CN102146641B - Process for manufacturing modified carbon fiber paper by adopting carbon nanotube implanting method - Google Patents
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Abstract
The invention discloses a process for manufacturing modified carbon fiber paper by adopting a carbon nanotube implanting method. The process comprises the following steps of: dispersing a prepared or commercial carbon nanotube, uniformly coating the dispersed carbon nanotube on the surface of carbon paper prepared with the conventional method by taking a phenolic resin solution as an adhesive, bonding the carbon nanotube on the carbon paper because the carbon nanotube with a 'pinning function' and carbonizing; and tightly fixing the carbon nanotube on the surface of the carbon paper by using deposited pyrolytic carbon with a chemical gas phase deposition method. By adopting the process, carbon nanotubes can be implanted into the surface of the carbon paper in a large area on a large scale, the adhesion of the carbon nanotubes on the surface of the carbon paper can be remarkably increased, the carbon nanotubes are prevented from being stripped easily and other unfavorable factors are avoided; and the method has low cost and is easy to operate.
Description
Technical field
The present invention relates to a kind of manufacturing technique of CNT (carbon nano-tube) implantation Modified Activated Carbon fibrous paper.
Background technology
The multiple advantageous premium properties of charcoal fibrous paper (abbreviation carbon paper) tool: low-density, high specific strength, high ratio modulus, good biocompatibility, high temperature resistant, corrosion-resistant, electrical and thermal conductivity and electromagnetic wave shielding etc.Therefore, the research of charcoal fiber conductive paper and composite thereof has caused domestic concern widely with application, at present military and civilian is industrial has also obtained a lot of gratifying achievements, especially as the critical component of Proton Exchange Membrane Fuel Cells diffusion layer, has become the focus of research and development.Carbon paper is as a kind of special functional paper, and its preparation method also technique with traditional papermaking is the same, roughly can be divided into two kinds of dry method and wet methods, the wet processing that current research is maximum.At present, the preparation carbon paper mainly contains following certain methods:
(1) can mix with chopped carbon fiber as the solution of polyvinyl alcohol (PVA) of binding agent and so on, utilize paper technology moulding on paper machine, make staple fibre adhered to one another after drying, but then flood with the weak solution of the charing materials such as phenolic resins, obtain the base paper material of charcoal bonded carbon fibre through overcuring, charring process.
(2) decentralized medium is mixed with the staple fibre with self-adhesive and energy charing, after papermaking, but the staple fibre with charing bonds chopped carbon fiber mutually, but then make the charing of charing staple fibre in the inert atmosphere of high temperature more than 1000 ℃, can make thus the porosity 60%～90%, the carbon fiber porous material of resistivity about 0.1 Ω cm.
(3) use chopped carbon fiber and be raw material as the paper pulp of binding agent, copy the paper moulding by paper technology, wherein oxidized in the paper pulp Water repellent treatment process afterwards as binding agent and gasification and removing stays simultaneously the effect that uniformly a large amount of holes have played pore creating material on carbon paper.This processing method is conducive to reduce the manufacturing cost of carbon paper, and can add the amount of paper pulp to control the size of air penetrability by control.
Have the combination properties such as good electric conductivity, mechanical property, water management properties due to CNT, in recent years, many research all wishes CNT is used for the electrode of fuel cell, but up to the present, become the focus of this area research at the study on the modification of electrode surface carbon nano-tube.Propose metallic catalyst is dispersed on the charcoal substrate as Japan Patent P2004-59428A, pass into carbon-source gas, at 400-900 ℃ of lower CVD method synthesizing carbon nanotubes, using plasma chemical gaseous phase depositing process synthesizing carbon nanotubes is arranged also.The method that adopts sputter, vaporization, CVD, plating or electroless coating is also arranged with iron, cobalt, nickel or loaded on charcoal cloth or charcoal fiber by the alloy that it consists of, then flow into the carbon source synthesizing carbon nanotubes.
The research of relevant CNT (carbon nano-tube) Modified Activated Carbon fibrous paper is mainly at charcoal fibrous paper surface direct growth CNT, its technological process roughly is: at first must carry out preliminary treatment to strengthen the wettability on carbon paper surface to carbon paper, then at the carbon paper surface impregnation or apply iron, cobalt, nickel or its mixture as catalyst, use again the way of chemical vapour deposition (CVD) directly at carbon paper superficial growth CNT, also want at last post processing to eliminate catalyst in order to avoid affect the application of charcoal fibrous paper.Owing to having introduced catalyst, distributing homogeneity and the adhesive force of CNT on the charcoal fibrous paper may be difficult to guarantee.And especially the required carbon paper size of automobile fuel battery is larger, may run into larger obstacle at carbon paper surface direct growth CNT.So not only technical difficulty is large for this way, complicated operation, program are many, and be difficult in enormous quantities and low-cost production, quality assurance difficult.
