CN109244501B - Fuel cell bipolar plate composite material and preparation method and application thereof - Google Patents
Fuel cell bipolar plate composite material and preparation method and application thereof Download PDFInfo
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- CN109244501B CN109244501B CN201811116196.5A CN201811116196A CN109244501B CN 109244501 B CN109244501 B CN 109244501B CN 201811116196 A CN201811116196 A CN 201811116196A CN 109244501 B CN109244501 B CN 109244501B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0223—Composites
- H01M8/0226—Composites in the form of mixtures
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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 invention provides a fuel cell bipolar plate composite material and a preparation method and application thereof. The fuel cell bipolar plate composite material comprises graphite powder, perovskite oxide, rare earth element modified lanthanum oxide and novolac epoxy type vinyl resin, and an effective conductive path is formed in an insulating layer in the novolac epoxy type vinyl resin under the compounding of the raw materials, so that the negative influence of a coating layer on the conductivity is weakened, and the conductivity is greatly improved; meanwhile, due to the addition of perovskite oxide and rare earth element modified lanthanum oxide, a conductive channel can be further increased to form tunnel current, so that the conductivity is improved; in addition, the bending strength of the composite material is improved under the compounding of the raw materials. The conductivity of the fuel cell bipolar plate composite material prepared by the invention is determined as follows: 502-590S/cm; the bending strength is 68-75 MPa.
Description
Technical Field
The invention relates to the field of conductive composite materials, in particular to a fuel cell bipolar plate composite material and a preparation method and application thereof.
Background
The bipolar plate is one of the key components of a Proton Exchange Membrane Fuel Cell (PEMFC), and has the functions of separating gas, introducing reaction gas into the fuel cell through a flow field, collecting conduction current, supporting a membrane electrode and simultaneously playing a role in heat dissipation and water drainage of the whole fuel cell system. Therefore, the bipolar plate composite material is required to have better conductivity and mechanical property. Currently, bipolar plates can be classified into the following three types according to material classification: the graphite bipolar plate has good electric and thermal conductivity and chemical stability, but the machining process of the graphite bipolar plate is long in time consumption and low in production efficiency, so that the machining cost of the graphite bipolar plate is higher and even exceeds the material cost, in addition, the performance of the graphite bipolar plate is brittle, and the air leakage is easily caused by the existence of internal pores of the graphite bipolar plate, so that the air tightness of the graphite bipolar plate is ensured by keeping a certain thickness, and the increase of the volume specific power and the weight specific power of a stack of the graphite bipolar plate is restricted; the metal mold has high precision requirement and high cost, and the metal mold has good electric and thermal conductivity to a metal base material, particularly to a surface plate of the metal base material, can be thinned to 0.1mm without air leakage, and a gas flow passage can be formed by punching, so that batch production is easy to realize, which is beneficial to the improvement of volume specific power and the reduction of manufacturing cost, but the finished surface of the metal bipolar plate is specially treated to improve the chemical stability of the metal bipolar plate, otherwise, the metal plate is easy to corrode and even rust, and the service life of a battery is shortened and even catastrophic damage occurs; the graphite/resin composite bipolar plate has the advantages of good processing performance, easy mass production, good corrosion resistance and low cost, thereby becoming a hotspot of research.
For example, chinese patent document CN1054105406092A discloses a fuel cell bipolar plate composite material and a preparation method thereof, wherein the composite material comprises the following raw materials: the method is characterized in that two natural crystalline flake graphite grading materials with different sizes are used as conductive fillers, graphene or conductive carbon black is used as auxiliary conductive fillers, novolac epoxy type vinyl resin is used as a binder, TBPB and BPO are used as resin curing composite initiators, the two natural crystalline flake graphite with different sizes are graded, a proper amount of nano filler conductive carbon black or graphene is added to prepare a mould pressing material by compounding with the novolac epoxy type vinyl resin binder, and the mould pressing material is pressed and cured at a certain temperature, pressure and time to prepare a sample. However, the electrical conductivity and bending strength of the fuel cell bipolar plate composite material prepared by the above-mentioned technology still need to be improved.
