuel power output height of its assembling, good endurance, long operational time, stable performance.
3) simple, the price and the proportion that have reduced bipolar plates of preparation technology of the present invention, this bipolar plates are used in that PEMFC goes up its price and proportion can be accepted.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
According to n (Ti): n (Si): n (TiC): n (Al)=1: 1.15: 2: 0.1 takes by weighing Ti powder, Si powder, TiC powder and Al powder respectively mixed, get compound, compound is added ball grinder, mill ball adopts stainless steel or carbide alloy, the weight ratio of ball and compound is 50: 1, ball grinder vacuumizes, and drum's speed of rotation is 200r/min, room-temperature ball-milling 2 hours; The purity of described Ti powder, Si powder, TiC powder, Al powder is all greater than 98wt%, and grain fineness is all less than 15 μ m; Take by weighing graphite powder, the percent by volume that graphite powder accounts for whole raw material components is 10%; Described graphite powder is artificial graphite powder, and purity is greater than 98wt%, and grain fineness is less than 30 μ m; Adopt the mechanical agitation mode fully to mix the compound behind graphite powder and the above-mentioned ball milling, mixed powder; Above-mentioned mixed powder is packed in the graphite jig, and the graphite jig inwall scribbles boron nitride (BN) coating, puts into the vacuum heating-press sintering stove and carries out hot pressed sintering; At first be pre-stressed to 3MPa during sintering, heat up then, 40 ℃/min of heating rate, temperature is pressurized to 35MPa after being raised to 1400 ℃ of sintering temperatures immediately, and heat-insulation pressure keeping 1hr (hour), feeding argon gas in the whole sintering process is protective gas; Naturally cool to room temperature under the pressurize, depanning also promptly gets tabula rasa with the sand papering sample surfaces then; Adopt conventional process for machining to make gas flowfield, get titanium silicon-carbon/graphite used in proton exchange membrane fuel cell bipolar plates on the tabula rasa surface.Its basic physical property test result such as table 1.
Embodiment 2:
The preparation method is with embodiment 1, and only the amount of graphite powder being replaced by the percent by volume that graphite powder accounts for whole raw material components is 20%.Its basic physical property test result such as table 1.
Embodiment 3:
The preparation method is with embodiment 1, and only the amount of graphite powder being replaced by the percent by volume that graphite powder accounts for whole raw material components is 30%.Its basic physical property test result such as table 1.
Embodiment 4:
According to n (Ti): n (Si): n (TiC): n (Al)=1: 0.85: 2: 0.2 takes by weighing Ti powder, Si powder, TiC powder and Al powder respectively mixed, get compound, compound is added ball grinder, mill ball adopts stainless steel or carbide alloy, the weight ratio of ball and compound is 50: 1, ball grinder vacuumizes, and drum's speed of rotation is 200r/min, room-temperature ball-milling 2 hours; The purity of described Ti powder, Si powder, TiC powder, Al powder is all greater than 98wt%, and grain fineness is less than 15 μ m; Take by weighing graphite powder, the percent by volume that graphite powder accounts for whole raw material components is 10%; Described graphite powder is artificial graphite powder, and purity is greater than 98wt%, and grain fineness is less than 30 μ m; Adopt the mechanical agitation mode fully to mix the compound behind graphite powder and the above-mentioned ball milling, mixed powder; Above-mentioned mixed powder is packed in the graphite jig, and the graphite jig inwall scribbles boron nitride (BN) coating, puts into the vacuum heating-press sintering stove and carries out hot pressed sintering; At first be pre-stressed to 3MPa during sintering, heat up then, 40 ℃/min of heating rate, temperature is pressurized to 50MPa after being raised to 1600 ℃ of sintering temperatures immediately, and heat-insulation pressure keeping 1hr, and feeding argon gas in the whole sintering process is protective gas; Naturally cool to room temperature under the pressurize, depanning also promptly gets tabula rasa with the sand papering sample surfaces then; Adopt conventional process for machining to make gas flowfield, get titanium silicon-carbon/graphite used in proton exchange membrane fuel cell bipolar plates on the tabula rasa surface.Its basic physical property test result such as table 1.
Embodiment 5:
The preparation method is with embodiment 4, and only the amount of graphite powder being replaced by the percent by volume that graphite powder accounts for whole raw material components is 20%.Its basic physical property test result such as table 1.
Embodiment 6:
The preparation method is with embodiment 4, and only the amount of graphite powder being replaced by the percent by volume that graphite powder accounts for whole raw material components is 30%.Its basic physical property test result such as table 1.
Table 1
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 |
| Conductivity (S/cm) | 5.1×10 4 | 1.5×10 4 | 7.5×10 3 | 9.1×10 4 | 6.2×10 4 | 4.1×10 4 |
| Bending strength (MPa) | 87 | 57 | 50 | 93 | 64 | 52 |
| Corrosion electric current density (A/cm 2) | 2.1×10 -6 | 8.3×10 -6 | 9.7×10 -6 | 1.5×10 -6 | 7.1×10 -6 | 9.4×10 -6 |
| Density (g/cm 3) | 3.24 | 3.02 | 2.79 | 3.08 | 2.97 | 2.82 |
The bound value and the interval value of Ti powder of the present invention, Si powder, TiC powder, Al powder and graphite powder raw material can both be realized the present invention, and the bound value of preparation process condition and interval value can both realize the present invention, just do not enumerate embodiment one by one at this.