It can be seen from the above, although the multiple method for preparing carbon paper is arranged in existing technology, also have and attempt CNT is used for the carbon paper modification to improve the technology of its performance, but be all at the surperficial direct growth CNT of carbon paper, also directly do not utilize the commercialization CNT to implant carbon paper surperficial, then adopt the method for chemical vapour deposition (CVD) fixed carbon nanotube.
Summary of the invention
The combination property that technical problem to be solved by this invention is to provide a kind of fuel cell electrode is high, can guarantee the uniformity that CNT distributes, the fastness of implanting, the cheap property of cost can not brought the manufacturing technique of the modified carbon fiber paper by adopting carbon nanotube implanting of other impurity into simultaneously.
In order to solve the problems of the technologies described above, the manufacturing technique of modified carbon fiber paper by adopting carbon nanotube implanting provided by the invention, make the carbon paper base substrate with the charcoal fibrous paper, implant CNT on its surface, even carbon nanotube is disperseed, CNT is in carbon paper billet surface uniform load, CNT and carbon paper base substrate strong bonded, and its several stages are as follows:
A. the pretreatment stage of CNT
The salpeter solution that CNT is placed in 0.1～1.0mol carries out oxidation processes 4～10h, so with distilled water, CNT is cleaned repeatedly repeatedly, then, then puts it into dry 4～10h in baking oven;
B. the scatter stage of CNT
Add the CNT (carbon nano-tube) of 0.2～10g/L in the ethanol solution of 2～3g/L of neopelex, the concussion time is 1.5～2.5h;
C. the scatter stage of resin
It is 10～30% absolute ethyl alcohol system that phenolic resins is made into resin quality concentration, then the solution for preparing is put into the ultrasonic concussion 1.5～2.5h of supersonic wave cleaning machine;
D. the implantation stage of CNT
Phenolic resins evenly is coated on the surface of carbon paper base substrate, the mass ratio of phenolic resins and carbon paper base substrate is controlled at 6～8: 2～4; The carbon paper base substrate dries the dry 1.5～2.5h of processing in the baking oven of 65～75 ℃ afterwards; Then hot-press solidifying moulding on vulcanizer, condition of cure are 3～5MPa, 170～190 ℃, 1.5～2.5h; Then charing in retort, carbonization condition are first to vacuumize below 10Pa, are warming up to 850-1000 ℃, and inflated with nitrogen is naturally cooling to the atmospheric pressure charing 2-10h; Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 1.5～2.5h under 1800～2200 ℃; Or
Phenolic resins evenly is coated on the surface of carbon paper base substrate, the mass ratio of phenolic resins and carbon paper base substrate is controlled at 6～8: 2～4; The carbon paper base substrate dries the dry 1.5～2.5h of processing in the baking oven of 65～75 ℃ afterwards; Then hot-press solidifying moulding on vulcanizer, condition of cure is 3～5MPa, 170～190 ℃, 1.5～2.5h, the moulding carbon paper is placed in cvd furnace, first be evacuated under 10Pa, then be warming up to 800～1000 ℃ with the programming rate of 5-10 per minute ℃, insulation 1～2h, then pass into the mist of carbon-source gas and diluent gas, volume ratio both is 1: 1, reaction gas flow 0.1～5L/ minute; To atmospheric furnace pressure condition, carbon-source gas is implemented continous mode or discontinuous is supplied gas at 1kPa, vacuumizes nature after deposition 0.2～2h cooling; Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 1.5～2.5h under 1800～2200 ℃.
The coating of carbon paper surface carbon nanotube in above-mentioned steps D refers to first coated with resins bonding agent, the CNT that rear coating ethanol disperses; Or first apply the CNT that ethanol disperses, rear coated with resins bonding agent; Or first carbon nanotube dispersed in resin solution, after be coated on the carbon paper surface.
Described carbon-source gas is methane, propylene or oil liquefied gas, and described diluent gas is nitrogen or argon gas.
Adopt the manufacturing technique of the modified carbon fiber paper by adopting carbon nanotube implanting of technique scheme.By first disperseing prepare or business-like CNT, make bonding agent with phenol resin solution, scattered even carbon nanotube be coated in carbon paper surface with conventional method preparation, CNT will be bonded on carbon paper, can be surperficial perpendicular to the carbon paper that adheres to because have " pinning effect " CNT, then charing; Can also with the method for chemical vapour deposition (CVD), be securely fixed in CNT on the surface of carbon paper by the deposition pyrolytic carbon at last.This invention can be in large area, CNT is implanted on the carbon paper surface in mass ground, the method not only cost is low, and is simple to operate, and can increase significantly CNT at the adhesive force on carbon paper surface, make CNT incrust, and can not bring other disadvantageous element into.Thereby be conducive to improve the combination properties such as surface property, electric conductivity of carbon paper, strengthen carbon paper when assembling fuel cell to the grappling effect of other parts, provide feasible prospect for CNT catalyst-loaded research and practical application simultaneously.