Therefore, it is a technical problem to be solved by those skilled in the art to develop a novel fuel cell bipolar plate composite material with better electrical conductivity and bending strength resistance to meet the requirement of the fuel cell field for a bipolar plate material with higher performance.
Disclosure of Invention
The invention provides a fuel cell bipolar plate composite material which has better electrical conductivity and bending strength resistance, and further provides a preparation method and application thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows:
in a first aspect of the present invention, a fuel cell bipolar plate composite is provided, which comprises the following raw materials: graphite powder, perovskite oxide, rare earth element modified lanthanum oxide and novolac epoxy type vinyl resin.
Preferably, the preparation method of the rare earth element modified lanthanum oxide is as follows:
dispersing lanthanum oxide into a water solution containing rare earth elements to perform ion exchange reaction, collecting a solid phase after the reaction is finished, and drying and roasting the solid phase to obtain rare earth element modified lanthanum oxide; the rare earth element is yttrium or cerium.
Preferably, the concentration of the aqueous solution containing the rare earth elements is 0.1-0.5 mol/L; the mass ratio of the lanthanum oxide to the rare earth elements is 1: (5-10); the reaction temperature is 20-80 ℃, and the reaction time is 4-6 h; the drying temperature is 90-150 ℃, and the drying time is 1-3 h; the roasting temperature is 400-600 ℃, and the roasting time is 1-6 h.
Preferably, the perovskite oxide is La0.7Sr0.3Fe0.3Mn0.7O3、LaCuO3、La0.6Sr0.4FeO3Or LaFe0.3Mn0.7O3。
In the fuel cell bipolar plate composite material, the mass ratio of the graphite powder to the perovskite oxide, the rare earth element modified lanthanum oxide and the novolac epoxy type vinyl resin is preferably (65-85): (1-2): (0.5-1): (10-20).
In a second aspect of the present invention, a method for preparing the fuel cell bipolar plate composite material is provided, which comprises the following steps:
(1) mixing graphite powder, perovskite oxide, rare earth element modified lanthanum oxide and novolac epoxy type vinyl resin by adopting ultrasound, wherein the ultrasonic mixing time is 10-20 min, preferably 15min, and forming a blend;
(2) vacuumizing and drying the blend in the step (1), wherein the drying temperature is 50-70 ℃, preferably 60 ℃, and the time is 6-10 hours, preferably 8 hours;
(3) compression molding the dried blend in the step (2) in a molding die, wherein the pressing temperature is 90-110 ℃, preferably 100 ℃, the pressing pressure is 12-20 Mpa, and the pressing time is 20-30 min; and then molding at 140-170 ℃ and preserving heat for 20-40 min, and demolding to obtain the fuel cell bipolar plate composite material.
In a third aspect of the invention, a fuel cell bipolar plate composite material prepared by the preparation method is provided.
In a fourth aspect of the invention, the invention provides a use of the fuel cell bipolar plate composite material or the fuel cell bipolar plate composite material prepared by the preparation method in preparing a fuel cell bipolar plate.
The technical scheme of the invention has the following advantages:
(1) the fuel cell bipolar plate composite material comprises graphite powder, perovskite oxide, rare earth element modified lanthanum oxide and novolac epoxy type vinyl resin, and an effective conductive path is formed in an insulating layer in the novolac epoxy type vinyl resin under the compounding of the raw materials, so that the negative influence of a coating layer on the conductivity is weakened, and the conductivity is greatly improved; meanwhile, due to the addition of perovskite oxide and rare earth element modified lanthanum oxide, a conductive channel can be further increased to form tunnel current, so that the conductivity is improved; in addition, the bending strength of the composite material is improved under the compounding of the raw materials. The conductivity of the fuel cell bipolar plate composite material prepared by the invention is determined as follows: 502-590S/cm; the bending strength is 68-75 MPa.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
The present embodiment provides a fuel cell bipolar plate composite;
the fuel cell bipolar plate composite material bagComprises the following raw materials: graphite powder, LaCuO3Cerium-modified lanthanum oxide and novolac epoxy type vinyl resin;
in the raw materials, the mass ratio of graphite powder to LaCuO3, cerium-modified lanthanum oxide and novolac epoxy type vinyl resin is 65:2:0.5: 10.
