CN112271303A - Fuel cell gas diffusion felt with uniformly distributed micropores and preparation method - Google Patents
Fuel cell gas diffusion felt with uniformly distributed micropores and preparation method Download PDFInfo
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Abstract
The invention relates to the field of fuel cells, and discloses a fuel cell gas diffusion felt with uniformly distributed micropores and a preparation method thereof. The preparation method comprises the following preparation processes: (1) heating and stirring a conductive carbon material, polyvinyl alcohol, glycerol and calcium salt to form paste; (2) carrying out hot melting and wire drawing on the paste to form a wire material; (3) cutting the wire into short fibers, and then flatly paving the short fibers with carbon fibers and carrying out hot pressing to prepare a fiber felt; (4) soaking the fiber felt into a sodium silicate solution, drawing, stretching and reacting to obtain a soaking reaction fiber felt; (5) and (3) eluting polyvinyl alcohol from the fiber felt subjected to the soaking reaction, drying and coiling to obtain the fuel cell gas diffusion felt with uniformly distributed micropores. The gas diffusion layer prepared by the invention generates calcium silicate fiber in situ as a support body of the conductive carbon material, has good toughness, good conductivity and air permeability, simple preparation process, easy large-scale continuous production, low energy consumption and low cost.
Description
Technical Field
The invention relates to the field of fuel cells, and discloses a fuel cell gas diffusion felt with uniformly distributed micropores and a preparation method thereof.
Background
A fuel cell is a chemical device that directly converts chemical energy of fuel into electrical energy, and is also called an electrochemical generator. It is a fourth power generation technology following hydroelectric power generation, thermal power generation and atomic power generation. The fuel cell converts the Gibbs free energy in the chemical energy of the fuel into electric energy through electrochemical reaction, and is not limited by the Carnot cycle effect, so the efficiency is high; in addition, fuel cells use fuel and oxygen as raw materials; meanwhile, no mechanical transmission part is arranged, so that no noise pollution is caused, and the discharged harmful gas is less. It follows that fuel cells are the most promising power generation technology from the viewpoint of energy conservation and ecological environment conservation.
The key technical core component of a fuel cell is the membrane electrode, which serves as the "core" of the fuel cell. The membrane electrode assembly is an assembly of a diffusion layer-catalyst layer-proton exchange membrane-catalyst layer and a diffusion layer structure, wherein the diffusion layer-catalyst layer-proton exchange membrane-catalyst layer and the diffusion layer structure are formed by respectively compounding a catalyst layer and a gas diffusion layer on two sides by taking a proton exchange membrane as an interlayer center. The fuel cell diffusion layer is a key component affecting the cell performance, and has the main functions of: supporting the catalyst and the membrane structure; uniformly distributing gas; support the whole structure and simultaneously require the diffusion layer to be a transmission channel of gas, electrons and water. Therefore, the diffusion layer is required to have the comprehensive characteristics of conductivity, air permeability, hydrophobicity and strength.
At present, carbon paper is mostly used for a diffusion layer of a fuel cell, and is prepared by compounding carbon fibers, polymer fibers and an adhesive, preparing the paper, and further carbonizing the paper at a high temperature of more than 1600 ℃ to obtain the carbon fiber paper. The carbon paper has excellent electrical conductivity and gas permeability for the gas diffusion layer due to complete carbonization. Such as carbon fiber paper produced by eastern Japan, SGL of Germany, Barrad of Canada, etc., has high performance. However, the existing carbon paper preparation technology has defects in the aspect of industrial preparation of carbon paper, the preforming of carbon fibers is difficult, the subsequent high-temperature carbonization energy consumption is high, and the prepared carbon fiber paper is brittle and not folding-resistant and is difficult to produce in large scale in batches. In particular, when used for a gas diffusion layer, the carbon paper is likely to be damaged due to the adhesion. How to ensure good conductivity and air permeability of the carbon paper and good flexibility is the problem which needs to be solved in the large-scale application of the carbon paper in the fuel cell at present.
In the prior art, the conductive carbon material and the polymer are dispersed, and the carbon paper is prepared by hot calendering, so that the method has the characteristics of simple process and easiness in batch production, and the obtained carbon paper is folding-resistant and good in flexibility. However, in actual preparation, the carbon paper prepared by the process contains a certain amount of polymers, so that the carbon paper is easy to coat carbon materials to influence the conductivity, and the difficulty in forming micropores to influence the air permeability, thereby restricting the development and application of the polymer-based gas diffusion layer.
