CN101051691A - Geo polymer base composite material double pole plate and its preparing method - Google Patents

Geo polymer base composite material double pole plate and its preparing method Download PDF

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Publication number
CN101051691A
CN101051691A CNA2007100521583A CN200710052158A CN101051691A CN 101051691 A CN101051691 A CN 101051691A CN A2007100521583 A CNA2007100521583 A CN A2007100521583A CN 200710052158 A CN200710052158 A CN 200710052158A CN 101051691 A CN101051691 A CN 101051691A
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metakaolin
water glass
graphite
carbon fiber
pole plate
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CN100438174C (en
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王发洲
沈春晖
张云升
丁庆军
胡曙光
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Wuhan University of Technology WUT
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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
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    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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Abstract

Characters of bipolar plate of polymer based composite material are that it is produced from materials of Meta kaolin, conductance material, and solution of water glass. The conductance material is composed of graphite and carbon fiber. Doping quantity of graphite is 20-40% of mass of meta kaolin, and doping quantity of carbon fiber is 10-20%. Mass ratio between solution of water glass, meta kaolin, and conductance material 0.4-0.8:1. The said Meta kaolin is obtained by calcinating kaolin in coal series sold on market or pure kaolin at 600-850 deg.C. Modulus m of solution of water glass is equal to 2.8-3.5, and Baume degree is equal to 35-45. Features of the bipolar plate are: low cost, good corrosion resistance, high mechanical strength, light weight, good conductivity, no poison and pollution on fuel cell of proton exchange membrane.

Description

A kind of geopolymer base composite material double pole plate and preparation method thereof
Technical field
The present invention relates to a kind of dual polar plates of proton exchange membrane fuel cell and preparation method thereof.
Background technology
Proton Exchange Membrane Fuel Cells (PEMFC) is owing to energy conversion efficiency height, environmental friendliness, stable performance, clean production, at aspects such as vehicle-mounted driving power, compact power and home-use power stations very wide application prospect is arranged, become an important development direction of novel energy.
But the too high PEMFC of being of cost is difficult to the principal element of commercial applications at present.Wherein, bipolar plates accounts for 70%～80% of whole PEMFC gross mass, and cost accounts for 40%～50% of total cost.At present, bipolar plate material mainly contains three kinds: graphite bi-polar plate, metal double polar plates and composite material double pole plate, but they all have obvious defects: graphite type material mechanical strength (particularly bending strength) is low, fragility is big, be difficult to sheet, poor air-tightness, and processing cost height (its processing cost accounts for more than 50% of total cost); The density of metal double polar plates is big, and is perishable; Composite material double pole plate then technology is still not really ripe, and cost is also high.Therefore, select suitable bipolar plate material, rational preparation technology,, improve the performance of battery in the hope of the internal resistance that reduces battery, the power output that improves battery.
Summary of the invention
The object of the present invention is to provide geopolymer base composite material double pole plate of a kind of low-cost and high-performance and preparation method thereof.
To achieve these goals, technical scheme of the present invention is: a kind of geopolymer base composite material double pole plate is characterized in that it is formed by metakaolin, conducting material and water glass solution feedstock production; Conducting material is made up of graphite and carbon fiber, and the graphite volume is 20～40% of a metakaolin quality, and carbon fiber content is 10%～20% of a metakaolin quality; The mass ratio of water glass solution and metakaolin and conducting material is 0.4～0.8: 1;
Described metakaolin is Coaseries kaolin or the washed kaolin that sell the market, calcines gained under 600～850 ℃ high temperature; Modulus m=2.8～3.5 of described water glass solution, Baume degrees Be=35～45.Water glass solution is made of sodium metasilicate, NaOH and water, adjusts modulus and Baume degrees by NaOH and water.
The modulus m=3.19 of described water glass solution, Baume degrees Be=39.2.
Purity 〉=the 99.85wt% of described graphite, fineness＜90 μ m.
The length of described carbon fiber is less than 4mm, diameter＜0.2mm.