In this example, the preparation method of the cerium-modified lanthanum oxide is as follows:
dispersing 1g of lanthanum oxide into a cerium nitrate aqueous solution with the concentration of 0.5mol/L (the mass ratio of lanthanum oxide to cerium is 1: 5), carrying out ion exchange at 20 ℃, filtering after 6h of reaction, collecting a solid phase, drying the solid phase at 150 ℃ for 1h, and roasting at 400 ℃ for 6h to prepare cerium modified lanthanum oxide;
the invention further provides a preparation method of the fuel cell bipolar plate composite material, which comprises the following steps:
(1) mixing the graphite powder, LaCuO3, cerium modified lanthanum oxide and novolac epoxy type vinyl resin in the selected mass ratio by ultrasound for 10min to form a blend;
(2) vacuumizing and drying the blend in the step (1) at the drying temperature of 70 ℃ for 6 hours;
(3) carrying out compression molding on the dried blend in the step (2) in a molding die, wherein the pressing temperature is 90 ℃, the pressing pressure is 20Mpa, and the pressing time is 20 min; and then molding at 140 ℃ and preserving heat for 40min, and demolding to obtain the fuel cell bipolar plate composite material.
Example 2
The present embodiment provides a fuel cell bipolar plate composite;
the fuel cell bipolar plate composite material comprises the following raw materials: graphite powder, La0.7Sr0.3Fe0.3Mn0.7O3Yttrium-modified lanthanum oxide and novolac epoxy type vinyl resins;
among the above raw materials, graphite powder and La0.7Sr0.3Fe0.3Mn0.7O3The mass ratio of yttrium modified lanthanum oxide to novolac epoxy type vinyl resin is 85:1:1:20。
In this example, the preparation method of the yttrium-modified lanthanum oxide is as follows:
dispersing 1g of lanthanum oxide into an yttrium nitrate aqueous solution with the concentration of 0.1mol/L (the mass ratio of lanthanum oxide to yttrium is 1: 10), carrying out ion exchange at 80 ℃, filtering after 4h of reaction, collecting a solid phase, drying the solid phase at 90 ℃ for 3h, and then roasting at 600 ℃ for 1h to prepare yttrium modified lanthanum oxide;
the invention further provides a preparation method of the fuel cell bipolar plate composite material, which comprises the following steps:
(1) mixing the graphite powder and La in the selected mass ratio0.7Sr0.3Fe0.3Mn0.7O3Mixing yttrium modified lanthanum oxide and novolac epoxy type vinyl resin by using ultrasound, wherein the ultrasonic mixing time is 20min, and forming a blend;
(2) vacuumizing and drying the blend in the step (1) at the drying temperature of 50 ℃ for 10 hours;
(3) carrying out compression molding on the dried blend in the step (2) in a molding die, wherein the pressing temperature is 110 ℃, the pressing pressure is 12Mpa, and the pressing time is 30 min; and then molding at 170 ℃ and preserving the heat for 20min, and demolding to obtain the fuel cell bipolar plate composite material.
Example 3
The present embodiment provides a fuel cell bipolar plate composite;
the fuel cell bipolar plate composite material comprises the following raw materials: graphite powder, La0.6Sr0.4FeO3Yttrium-modified lanthanum oxide and novolac epoxy type vinyl resins;
among the above raw materials, graphite powder and La0.6Sr0.4FeO3The mass ratio of yttrium modified lanthanum oxide to novolac epoxy type vinyl resin is 80:1.5:0.8: 15.