Chinese patent application No. 200810115729.8 discloses a preparation method of carbon fiber paper for a gas diffusion layer of a fuel cell, belonging to the field of fuel cells. The carbon fiber mat phenolic resin prepreg is obtained by impregnating a carbon fiber mat into an ethanol solution of phenolic resin; performing low-temperature carbonization treatment on the prepreg after the prepreg is molded to prepare a carbon fiber paper blank; soaking the mixture in ethanol solution of phenolic resin again and curing; and finally, carrying out high-temperature carbonization treatment to obtain the carbon fiber paper for the gas diffusion layer of the fuel cell.
The Chinese patent application No. 201310504496.1 discloses a high-performance carbon paper special for a fuel cell gas diffusion layer and a preparation method thereof, wherein the carbon paper is prepared by taking chopped carbon fibers, plant fibers, thermal bonding fibers and carbon black as raw materials, defibering, pulping, preparing pulp, then papermaking by a wet papermaking process, and then coating by waterproof paint, wherein the mixture ratio of the raw materials is as follows in parts by weight: 65-75 parts of short carbon fiber, 10-15 parts of plant fiber, 10-15 parts of thermal bonding fiber and 0-10 parts of carbon black.
According to the above, the completely carbonized carbon fiber paper used for the gas diffusion layer of the membrane electrode of the fuel cell in the prior art is easy to be brittle and easy to break or even break when in use, and the carbon fiber paper for the fuel cell prepared by calendering the conductive carbon material and the polymer has the defects of poor conductivity and poor air permeability although the toughness is good.
Disclosure of Invention
The invention provides a fuel cell gas diffusion felt with uniformly distributed micropores and a preparation method thereof, which can effectively solve the technical problems.
In order to solve the problems, the invention adopts the following technical scheme:
a preparation method of a fuel cell gas diffusion felt with uniformly distributed micropores comprises the following specific steps:
(1) mixing conductive carbon material with polyvinyl alcohol, glycerol and calcium salt, heating and stirring until a homogeneous viscous paste is formed;
(2) feeding the paste prepared in the step (1) into a screw extruder, carrying out hot melt extrusion and wire drawing to form a wire with the diameter of 0.05-0.1 mm;
(3) cutting the wire material obtained in the step (2) into short fibers with the length of 3-5 mm, uniformly dispersing the cut short fibers and carbon fibers with the diameter of 7-16 mu m and the length of 2-6 mm, continuously spreading dry powder, and performing hot pressing through a compression molding roller to interweave the short fibers and the carbon fibers to form a fibrofelt with the thickness of less than 0.3-0.4 mm;
(4) immersing the fibrofelt obtained in the step (3) into a sodium silicate solution with the mass concentration of 30-40%, controlling the temperature for conveying, stretching by using a traction roller to loosen the fibrofelt, reacting to generate calcium silicate fibers, and carrying out in-situ network bonding on the calcium silicate fibers to obtain a fibrofelt subjected to soaking reaction;
(5) and (3) firstly, feeding the fibrofelt obtained in the step (4) after the soaking reaction into clear water, eluting polyvinyl alcohol, then introducing the fibrofelt into a drying tunnel with a step temperature through a traction roller, drying and then coiling to obtain the fuel cell gas diffusion felt with the thickness of 0.1-0.2 mm and uniformly distributed micropores.
In the scheme of the invention, the conductive carbon material is a conventional high-conductivity carbon-based material, and the calcium salt is a water-soluble calcium salt. Preferably, the conductive carbon material in the step (1) is at least one of carbon fiber, carbon nanotube, mesoporous carbon, carbon black, carbon aerogel, graphite and graphene; the calcium salt is calcium chloride.
Preferably, the heating and stirring temperature in the step (1) is 90-100 ℃, the rotating speed is 150-200 r/min, and the time is 2-3 h.