The preparation method of above-mentioned a kind of geopolymer base composite material double pole plate is characterized in that it comprises the steps:
1) be 20～40% of metakaolin quality according to the graphite volume, carbon fiber content is 10%～20% of a metakaolin quality, the mass ratio of water glass solution and metakaolin and conducting material is to choose metakaolin, graphite, carbon fiber and water glass solution raw material at 0.4～0.8: 1, and wherein conducting material is made up of graphite and carbon fiber; Described metakaolin is Coaseries kaolin or the washed kaolin that sell the market, calcines gained under 600～850 ℃ high temperature; Modulus m=2.8～3.5 of described water glass solution, Baume degrees Be=35～45;
2), get powder with metakaolin and conducting material mixing and stirring; Water glass solution is joined in the powder, fully stir again and obtain slurry;
3) slurry injects the metal die that has reverse gas flow, hot pressing 15min～20min under 120～180 ℃ of conditions, and the demoulding is placed on 20 ± 2 ℃ after the demoulding, and maintenance 14d obtains the bipolar plates biscuit under the condition of relative humidity 95 ± 5%;
4) the bipolar plates biscuit is placed in the weak acid solution of circulation and soaks 10～12h, the pH=5 of weak acid solution～6, pass through water purification circulation rinsing then after, be dried into the geopolymer base composite material double pole plate.
Hydration mechanism of the present invention is: when water glass solution adds in the powder (metakaolin and conducting material), after the powder particle contacts, dissolve OH in a large number -Anion forms alkali metal cation and OH -Ion colloidal solution, these ion bonding forces dissolve covalent bonds such as Si-O-Si, Si-O-Al rapidly, discharge the Si and the Al monomer that move freely, dissolving the monomer that then is reconstructed and self-organizing, polycondensation reaction when the monomer of reconstruct is similar to organic high molecular polymer formation, polymerization becomes network-like class zeolite silicoaluminate, and chemical formula is expressed as follows:
Figure A20071005215800041
Figure A20071005215800042
Figure A20071005215800044
The silicate cement hydration sclerosis generates Ca (OH) 2Crystal and oligomeric aquation silicic acid gel (mainly at dimerization and tripolymer), crystal interweaves mutually and bonds together with unformed material, mainly based on Van der Waals key and hydrogen bond.And that the geopolymer material is [Si-O-Al-O-] nThe three-dimensional net structure of forming, the extent of polymerization height, and there is not the Ca component, mainly based on ionic bond and covalent bond, at high temperature also can keep network configuration complete, thereby the geopolymer material has the intensity higher than cement, hardness, toughness, high-temperature stability, the burn into of anti-strong acid is water-fast thermal environment effect.
Metakaolin (geopolymer) has following main feature:
1) excellent corrosion resistance, the H 5% 2SO 4After solution soaked 60d, mass loss rate had only 7%;
2) volume stability is good, and the volume contraction value of 28d has only 0.5%;
3) hypotonicity, the permeability of metakaolin are 10 -10(normal concrete then is 10 to the order of magnitude of m/s -9～10 -10The order of magnitude);
4) intensity height, 28d bending strength 10～15MPa, compression strength is more than the 90MPa;
5) production cost is low, and the energy consumption of metakaolin is to produce 1/6～1/4 of cement, 1/20 of pottery, 1/70 of steel, 1/150 of plastics.
The performance index of geopolymer base composite material double pole plate:
1), conductivity＞100S/cm;
2), corrosion resistance: corrosion rate＜0.016mA/cm 2
3), intensity: bending strength＞20MPa;
4), gas barrier property: maximum average transmission coefficient＜1.0 * 10 -4Cm 3/ (scm 2);
5), density:＜2.2g/cm 3
6), cost of material:＜100RMB/kg;
7), bipolar plates total cost:＜0.05RMB/cm 2
The present invention is to be matrix with metakaolin (geopolymer), add graphite and carbon fiber and do conductive filler, with the water glass solution is alkali-activator, thereby obtains a kind of geopolymer base composite material double pole plate (guaranteeing to reduce cost of bipolar plates significantly on conductance, the intensity based) of low-cost and high-performance.The bipolar plates that the present invention makes has that cost is low, corrosion resistance and good, mechanical strength height, in light weight, conduct electricity very well, long-time running is to Proton Exchange Membrane Fuel Cells nonhazardous and pollution, cheap characteristics.