In this example, the preparation method of the yttrium-modified lanthanum oxide is as follows:
dispersing 1g of lanthanum oxide into an yttrium nitrate aqueous solution with the concentration of 0.2mol/L (the mass ratio of lanthanum oxide to yttrium is 1: 8), carrying out ion exchange at 60 ℃, filtering after 5h of reaction, collecting a solid phase, drying the solid phase at 120 ℃ for 2h, and roasting at 500 ℃ for 5h to prepare yttrium modified lanthanum oxide;
the invention further provides a preparation method of the fuel cell bipolar plate composite material, which comprises the following steps:
(1) mixing the graphite powder and La in the selected mass ratio0.6Sr0.4FeO3Mixing yttrium modified lanthanum oxide and novolac epoxy type vinyl resin by using ultrasound, wherein the ultrasonic mixing time is 15min, and forming a blend;
(2) vacuumizing and drying the blend in the step (1) at the drying temperature of 60 ℃ for 8 hours;
(3) carrying out compression molding on the dried blend in the step (2) in a molding die, wherein the pressing temperature is 100 ℃, the pressing pressure is 15Mpa, and the pressing time is 25 min; and then molding at 150 ℃ and preserving the temperature for 30min, and demolding to obtain the fuel cell bipolar plate composite material.
Example 4
The present embodiment provides a fuel cell bipolar plate composite;
the fuel cell bipolar plate composite material comprises the following raw materials: graphite powder, LaFe0.3Mn0.7O3Cerium-modified lanthanum oxide and novolac epoxy type vinyl resin;
among the above raw materials, graphite powder and LaFe0.3Mn0.7O3The mass ratio of the cerium modified lanthanum oxide to the novolac epoxy type vinyl resin is 70:1.2:0.6: 12.
In this example, the preparation method of the cerium-modified lanthanum oxide is as follows:
dispersing 1g of lanthanum oxide into a cerium nitrate aqueous solution with the concentration of 0.4mol/L (the mass ratio of lanthanum oxide to cerium is 1: 6), carrying out ion exchange at 30 ℃, filtering after 4h of reaction, collecting a solid phase, drying the solid phase at 130 ℃ for 3h, and roasting at 550 ℃ for 2h to prepare cerium modified lanthanum oxide;
the invention further provides a preparation method of the fuel cell bipolar plate composite material, which comprises the following steps:
(1) mixing graphite powder and LaFe at the mass ratio0.3Mn0.7O3Mixing the cerium modified lanthanum oxide and the novolac epoxy type vinyl resin by adopting ultrasound, wherein the ultrasonic mixing time is 18min, and forming a blend;
(2) vacuumizing and drying the blend in the step (1) at 65 ℃ for 7 hours;
(3) carrying out compression molding on the dried blend in the step (2) in a molding die, wherein the pressing temperature is 105 ℃, the pressing pressure is 18Mpa, and the pressing time is 28 min; and then molding at 160 ℃ and preserving heat for 35min, and demolding to obtain the fuel cell bipolar plate composite material.
Example 5
The present embodiment provides a fuel cell bipolar plate composite;
the fuel cell bipolar plate composite material comprises the following raw materials: graphite powder, LaFe0.3Mn0.7O3Cerium-modified lanthanum oxide and novolac epoxy type vinyl resin;
among the above raw materials, graphite powder and LaFe0.3Mn0.7O3The mass ratio of the cerium modified lanthanum oxide to the novolac epoxy type vinyl resin is 75:1.8:0.8: 18.
In this example, the preparation method of the cerium-modified lanthanum oxide is as follows:
dispersing 1g of lanthanum oxide into a cerium nitrate aqueous solution with the concentration of 0.1mol/L (the mass ratio of lanthanum oxide to cerium is 1: 9), carrying out ion exchange at 70 ℃, filtering after 6h of reaction, collecting a solid phase, drying the solid phase at 150 ℃ for 3h, and then roasting at 400 ℃ for 1h to prepare cerium modified lanthanum oxide;
the invention further provides a preparation method of the fuel cell bipolar plate composite material, which comprises the following steps:
(1) mixing graphite powder and LaFe at the mass ratio0.3Mn0.7O3The cerium modified lanthanum oxide and the novolac epoxy type vinyl resin are mixed by ultrasound, the ultrasonic mixing time is 11min, and the mixture is shapedForming a blend;
(2) vacuumizing and drying the blend in the step (1) at 55 ℃ for 9 hours;
(3) carrying out compression molding on the dried blend in the step (2) in a molding die, wherein the pressing temperature is 110 ℃, the pressing pressure is 18Mpa, and the pressing time is 30 min; and then molding at 170 ℃ and preserving the heat for 40min, and demolding to obtain the fuel cell bipolar plate composite material.