The melting point temperature of the polyvinyl alcohol is very close to the decomposition temperature, so that the traditional melt forming process cannot be used, and the melting point of the polyvinyl alcohol can be effectively reduced to be lower than the decomposition temperature by using the glycerol, so that the polyvinyl alcohol has better thermal stability and better spinnability at 230-250 ℃. As a preferred embodiment of the present invention, in the step (1): 15-20 parts of conductive carbon material, 39-51 parts of polyvinyl alcohol, 14-18 parts of glycerol and 20-23 parts of calcium salt.
Furthermore, while the hot-melt extrusion temperature is ensured, the wire drawing linear velocity must be kept continuously and stably, fiber breakage is easily caused when the speed is too high, and the diameter of the obtained fiber cannot be controlled when the speed is too low. As a preferable scheme of the invention, the temperature of the hot-melt extrusion in the step (2) is 230-250 ℃.
Carbon fiber is a high-conductivity material with excellent comprehensive performance, and has the characteristics of corrosion resistance, wear resistance, high temperature resistance, high strength, light weight and the like besides high conductivity, so that the carbon fiber is a preferred material for preparing the gas diffusion layer. Furthermore, the short fibers and the carbon fibers are used as raw materials, the fiber felt is prepared by a hot rolling process, the short fibers containing the polymer and the carbon fibers can generate thermal bonding at a certain temperature, and the formed thermal bonding is point bonding instead of area bonding, so that the obtained product has the characteristics of good flexibility and air permeability. Preferably, the dispersion ratio of the short fibers and the carbon fibers in the step (3) is: 50-60 parts of short fibers and 40-50 parts of carbon fibers; the hot pressing temperature is 120-135 ℃, the pressure is 1-3 MPa, and the pressure maintaining time is 15-25 s.
Preferably, in the step (4), the soaking temperature is 80-90 ℃, the stretching ratio is 1.5-2, and the soaking reaction time is 40-60 min.
The sectional drying process can avoid the defects of long drying time and low production efficiency caused by the fact that materials are in a static state and the static state drying depends on conduction or radiation heat transfer, and in addition, if the products are directly dried at a high temperature, due to the fact that the products are directly contacted with the high temperature in a high-moisture state, due to sudden temperature increase and rapid dehydration, due physicochemical indexes of the products are changed, and due beneficial properties are lost or reduced, so that the sectional drying process is selected. As a preferable scheme of the invention, the step temperature of the drying tunnel in the step (5) is divided into three sections, the temperature of the first section is 120-150 ℃, the temperature of the second section is 160-180 ℃, the temperature of the third section is 200-250 ℃, and the total drying time is 15-20 min.
The conductive carbon material and the calcium salt are dispersed in polyvinyl alcohol to prepare short fibers, and the short fibers and the carbon fibers are spread and hot-pressed to prepare a fiber felt; the fiber felt is loosened by soaking sodium silicate during later treatment and stretching through a traction roller while conveying, the loosened fiber felt not only has pores with excellent distribution, but also calcium ions in calcium salt and sodium silicate can generate calcium silicate fibers in the pores and the calcium silicate fibers are bonded to carbon fibers in an in-situ network manner, the calcium silicate fibers are used as a support body of the conductive carbon material, the fiber characteristics and network gaps of the conductive carbon material are better kept, and the calcium silicate fibers and the carbon fibers form a gas diffusion layer with excellent conductivity and uniform network air permeability. In addition, the toughness of the gas diffusion layer is greatly improved by replacing the in-situ calcium silicate fibers and utilizing the performance of the calcium silicate, and the defect that the conductivity and the air permeability are influenced by using a polymer is avoided.
The fuel cell gas diffusion felt with uniformly distributed micropores prepared by the method not only has good toughness, folding resistance and good flexibility, but also has conductivity and air permeability similar to those of the existing carbon fiber paper.
The invention provides a fuel cell gas diffusion felt with uniformly distributed micropores, which is characterized in that a conductive carbon material, polyvinyl alcohol, glycerol and calcium salt are heated and stirred until a homogeneous viscous paste is formed; feeding the paste into a screw extruder for hot melt extrusion and wire drawing to form a wire material; cutting the silk material into short fibers, uniformly dispersing the cut short fibers and carbon fibers, continuously spreading dry powder, hot-pressing by a mould pressing roller, and interweaving the short fibers and the carbon fibers to form a fiber felt; immersing the fiber felt into a sodium silicate solution, controlling the temperature, conveying and stretching the fiber felt by a traction roller to loosen the fiber felt, generating calcium silicate fibers by calcium ions in calcium salt and sodium silicate, and carrying out in-situ network bonding on the carbon fibers; and (3) feeding the fibrofelt subjected to the soaking reaction into clear water to elute polyvinyl alcohol, introducing the fibrofelt into a drying tunnel with a step temperature through a traction roller, drying the tunnel, and coiling after drying.