Embodiment
Comparing embodiment 1 (electric conducting material is a graphite):
1) choose 3 groups of raw materials (sequence number 1-3) by table 1, liquid is water glass solution in the table 1, admittedly be metakaolin and conducting material (following identical).
2) metakaolin and conducting material are fully stirred with JJ-5 type cement plaster blender, mix, get powder; Water glass solution is joined in the powder that mixes, fully stir again and obtain slurry;
3) slurry injects the metal die that has reverse gas flow, hot pressing 15min under 120～180 ℃ of conditions, and the demoulding is placed on 20 ℃ after the demoulding, and maintenance 14d obtains the bipolar plates biscuit under the condition of relative humidity 95 ± 5%;
4) the bipolar plates biscuit be placed on soak 12h in the weak acid solution (pH=5～6) of circulation, pass through water purification circulation rinsing then after, be dried into the geopolymer base composite material double pole plate.
Its every performance is tested, the results are shown in Table 2.
Table 1
Sequence number Metakaolin/g Electric conducting material/g Liquid-solid ratio The water glass solution parameter
Graphite Carbon fiber Modulus/m Baume degrees/Be Volume/g
1 1000 100 0 0.4 3.19 39.2 440
2 1000 200 0 0.4 3.19 39.2 480
3 1000 400 0 0.4 3.19 39.2 560
Table 2 The performance test results
Sequence number Conductivity Intensity/MPa Rate of corrosion Maximum average saturating Density
S/cm Compression strength Bending strength mA/cm 2 Cross coefficient cm 3/ (s·cm 2) g/cm 2
1 56 80 18 0.0057 3.7×10 -6 2.34
2 89 67 14 0.0059 1.9×10 -6 2.08
3 112 50 12 0.0048 0.7×10 -6 1.82
The result of table 2 shows: when electric conducting material was graphite, intensity was low.
Comparing embodiment 2 (electric conducting material is a carbon fiber):
1) chooses 2 groups of raw materials (sequence number 1-2) by table 3.
2) metakaolin and conducting material are fully stirred with JJ-5 type cement plaster blender, mix, get powder; Water glass solution is joined in the powder that mixes, fully stir again and obtain slurry;
3) slurry injects the metal die that has reverse gas flow, hot pressing 15min under 120～180 ℃ of conditions, and the demoulding is placed on 20 ℃ after the demoulding, and maintenance 14d obtains the bipolar plates biscuit under the condition of relative humidity 95 ± 5%;
4) the bipolar plates biscuit be placed on soak 12h in the weak acid solution (pH=5～6) of circulation, pass through water purification circulation rinsing then after, be dried into the geopolymer base composite material double pole plate.
Its every performance is tested, the results are shown in Table 4.
Table 3
Sequence number Metakaolin/g Electric conducting material/g Liquid-solid ratio The water glass solution parameter
Graphite Carbon fiber Modulus/m Baume degrees/Be Volume/g
1 1000 0 100 0.4 3.19 39.2 440
2 1000 0 200 0.4 3.19 39.2 480
Table 4 The performance test results
Sequence number Conductivity S/cm Intensity/MPa Rate of corrosion mA/cm 2 Maximum average transmission coefficient cm 3/ (s·cm 2) Density g/cm 2
Compression strength Bending strength
1 67.8 90 23 0.0041 2.8×10 -6 1.98
2 89.7 98.7 28 0.0048 1.7×10 -6 1.73
The result of table 4 shows: when electric conducting material is carbon fiber, and the intensity height.
Comparing embodiment 3 (electric conducting material is graphite and carbon fiber):
1) chooses 2 groups of raw materials (sequence number 1-2) by table 5.