Experimental example 1
The electrical conductivity and bending strength of the fuel cell bipolar plate composite materials prepared in examples 1 to 5 were measured. The results are shown in Table 1.
TABLE 1 conductivity and flexural Strength of Fuel cell Bipolar plate composites prepared in examples 1-5
| Conductivity (s/cm) | Flexural Strength (MPa) | |
| Example 1 | 502 | 70 |
| Example 2 | 511 | 68 |
| Example 3 | 590 | 74 |
| Example 4 | 583 | 75 |
| Example 5 | 567 | 72 |
As can be seen from Table 1, the bending strength of the fuel cell bipolar plate composite material prepared by the embodiment of the invention is higher than the technical index (25MPa) of US DOE.
The fuel cell bipolar plate composite material prepared by the invention has higher conductivity and bending strength.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (5)
1. A fuel cell bipolar plate composite material is characterized by comprising the following raw materials: graphite powder, perovskite oxide, rare earth element modified lanthanum oxide and novolac epoxy type vinyl resin;
the preparation method of the rare earth element modified lanthanum oxide comprises the following steps:
dispersing lanthanum oxide into a water solution containing rare earth elements to perform ion exchange reaction, collecting a solid phase after the reaction is finished, and drying and roasting the solid phase to obtain rare earth element modified lanthanum oxide;
the concentration of the aqueous solution containing the rare earth elements is 0.1-0.5 mol/L; the mass ratio of the lanthanum oxide to the rare earth elements is 1: (5-10); the rare earth element is yttrium or cerium;
the mass ratio of the graphite powder to the perovskite oxide, the rare earth element modified lanthanum oxide and the novolac epoxy type vinyl resin is (65-85): (1-2): (0.5-1): (10-20);
the perovskite oxide is La0 .7Sr0 .3Fe0 .3Mn0 .7O3、LaCuO3、La0 .6Sr0 .4FeO3Or LaFe0 .3Mn0 .7O3。
2. The fuel cell bipolar plate composite of claim 1,
the ion exchange reaction temperature is 20-80 ℃, and the time is 4-6 h;
the drying temperature is 90-150 ℃, and the drying time is 1-3 h;
the roasting temperature is 400-600 ℃, and the roasting time is 1-6 h.
3. A method of making the fuel cell bipolar plate composite of claim 1 or 2, comprising the steps of:
(1) mixing graphite powder, perovskite oxide, rare earth element modified lanthanum oxide and novolac epoxy type vinyl resin by adopting ultrasound, wherein the ultrasonic mixing time is 10-20 min, and forming a blend;
(2) vacuumizing and drying the blend in the step (1), wherein the drying temperature is 50-70 ℃, and the drying time is 6-10 hours;
(3) compression molding the dried blend in the step (2) in a molding die, wherein the pressing temperature is 90-110 ℃, the pressing pressure is 12-20 MPa, and the pressing time is 20-30 min; and then molding at 140-170 ℃ and preserving heat for 20-40 min, and demolding to obtain the fuel cell bipolar plate composite material.
4. A fuel cell bipolar plate composite produced by the production method according to claim 3.
5. Use of the fuel cell bipolar plate composite material according to claim 1 or 2 or the fuel cell bipolar plate composite material prepared by the preparation method according to claim 3 in the preparation of a fuel cell bipolar plate.
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| CN1555106A (en) * | 2003-12-26 | 2004-12-15 | 清华大学 | Process for preparing fuel cell bipolar plate and composite material used thereof |
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