Compared with the prior art, the invention provides the fuel cell gas diffusion felt with uniformly distributed micropores and the preparation method thereof, and the outstanding characteristics and excellent effects are as follows:
1. provides a method for preparing a fuel cell gas diffusion felt with uniformly distributed micropores by utilizing the co-hot pressing of the generated calcium silicate fibers and carbon fibers.
2. Calcium silicate fibers are generated in situ as a support of the conductive carbon material, so that the gas diffusion layer has good toughness and excellent electrical conductivity and air permeability together with the carbon fibers.
3. The preparation method has the advantages of simple preparation process, easy large-scale continuous production, low energy consumption and low cost.
Drawings
FIG. 1: high-light electron microscopy of the fuel cell gas diffusion felt obtained in example 1.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Mixing conductive carbon material with polyvinyl alcohol, glycerol and calcium salt, heating and stirring until a homogeneous viscous paste is formed;
the conductive carbon material is carbon fiber; the calcium salt is calcium chloride; the heating and stirring temperature is 96 ℃, the rotating speed is 170r/min, and the time is 2.5 h; wherein: 17 parts of conductive carbon material, 46 parts of polyvinyl alcohol, 15 parts of glycerol and 22 parts of calcium salt;
(2) feeding the paste prepared in the step (1) into a screw extruder, carrying out hot melt extrusion and wire drawing to form a wire with the average diameter of 0.07 mm;
the temperature of hot melt extrusion is 238 ℃;
(3) cutting the wire material obtained in the step (2) into short fibers with the average length of 4mm, uniformly dispersing the cut short fibers and carbon fibers with the average diameter of 11 mu m and the average length of 5mm, continuously spreading dry powder, and hot-pressing through a compression molding roller to interweave the short fibers and the carbon fibers to form a fiber felt with the average thickness of 0.32 mm;
wherein: 56 parts of short fibers and 44 parts of carbon fibers; the hot pressing temperature is 128 ℃, the pressure is 1.8MPa, and the pressure maintaining time is 21 s;
(4) immersing the fiber felt obtained in the step (3) into a sodium silicate solution with the mass concentration of 36%, controlling the temperature for conveying, simultaneously stretching by using a traction roller to loosen the fiber felt, simultaneously reacting to generate calcium silicate fibers and bonding the carbon fibers in an in-situ network manner to obtain a fiber felt subjected to soaking reaction;
in the soaking reaction system, the temperature is 86 ℃, the stretching ratio is 1.7, and the soaking reaction time is 49 min;
(5) firstly, feeding the fibrofelt obtained in the step (4) after the soaking reaction into clear water, eluting polyvinyl alcohol, then introducing the fibrofelt into a drying tunnel with a step temperature through a traction roller, drying and then coiling to obtain a fuel cell gas diffusion felt with uniformly distributed micropores and an average thickness of 0.14 mm;
the step temperature of the drying tunnel is divided into three sections, the temperature of the first section is 130 ℃, the temperature of the second section is 178 ℃, the temperature of the third section is 230 ℃, and the total drying time is 17 min.
The obtained gas diffusion felt of the fuel cell is observed by a high-light electron microscope, and micropores of the diffusion felt are uniformly dispersed, as shown in figure 1.