2) metakaolin and conducting material are fully stirred with JJ-5 type cement plaster blender, mix, get powder; Water glass solution is joined in the powder that mixes, fully stir again and obtain slurry;
3) slurry injects the metal die that has reverse gas flow, hot pressing 15min under 120～180 ℃ of conditions, and the demoulding is placed on 20 ℃ after the demoulding, and maintenance 14d obtains the bipolar plates biscuit under the condition of relative humidity 95 ± 5%;
4) the bipolar plates biscuit be placed on soak 12h in the weak acid solution (pH=5～6) of circulation, pass through water purification circulation rinsing then after, be dried into the geopolymer base composite material double pole plate.
Its every performance is tested, the results are shown in Table 6.
Table 5
Sequence number Metakaolin/g Electric conducting material/g Liquid-solid ratio The water glass solution parameter
Graphite Carbon fiber Modulus/m Baume degrees/Be Volume/g
1 1000 100 100 0.4 3.19 39.2 480
2 1000 100 200 0.4 3.19 39.2 520
Table 6 The performance test results
Sequence number Conductivity S/cm Intensity/MPa Rate of corrosion mA/cm 2 Maximum average transmission coefficient cm 3/ (s·cm 2) Density g/cm 2
Compression strength Bending strength
1 86.7 86 14 0.0049 2.7×10 -6 2.27
2 97.1 98 24 0.0044 2.4×10 -6 2.21
Table 6 The performance test results shows, when the graphite volume less than the metakaolin quality 20% the time, conductivity＜100S/cm.
Embodiment 1:
A kind of preparation method of geopolymer base composite material double pole plate, it comprises the steps:
1) chooses 4 groups of raw materials (sequence number 1-4) by table 7.Described metakaolin is Coaseries kaolin or the washed kaolin that sell the market, calcines gained under 600～850 ℃ high temperature.Purity 〉=the 99.85wt% of described graphite, fineness＜90 μ m.The length of described carbon fiber is less than 4mm, diameter＜0.2mm.
2) metakaolin and conducting material are fully stirred with JJ-5 type cement plaster blender, mix, get powder; Water glass solution is joined in the powder that mixes, fully stir again and obtain slurry;
3) slurry is after JJ-5 type cement plaster blender fully stirs, injection has the metal die (bipolar plates mould) of reverse gas flow, hot pressing 15min under 120～180 ℃ of conditions, the demoulding, be placed on 20 ± 2 ℃ after the demoulding, maintenance 14d obtains the bipolar plates biscuit under the condition of relative humidity 95 ± 5%, and the biscuit quality that obtains is hard, smooth surface is smooth, flawless;
4) because alkali-activator (being water glass solution) can not complete reaction fall when geopolymer (being metakaolin) forms, a small amount of unnecessary waterglass will decompose Na in fuel cell +, SiO 3 2-The plasma stripping, thus the power output of fuel cell influenced; In order to address this problem, the bipolar plates biscuit is placed in the weak acid solution (pH=5～6 are as sulfuric acid solution) of circulation and soaks 10～12h, pass through water purification circulation rinsing then after, be dried into the geopolymer base composite material double pole plate.
Geopolymer base composite material double pole plate The performance test results sees Table 8
Table 7
Sequence number Metakaolin/g Electric conducting material/g Liquid-solid ratio The water glass solution parameter
Graphite Carbon fiber Modulus/m Baume degrees/Be Volume/g
1 1000 200 100 0.4 3.19 39.2 520
2 1000 200 200 0.4 3.19 39.2 480
3 1000 400 100 0.4 3.19 39.2 600
4 1000 400 200 0.4 3.19 39.2 640
Table 8 The performance test results
Sequence number Conductivity S/cm Intensity/MPa Rate of corrosion mA/cm 2 Maximum average transmission coefficient cm 3/ (s·cm 2) Density g/cm 2
Compression strength Bending strength
1 130.7 87 23 0.0052 3.1×10 -6 2.14
2 157.8 89 28 0.0049 2.9×10 -6 1.98
3 166.5 64 21 0.0057 3.4×10 -6 1.67
4 187.9 70 24 0.0055 3.1×10 -6 1.59
Table 8 The performance test results shows gained geopolymer base composite material double pole plate, low-cost and high-performance (cost of graphite is low, and carbon fiber improves performance, and the metakaolin cost is low).