Description of drawings
Shown in Figure 1 is the general flowchart of carbon nanotube dispersed in the present invention;
Shown in Figure 2 is the general flowchart of the preparation method of carbon nano-tube modification carbon paper in the present invention;
Fig. 3 is the SEM figure that adopts the modification carbon paper surface of the embodiment of the present invention 1.
Fig. 4 is the SEM figure that adopts the modification carbon paper surface of the embodiment of the present invention 2.
Fig. 5 is the SEM figure that adopts the modification carbon paper surface of the embodiment of the present invention 3.
The specific embodiment
The invention will be further described below in conjunction with accompanying drawing and several specific embodiment of the present invention.。
Embodiment 1: referring to Fig. 1 and Fig. 2,
A. the pretreatment stage of CNT
For CNT is further purified, remove the impurity such as catalyst of bringing in preparation process, improve simultaneously the dispersiveness of CNT, commercially available CNT is dipped in the aqueous solution of nitric acid of 0.2mol, with distilled water, CNT is cleaned repeatedly repeatedly after 10h, then put it into dry 10h in the baking oven of 100 ℃ then;
B. the scatter stage of CNT
1. take the 10g CNT (carbon nano-tube), add the absolute ethyl alcohol of 1000ml;
2. configure neopelex 3g/L (with the volume ratio of absolute ethyl alcohol), be placed in the ultrasonic concussion of supersonic wave cleaning machine, the concussion time is 1.5h;
C. the scatter stage of resin
It is 10% ethanol system that phenolic resins is made into resin quality concentration, then the solution for preparing is put into the ultrasonic concussion of supersonic wave cleaning machine 2h;
D. the implantation stage of CNT
Phenolic resins is added scattered carbon nano-tube solution of B stage, and resin quality concentration is controlled to be 10%, and then mechanical dispersion evenly is coated on the surface of carbon paper base substrate, and the mass ratio of phenolic resins and carbon paper base substrate is controlled at 7: 3; The carbon paper base substrate dries the dry 2h of processing in the baking oven of 70 ℃ afterwards; Then hot-press solidifying moulding on vulcanizer, condition of cure are 4MPa, 180 ℃, 2h; Then charing in retort, carbonization condition are first to vacuumize below 10Pa, are warming up to 1000 ℃, and inflated with nitrogen is naturally cooling to the atmospheric pressure charing 2h; Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 2h under 2000 ℃, and the SEM figure on modification carbon paper surface is referring to Fig. 3.
Embodiment 2: referring to Fig. 1 and Fig. 2,
The technological parameter in A, B, C stage is identical with example 1, and the D stage carries out by the following method:
Phenol resin solution is coated on hot-forming moulding carbon paper surface, controls resin demand, then carbon nano-tube coating solution; Dry the dry 2h of processing in the baking oven of 70 ℃ afterwards; Then charing in retort, carbonization condition are first to vacuumize below 10Pa, are warming up to 1000 ℃, and inflated with nitrogen is naturally cooling to the atmospheric pressure charing 2h; Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 2h under 2000 ℃, and the SEM figure on modification carbon paper surface is referring to Fig. 4.
Embodiment 3:
The technological parameter in A, B, C stage is identical with example 2, and the D stage, it is identical with example 2 that all the other steps all adopt except the moulding carbon paper not being carried out charing and graphitization processing, and the E stage carries out by the following method:
The moulding carbon paper that has applied CNT is placed in cvd furnace, first is evacuated under 10Pa, then be warming up to 1000 ℃ with the programming rate of 5 ℃ per minute, insulation 2h, pass into the mist of methane and nitrogen, volume ratio both is 1: 1 again, reaction gas flow 0.1L/ minute.To atmospheric furnace pressure condition, methane is implemented continous mode and is supplied gas at 1kPa.Vacuumize nature after deposition 0.2h cooling.Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 2h under 2000 ℃, and the SEM figure on modification carbon paper surface is referring to Fig. 5.