Example 2
(1) Mixing conductive carbon material with polyvinyl alcohol, glycerol and calcium salt, heating and stirring until a homogeneous viscous paste is formed;
the conductive carbon material is a carbon nanotube; the calcium salt is calcium chloride; the heating and stirring temperature is 92 ℃, the rotating speed is 160r/min, and the time is 3 h; wherein: 16 parts of conductive carbon material, 48 parts of polyvinyl alcohol, 15 parts of glycerol and 21 parts of calcium salt;
(2) feeding the paste prepared in the step (1) into a screw extruder, carrying out hot melt extrusion and wire drawing to form a wire with the average diameter of 0.06 mm;
the temperature of hot melt extrusion is 235 ℃;
(3) cutting the wire material obtained in the step (2) into short fibers with the average length of 3.5mm, uniformly dispersing the cut short fibers and carbon fibers with the average diameter of 9 mu m and the average length of 3mm, continuously spreading dry powder, and carrying out hot pressing through a compression molding roller to interweave the short fibers and the carbon fibers to form a fibrofelt with the average thickness of 0.33 mm;
wherein: 52 parts of short fibers and 48 parts of carbon fibers; the hot pressing temperature is 125 ℃, the pressure is 1.5MPa, and the pressure maintaining time is 23 s;
(4) immersing the fiber felt obtained in the step (3) into a sodium silicate solution with the mass concentration of 32%, controlling the temperature for conveying, simultaneously stretching by using a traction roller to loosen the fiber felt, simultaneously reacting to generate calcium silicate fibers and bonding the carbon fibers in an in-situ network manner to obtain a fiber felt subjected to soaking reaction;
in a soaking reaction system, the temperature is 82 ℃, the stretching ratio is 1.6, and the soaking reaction time is 55 min;
(5) firstly, feeding the fibrofelt obtained in the step (4) after the soaking reaction into clear water, eluting polyvinyl alcohol, then introducing the fibrofelt into a drying tunnel with a step temperature through a traction roller, drying and then coiling to obtain a fuel cell gas diffusion felt with uniformly distributed micropores and an average thickness of 0.12 mm;
the step temperature of the drying tunnel is divided into three sections, the temperature of the first section is 125 ℃, the temperature of the second section is 165 ℃, the temperature of the third section is 220 ℃, and the total drying time is 19 min.
Example 3
(1) Mixing conductive carbon material with polyvinyl alcohol, glycerol and calcium salt, heating and stirring until a homogeneous viscous paste is formed;
the conductive carbon material is mesoporous carbon; the calcium salt is calcium chloride; the heating and stirring temperature is 90 ℃, the rotating speed is 190r/min, and the time is 3 h; wherein: 15 parts of conductive carbon material, 51 parts of polyvinyl alcohol, 14 parts of glycerol and 20 parts of calcium salt;
(2) feeding the paste prepared in the step (1) into a screw extruder, carrying out hot melt extrusion and wire drawing to form a wire with the average diameter of 0.05 mm;
the temperature of hot melt extrusion is 230 ℃;
(3) cutting the wire material obtained in the step (2) into short fibers with the average length of 3mm, uniformly dispersing the cut short fibers and carbon fibers with the average diameter of 7 mu m and the average length of 2mm, continuously spreading dry powder, and hot-pressing through a compression molding roller to interweave the short fibers and the carbon fibers to form a fiber felt with the average thickness of 0.3 mm;
wherein: 50 parts by weight of short fibers and 40-50 parts by weight of short fibers; the hot pressing temperature is 120 ℃, the pressure is 1MPa, and the pressure maintaining time is 25 s;
(4) immersing the fiber felt obtained in the step (3) into a sodium silicate solution with the mass concentration of 30%, controlling the temperature for conveying, simultaneously stretching by using a traction roller to loosen the fiber felt, simultaneously reacting to generate calcium silicate fibers and bonding the carbon fibers in an in-situ network manner to obtain a fiber felt subjected to soaking reaction;
soaking the mixture in a soaking reaction system at 80 deg.C for 60min, wherein the stretching ratio is 1.5;
(5) firstly, feeding the fibrofelt obtained in the step (4) after the soaking reaction into clear water, eluting polyvinyl alcohol, then introducing the fibrofelt into a drying tunnel with a step temperature through a traction roller, drying and then coiling to obtain a fuel cell gas diffusion felt with uniformly distributed micropores and an average thickness of 0.1 mm;
the step temperature of the drying tunnel is divided into three sections, the temperature of the first section is 120 ℃, the temperature of the second section is 160 ℃, the temperature of the third section is 200 ℃, and the total drying time is 20 min.