Embodiment 2:
A kind of preparation method of geopolymer base composite material double pole plate, it comprises the steps:
1) chooses 12 groups of raw materials (sequence number 1-12, corresponding make 12 bipolar plates) by table 9.Described metakaolin is Coaseries kaolin or the washed kaolin that sell the market, calcines gained under 600～850 ℃ high temperature.Purity 〉=the 99.85wt% of described graphite, fineness＜90 μ m.The length of described carbon fiber is less than 4mm, diameter＜0.2mm.
2) metakaolin and conducting material are fully stirred with JJ-5 type cement plaster blender, mix, get powder; Water glass solution is joined in the powder that mixes, fully stir again and obtain slurry;
3) slurry is after JJ-5 type cement plaster blender fully stirs, injection has the metal die (the bipolar plates moulding is implemented by existing method) of reverse gas flow, hot pressing 15min under 120～180 ℃ of conditions, the demoulding, be placed on 20 ± 2 ℃ after the demoulding, maintenance 14d obtains the bipolar plates biscuit under the condition of relative humidity 95 ± 5%, and the biscuit quality that obtains is hard, smooth surface is smooth, flawless;
4) because alkali-activator (being water glass solution) can not complete reaction fall when geopolymer (being metakaolin) forms, a small amount of unnecessary waterglass will decompose Na in fuel cell +, SiO 3 2-The plasma stripping, thus the power output of fuel cell influenced; In order to address this problem, the bipolar plates biscuit is placed in the weak acid solution (pH=5～6 are as sulfuric acid solution) of circulation and soaks 10～12h, pass through water purification circulation rinsing then after, be dried into the geopolymer base composite material double pole plate.
Table 9
Sequence number Metakaolin/g Electric conducting material/g Liquid-solid ratio The water glass solution parameter
Graphite Carbon fiber Modulus/m Baume degrees/Be Volume/g
1 1000 100 100 0.6 3.19 39.2 720
2 1000 100 200 0.6 3.19 39.2 780
3 1000 200 100 0.6 3.19 39.2 780
4 1000 200 200 0.6 3.19 39.2 840
5 1000 400 100 0.6 3.19 39.2 900
6 1000 400 200 0.6 3.19 39.2 960
7 1000 100 100 0.8 3.19 39.2 960
8 1000 100 200 0.8 3.19 39.2 1040
9 1000 200 100 0.8 3.19 39.2 1040
10 1000 200 200 0.8 3.19 39.2 1120
11 1000 400 100 0.8 3.19 39.2 1200
12 1000 400 200 0.8 3.19 39.2 1280
Embodiment 3:
A kind of preparation method of geopolymer base composite material double pole plate, it comprises the steps:
1) be 20% of metakaolin quality according to the graphite volume, carbon fiber content is 10% of a metakaolin quality; The mass ratio of water glass solution and metakaolin and conducting material is to choose metakaolin, graphite, carbon fiber and water glass solution raw material at 0.4: 1, and wherein conducting material is made up of graphite and carbon fiber; Described metakaolin is that the Coaseries kaolin that sell the market is calcined gained under 600 ℃ high temperature; The modulus m=2.8 of described water glass solution, Baume degrees Be=35; Purity 〉=the 99.85wt% of described graphite, fineness＜90 μ m; The length of described carbon fiber is less than 4mm, diameter＜0.2mm;
2) metakaolin and conducting material are fully stirred with JJ-5 type cement plaster blender, mix, get powder; Water glass solution is joined in the powder that mixes, fully stir again and obtain slurry;
3) slurry is after JJ-5 type cement plaster blender fully stirs, injection has the metal die of reverse gas flow, hot pressing 15min under 120 ℃ of conditions, the demoulding, be placed on 18 ℃ after the demoulding, maintenance 14d obtains the bipolar plates biscuit under the condition of relative humidity 90%, and the biscuit quality that obtains is hard, smooth surface is smooth, flawless;
4) the bipolar plates biscuit be placed on soak 10h in the weak acid solution (pH=5 is as sulfuric acid solution) of circulation, pass through water purification circulation rinsing then after, be dried into the geopolymer base composite material double pole plate.