Claims (2)
1. titanium silicon-carbon/graphite used in proton exchange membrane fuel cell bipolar plates, it is characterized in that it is mixed after hot pressed sintering forms by Ti powder, Si powder, TiC powder, Al powder and graphite powder raw material, the mol ratio of Ti powder, Si powder, TiC powder, Al powder raw material is 1: (0.85-1.15): 2: (0.1-0.2), the percent by volume that graphite powder accounts for whole raw material components is 10-30%; The purity of described Ti powder, Si powder, TiC powder, Al powder is all greater than 98wt%, and grain fineness is less than 15 μ m; Described graphite powder is artificial graphite powder, and purity is greater than 98wt%, and grain fineness is less than 30 μ m.
2. the preparation method of a kind of titanium silicon-carbon as claimed in claim 1/graphite used in proton exchange membrane fuel cell bipolar plates is characterized in that it comprises the steps:
1) mol ratio by Ti powder, Si powder, TiC powder, Al powder raw material is 1: (0.85-1.15): 2: (0.1-0.2) take by weighing Ti powder, Si powder, TiC powder and Al powder and mix, get compound, the percent by volume that compound accounts for whole raw material components is 70-90%; Compound is added ball grinder, and mill ball adopts stainless steel or carbide alloy, and the weight ratio of ball and compound is 10: 1-100: 1, and ball grinder vacuumizes, and drum's speed of rotation is 150-350r/min, room-temperature ball-milling 1-4 hour; The purity of described Ti powder, Si powder, TiC powder, Al powder is all greater than 98wt%, and grain fineness is less than 15 μ m;
2) take by weighing graphite powder, the percent by volume that graphite powder accounts for whole raw material components is 10-30%; Adopt the mechanical agitation mode fully to mix the compound behind graphite powder and the above-mentioned ball milling, mixed powder; Described graphite powder is artificial graphite powder, and purity is greater than 98wt%, and grain fineness is less than 30 μ m;
3) above-mentioned mixed powder is packed in the graphite jig, the graphite jig inwall scribbles boron nitride coating, puts into the vacuum heating-press sintering stove and carries out hot pressed sintering; At first be pre-stressed to 3-5MPa during sintering, heat up then, heating rate 20-60 ℃/min, temperature is pressurized to 30-60MPa after being raised to sintering temperature 1300-1800 ℃ immediately, and heat-insulation pressure keeping 1hr, and feeding argon gas in the whole sintering process is protective gas;
4) naturally cool to room temperature under the pressurize, depanning also promptly gets tabula rasa with the sand papering sample surfaces then;
5) adopt conventional process for machining to make gas flowfield, get titanium silicon-carbon/graphite used in proton exchange membrane fuel cell bipolar plates on the tabula rasa surface.
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|---|---|---|---|
| CNB2007100512688A CN100479246C (en) | 2007-01-16 | 2007-01-16 | Dual-electrode plate for Ti3SiC2/graphite proton exchange film fuel battery and its preparing method |
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| CN100479246C CN100479246C (en) | 2009-04-15 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009108102A1 (en) * | 2008-02-27 | 2009-09-03 | Impact Coatings Ab | Electrode with a coating, method in production thereof and use of a material |
| CN107146898A (en) * | 2017-05-31 | 2017-09-08 | 安徽理工大学 | A kind of proton exchange mould fuel battery metal double polar plate wet-milling warm-pressing sintering method |
| CN112786909A (en) * | 2020-12-18 | 2021-05-11 | 国科微城市智能科技(南京)有限责任公司 | Ceramic composite bipolar plate for hydrogen fuel cell |
| CN113524768A (en) * | 2021-06-23 | 2021-10-22 | 河南城建学院 | Pressing device for graphite bipolar plate of fuel cell |
| CN115332554A (en) * | 2022-10-14 | 2022-11-11 | 江苏金亚隆科技有限公司 | Manufacturing method of fuel cell pole plate based on expanded graphite |
| CN117776690A (en) * | 2024-02-27 | 2024-03-29 | 北京利尔高温材料股份有限公司 | Sol-combined blast furnace iron runner gunning material |
-
2007
- 2007-01-16 CN CNB2007100512688A patent/CN100479246C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009108102A1 (en) * | 2008-02-27 | 2009-09-03 | Impact Coatings Ab | Electrode with a coating, method in production thereof and use of a material |
| CN107146898A (en) * | 2017-05-31 | 2017-09-08 | 安徽理工大学 | A kind of proton exchange mould fuel battery metal double polar plate wet-milling warm-pressing sintering method |
| CN112786909A (en) * | 2020-12-18 | 2021-05-11 | 国科微城市智能科技(南京)有限责任公司 | Ceramic composite bipolar plate for hydrogen fuel cell |
| CN112786909B (en) * | 2020-12-18 | 2022-04-12 | 国科微城市智能科技(南京)有限责任公司 | Ceramic composite bipolar plate for hydrogen fuel cell |
| CN113524768A (en) * | 2021-06-23 | 2021-10-22 | 河南城建学院 | Pressing device for graphite bipolar plate of fuel cell |
| CN115332554A (en) * | 2022-10-14 | 2022-11-11 | 江苏金亚隆科技有限公司 | Manufacturing method of fuel cell pole plate based on expanded graphite |
| CN117776690A (en) * | 2024-02-27 | 2024-03-29 | 北京利尔高温材料股份有限公司 | Sol-combined blast furnace iron runner gunning material |
| CN117776690B (en) * | 2024-02-27 | 2024-05-31 | 北京利尔高温材料股份有限公司 | Sol-combined blast furnace iron runner gunning material |
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