Example 4
(1) Mixing conductive carbon material with polyvinyl alcohol, glycerol and calcium salt, heating and stirring until a homogeneous viscous paste is formed;
the conductive carbon material is carbon black; the calcium salt is calcium hypochlorite; the heating and stirring temperature is 98 ℃, the rotating speed is 150r/min, and the time is 2 h; wherein: 18 parts of conductive carbon material, 43 parts of polyvinyl alcohol, 17 parts of glycerol and 22 parts of calcium salt;
(2) feeding the paste prepared in the step (1) into a screw extruder, carrying out hot melt extrusion and wire drawing to form a wire with the average diameter of 0.09 mm;
the temperature of hot melt extrusion is 245 ℃;
(3) cutting the wire material obtained in the step (2) into short fibers with the average length of 4.5mm, uniformly dispersing the cut short fibers and carbon fibers with the average diameter of 13 mu m and the average length of 5mm, continuously spreading dry powder, and carrying out hot pressing through a compression molding roller to interweave the short fibers and the carbon fibers to form a fiber felt with the average thickness of 0.38 mm;
wherein: 58 parts of short fibers and 42 parts of carbon fibers; the hot pressing temperature is 130 ℃, the pressure is 2.5MPa, and the pressure maintaining time is 18 s;
(4) immersing the fiber felt obtained in the step (3) into a sodium silicate solution with the mass concentration of 38%, controlling the temperature for conveying, simultaneously stretching by using a traction roller to loosen the fiber felt, simultaneously reacting to generate calcium silicate fibers and bonding the carbon fibers in an in-situ network manner to obtain a fiber felt subjected to soaking reaction;
soaking in a reaction system at 88 deg.C for 45min, wherein the stretching ratio is 1.8;
(5) firstly, feeding the fibrofelt obtained in the step (4) after the soaking reaction into clear water, eluting polyvinyl alcohol, then introducing the fibrofelt into a drying tunnel with a step temperature through a traction roller, drying and then coiling to obtain a fuel cell gas diffusion felt with uniformly distributed micropores and an average thickness of 0.17 mm;
the step temperature of the drying tunnel is divided into three sections, the temperature of the first section is 140 ℃, the temperature of the second section is 175 ℃, the temperature of the third section is 240 ℃, and the total drying time is 16 min.
Example 5
(1) Mixing conductive carbon material with polyvinyl alcohol, glycerol and calcium salt, heating and stirring until a homogeneous viscous paste is formed;
the conductive carbon material is carbon aerogel; the calcium salt is calcium chloride; the heating and stirring temperature is 100 ℃, the rotating speed is 200r/min, and the time is 2 h; wherein: 20 parts of conductive carbon material, 39 parts of polyvinyl alcohol, 18 parts of glycerol and 23 parts of calcium salt;
(2) feeding the paste prepared in the step (1) into a screw extruder, carrying out hot melt extrusion and wire drawing to form a wire with the average diameter of 0.1 mm;
the temperature of hot melt extrusion is 250 ℃;
(3) cutting the wire material obtained in the step (2) into short fibers with the average length of 5mm, uniformly dispersing the cut short fibers and carbon fibers with the average diameter of 16 mu m and the average length of 6mm, continuously spreading dry powder, and hot-pressing through a compression molding roller to interweave the short fibers and the carbon fibers to form a fiber felt with the average thickness of 0.4 mm;
wherein: 60 parts of short fibers and 40 parts of carbon fibers; the hot pressing temperature is 135 ℃, the pressure is 3MPa, and the pressure maintaining time is 15 s;
(4) immersing the fiber felt obtained in the step (3) into a sodium silicate solution with the mass concentration of 40%, controlling the temperature for conveying, simultaneously stretching by using a traction roller to loosen the fiber felt, simultaneously reacting to generate calcium silicate fibers and bonding the carbon fibers in an in-situ network manner to obtain a fiber felt subjected to soaking reaction;
soaking the mixture in a soaking reaction system at 90 ℃ and a stretching ratio of 2 for 40 min;
(5) firstly, feeding the fibrofelt obtained in the step (4) after the soaking reaction into clear water, eluting polyvinyl alcohol, then introducing the fibrofelt into a drying tunnel with a step temperature through a traction roller, drying and then coiling to obtain a fuel cell gas diffusion felt with uniformly distributed micropores and an average thickness of 0.1-0.2 mm;
the step temperature of the drying tunnel is divided into three sections, the temperature of the first section is 150 ℃, the temperature of the second section is 180 ℃, the temperature of the third section is 250 ℃, and the total drying time is 15 min.