Embodiment 4:
A kind of preparation method of geopolymer base composite material double pole plate, it comprises the steps:
1) be 40% of metakaolin quality according to the graphite volume, carbon fiber content is 20% of a metakaolin quality; The mass ratio of water glass solution and metakaolin and conducting material is to choose metakaolin, graphite, carbon fiber and water glass solution raw material at 0.8: 1, and wherein conducting material is made up of graphite and carbon fiber; Described metakaolin is that washed kaolin is calcined gained under 850 ℃ high temperature; The modulus m=3.5 of described water glass solution, Baume degrees Be=45; Purity 〉=the 99.85wt% of described graphite, fineness＜90 μ m; The length of described carbon fiber is less than 4mm, diameter＜0.2mm;
2) metakaolin and conducting material are fully stirred with JJ-5 type cement plaster blender, mix, get powder; Water glass solution is joined in the powder that mixes, fully stir again and obtain slurry;
3) slurry is after JJ-5 type cement plaster blender fully stirs, injection has the metal die of reverse gas flow, hot pressing 15min under 180 ℃ of conditions, the demoulding, be placed on 22 ℃ after the demoulding, maintenance 14d under the condition of relative humidity 100% (my god) obtaining the bipolar plates biscuit, the biscuit quality that obtains is hard, smooth surface is smooth, flawless;
4) the bipolar plates biscuit be placed on soak 12h in the weak acid solution (pH=6 is as sulfuric acid solution) of circulation, pass through water purification circulation rinsing then after, be dried into the geopolymer base composite material double pole plate.

Claims (5)

1. a geopolymer base composite material double pole plate is characterized in that it is formed by metakaolin, conducting material and water glass solution feedstock production; Conducting material is made up of graphite and carbon fiber, and the graphite volume is 20～40% of a metakaolin quality, and carbon fiber content is 10%～20% of a metakaolin quality; The mass ratio of water glass solution and metakaolin and conducting material is 0.4～0.8: 1;
Described metakaolin is Coaseries kaolin or the washed kaolin that sell the market, calcines gained under 600～850 ℃ high temperature; Modulus m=2.8～3.5 of described water glass solution, Baume degrees Be=35～45.
2. a kind of geopolymer base composite material double pole plate according to claim 1 is characterized in that: the modulus m=3.19 of described water glass solution, Baume degrees Be=39.2.
3. a kind of geopolymer base composite material double pole plate according to claim 1 is characterized in that: the purity 〉=99.85wt% of described graphite, fineness＜90 μ m.
4. a kind of geopolymer base composite material double pole plate according to claim 1 is characterized in that: the length of described carbon fiber is less than 4mm, diameter＜0.2mm.
5. the preparation method of a kind of geopolymer base composite material double pole plate as claimed in claim 1 is characterized in that it comprises the steps:
1) be 20～40% of metakaolin quality according to the graphite volume, carbon fiber content is 10%～20% of a metakaolin quality, the mass ratio of water glass solution and metakaolin and conducting material is to choose metakaolin, graphite, carbon fiber and water glass solution raw material at 0.4～0.8: 1, and wherein conducting material is made up of graphite and carbon fiber; Described metakaolin is Coaseries kaolin or the washed kaolin that sell the market, calcines gained under 600～850 ℃ high temperature; Modulus m=2.8～3.5 of described water glass solution, Baume degrees Be=35～45;
2), get powder with metakaolin and conducting material mixing and stirring; Water glass solution is joined in the powder, fully stir again and obtain slurry;
3) slurry injects the metal die that has reverse gas flow, hot pressing 15～20min under 120～180 ℃ of conditions, and the demoulding is placed on 20 ± 2 ℃ after the demoulding, and maintenance 14d obtains the bipolar plates biscuit under the condition of relative humidity 95 ± 5%;
4) the bipolar plates biscuit is placed in the weak acid solution of circulation and soaks 10～12h, the pH=5 of weak acid solution～6, pass through water purification circulation rinsing then after, be dried into the geopolymer base composite material double pole plate.
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