Example 6
(1) Mixing conductive carbon material with polyvinyl alcohol, glycerol and calcium salt, heating and stirring until a homogeneous viscous paste is formed;
the conductive carbon material is graphene; the calcium salt is calcium chloride; the heating and stirring temperature is 90-100 ℃, the rotating speed is 180r/min, and the time is 2-3 h; wherein: 18 parts of conductive carbon material, 44 parts of polyvinyl alcohol, 16 parts of glycerol and 22 parts of calcium salt;
(2) feeding the paste prepared in the step (1) into a screw extruder, carrying out hot melt extrusion and wire drawing to form a wire with the average diameter of 0.08 mm;
the temperature of hot melt extrusion is 240 ℃;
(3) cutting the wire material obtained in the step (2) into short fibers with the average length of 4mm, uniformly dispersing the cut short fibers and carbon fibers with the average diameter of 12 mu m and the average length of 4mm, continuously spreading dry powder, and hot-pressing through a compression molding roller to interweave the short fibers and the carbon fibers to form a fiber felt with the average thickness of 0.35 mm;
wherein: 55 parts of short fibers and 45 parts of carbon fibers; the hot pressing temperature is 130 ℃, the pressure is 2MPa, and the pressure maintaining time is 20 s;
(4) immersing the fiber felt obtained in the step (3) into a sodium silicate solution with the mass concentration of 35%, controlling the temperature for conveying, simultaneously stretching by using a traction roller to loosen the fiber felt, simultaneously reacting to generate calcium silicate fibers and bonding the carbon fibers in an in-situ network manner to obtain a fiber felt subjected to soaking reaction;
soaking the mixture in a soaking reaction system at 85 deg.C for 50min, wherein the stretching ratio is 1.8;
(5) firstly, feeding the fibrofelt obtained in the step (4) after the soaking reaction into clear water, eluting polyvinyl alcohol, then introducing the fibrofelt into a drying tunnel with a step temperature through a traction roller, drying and then coiling to obtain a fuel cell gas diffusion felt with uniformly distributed micropores and an average thickness of 0.15 mm;
the step temperature of the drying tunnel is divided into three sections, the temperature of the first section is 135 ℃, the temperature of the second section is 170 ℃, the temperature of the third section is 225 ℃, and the total drying time is 18 min.
Comparative example 1
Comparative example 1 a gas diffusion layer was prepared without treating the fiber mat by dipping it in a sodium silicate solution, i.e., without forming a calcium silicate fiber binder, which affects the formation of micropores, under the same other conditions as in example 6. Since calcium silicate-bonded carbon fibers are not formed, polyvinyl alcohol is eluted at the time of later washing, which affects the adhesiveness of the diffusion layer mat and has no use value.
Comparative example 2
A commercially available carbon paper having model number CDS090, carbon energy corporation, taiwan, china.
Basic performance tests were performed on the porosity and resistivity of the gas diffusion layers of examples 1 to 6 and comparative example 2:
porosity: testing by a mercury pressure method;
resistivity: rapidly detecting by adopting a four-probe method;
air permeability: referring to GB/T5453 method for measuring textile fabric air permeability, 20cm is selected2The test head of (1); a pressure difference of 100Pa was tested.
Folding resistance: flexibility is measured as the number of bends at 75 °.
The test data are shown in table 1.
Table 1:
at present, carbon paper is mainly adopted as a gas diffusion layer of a fuel cell in the conventional way, and the preparation process of the carbon paper mainly comprises the steps of compounding carbon fibers, polymer fibers and an adhesive, preparing the paper, and carbonizing the paper at 1600 ℃ to obtain carbon fiber paper; the preparation process is complex, and the obtained carbon paper is brittle. The invention is realized by in-situ generation and bonding of inorganic calcium silicate fibers. The carbon fibers are directly bonded into a felt shape, through testing, the obtained fuel cell gas diffusion felt keeps good gaps and air permeability, and micropores of the diffusion felt are uniformly dispersed through observation of a high-gloss electron microscope. Furthermore, the calcium silicate fiber formed in situ is bonded, and the crops are bonded in an inorganic mode, so that the obtained gas diffusion layer felt is stable and does not deform in hot and water environments, is impact-resistant, has certain flexibility, and has low surface resistivity similar to that of carbon fiber paper. Opens up a large-scale stable preparation technical approach for preparing the gas diffusion layer of the fuel cell.
Claims (10)
1. A preparation method of a fuel cell gas diffusion felt with uniformly distributed micropores is characterized by comprising the following specific preparation processes:
(1) mixing conductive carbon material with polyvinyl alcohol, glycerol and calcium salt, heating and stirring until a homogeneous viscous paste is formed;
(2) feeding the paste prepared in the step (1) into a screw extruder, carrying out hot melt extrusion and wire drawing to form a wire with the diameter of 0.05-0.1 mm;
(3) cutting the wire material obtained in the step (2) into short fibers with the length of 3-5 mm, uniformly dispersing the cut short fibers and carbon fibers with the diameter of 7-16 mu m and the length of 2-6 mm, continuously spreading dry powder, and performing hot pressing through a compression molding roller to interweave the short fibers and the carbon fibers to form a fibrofelt with the thickness of less than 0.3-0.4 mm;
(4) immersing the fibrofelt obtained in the step (3) into a sodium silicate solution with the mass concentration of 30-40%, controlling the temperature for conveying, stretching by using a traction roller to loosen the fibrofelt, reacting to generate calcium silicate fibers, and carrying out in-situ network bonding on the calcium silicate fibers to obtain a fibrofelt subjected to soaking reaction;
(5) and (3) firstly, feeding the fibrofelt obtained in the step (4) after the soaking reaction into clear water, eluting polyvinyl alcohol, then introducing the fibrofelt into a drying tunnel with a step temperature through a traction roller, drying and then coiling to obtain the fuel cell gas diffusion felt with the thickness of 0.1-0.2 mm and uniformly distributed micropores.
2. The method of claim 1 for preparing a fuel cell gas diffusion felt with uniformly distributed pores, wherein the method comprises the following steps: the conductive carbon material in the step (1) is at least one of carbon fiber, carbon nano tube, mesoporous carbon, carbon black, carbon aerogel, graphite and graphene, and the calcium salt is calcium chloride.
3. The method of claim 1 for preparing a fuel cell gas diffusion felt with uniformly distributed pores, wherein the method comprises the following steps: the heating and stirring temperature in the step (1) is 90-100 ℃, the rotating speed is 150-200 r/min, and the time is 2-3 h.
4. The method of claim 1 for preparing a fuel cell gas diffusion felt with uniformly distributed pores, wherein the method comprises the following steps: in the step (1): 15-20 parts of conductive carbon material, 39-51 parts of polyvinyl alcohol, 14-18 parts of glycerol and 20-23 parts of calcium salt.
5. The method of claim 1 for preparing a fuel cell gas diffusion felt with uniformly distributed pores, wherein the method comprises the following steps: the temperature of the hot-melt extrusion in the step (2) is 230-250 ℃.
6. The method of claim 1 for preparing a fuel cell gas diffusion felt with uniformly distributed pores, wherein the method comprises the following steps: in the step (3), the dispersion ratio of the short fibers and the carbon fibers is as follows: 50-60 parts of short fibers and 40-50 parts of carbon fibers.
7. The method of claim 1 for preparing a fuel cell gas diffusion felt with uniformly distributed pores, wherein the method comprises the following steps: and (3) carrying out hot pressing at the temperature of 120-135 ℃, under the pressure of 1-3 MPa, and keeping the pressure for 15-25 s.
8. The method of claim 1 for preparing a fuel cell gas diffusion felt with uniformly distributed pores, wherein the method comprises the following steps: and (4) the conveying temperature is 80-90 ℃, the stretching ratio is 1.5-2, and the soaking reaction time is 40-60 min.
9. The method of claim 1 for preparing a fuel cell gas diffusion felt with uniformly distributed pores, wherein the method comprises the following steps: and (5) dividing the step temperature of the drying tunnel into three sections, wherein the temperature of the first section is 120-150 ℃, the temperature of the second section is 160-180 ℃, the temperature of the third section is 200-250 ℃, and the total drying time is 15-20 min.
10. A fuel cell gas diffusion felt with uniformly distributed micropores, prepared by the method of any one of claims 1 to 9.
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