Embodiment 4:
A. the pretreatment stage of CNT
For CNT is further purified, remove the impurity such as catalyst of bringing in preparation process, improve simultaneously the dispersiveness of CNT, commercially available CNT is dipped in the aqueous solution of nitric acid of 0.1mol, with distilled water, CNT is cleaned repeatedly repeatedly after 4h, then put it into dry 4h in the baking oven of 100 ℃ then;
B. the scatter stage of CNT
1. take the 0.2g CNT (carbon nano-tube), add the absolute ethyl alcohol of 1000ml;
2. configure neopelex 2g/L (with the volume ratio of absolute ethyl alcohol), be placed in the ultrasonic concussion of supersonic wave cleaning machine, the concussion time is 1.5h;
C. the scatter stage of resin
It is 10% ethanol system that phenolic resins is made into resin quality concentration, then the solution for preparing is put into the ultrasonic concussion of supersonic wave cleaning machine 1.5h;
D. the implantation stage of CNT
Phenolic resins is added scattered carbon nano-tube solution of B stage, and the phenolic resins mass concentration is controlled to be 10%, and then mechanical dispersion evenly is coated on the surface of carbon paper base substrate, and the mass ratio of phenolic resins and carbon paper base substrate is controlled at 6: 4; Dry the dry 2.5h of processing in the baking oven of 65 ℃ afterwards; Then hot-press solidifying moulding on vulcanizer, condition of cure are 2MPa, 170 ℃, 1.5h; Then charing in retort, carbonization condition are first to vacuumize below 10Pa, are warming up to 850 ℃, and inflated with nitrogen is naturally cooling to the atmospheric pressure charing 6h; Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 2.5h under 1800 ℃.
Embodiment 5:
A. the pretreatment stage of CNT
For CNT is further purified, remove the impurity such as catalyst of bringing in preparation process, improve simultaneously the dispersiveness of CNT, commercially available CNT is dipped in the aqueous solution of nitric acid of 1.0mol, with distilled water, CNT is cleaned repeatedly repeatedly after 6h, then put it into dry 6h in the baking oven of 100 ℃ then;
B. the scatter stage of CNT
1. take the 0.6g CNT (carbon nano-tube), add the absolute ethyl alcohol of 1000ml;
2. configure neopelex 2g/L (with the volume ratio of absolute ethyl alcohol), be placed in the ultrasonic concussion of supersonic wave cleaning machine, the concussion time is 2.5h;
C. the scatter stage of resin
It is 20% ethanol system that phenolic resins is made into resin quality concentration, then the solution for preparing is put into the ultrasonic concussion of supersonic wave cleaning machine 2h;
D. the implantation stage of CNT
Phenolic resins is added scattered carbon nano-tube solution of B stage, and the phenolic resins mass concentration is controlled to be 10%, and then mechanical dispersion evenly is coated on the surface of carbon paper base substrate, and the mass ratio of phenolic resins and carbon paper base substrate is controlled at 8: 2; Dry the dry 1.5h of processing in the baking oven of 75 ℃ afterwards; Then hot-press solidifying moulding on vulcanizer, condition of cure are 5MPa, 190 ℃, 2.5h; Then charing in retort, carbonization condition are first to vacuumize below 10Pa, are warming up to 900 ℃, and inflated with nitrogen is naturally cooling to the atmospheric pressure charing 10h; Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 1.5h under 2200 ℃.
Embodiment 6:
The technological parameter in A, B, C stage is identical with example 2, and the D stage, it is identical with example 2 that all the other steps all adopt except the moulding carbon paper not being carried out charing and graphitization processing, and the E stage carries out by the following method:
The moulding carbon paper that has applied CNT is placed in cvd furnace, first is evacuated under 10Pa, then be warming up to 800 ℃ with the programming rate of 8 ℃ per minute, insulation 2h, pass into the mist of propylene and argon gas, volume ratio both is 1: 1 again, reaction gas flow 5L/ minute.To atmospheric furnace pressure condition, propylene gas is implemented discontinuous and is supplied gas at 1kPa.Vacuumize nature after deposition 2h cooling.Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 2.5h under 1800 ℃.
Embodiment 7:
The technological parameter in A, B, C stage is identical with example 2, and the D stage, it is identical with example 2 that all the other steps all adopt except the moulding carbon paper not being carried out charing and graphitization processing, and the E stage carries out by the following method:
The moulding carbon paper that has applied CNT is placed in cvd furnace, first is evacuated under 10Pa, then be warming up to 900 ℃ with the programming rate of 10 ℃ per minute, insulation 2h, pass into the mist of oil liquefied gas and nitrogen, volume ratio both is 1: 1 again, reaction gas flow 2L/ minute.To atmospheric furnace pressure condition, oil liquefied gas is implemented continous mode and is supplied gas at 1kPa, vacuumizes nature after deposition 1h cooling.Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 1.5h under 2200 ℃.
Claims (2)
1. the manufacturing technique of a modified carbon fiber paper by adopting carbon nanotube implanting, make the carbon paper base substrate with the charcoal fibrous paper, implant CNT on its surface, even carbon nanotube is disperseed, CNT is in carbon paper billet surface uniform load, CNT and carbon paper base substrate strong bonded is characterized in that: its several stages are as follows:
A. the pretreatment stage of CNT
The aqueous solution of nitric acid that CNT is placed in 0.1～1.0mol/L carries out oxidation processes 4～10h, so with distilled water, CNT is cleaned repeatedly repeatedly, then, then puts it into dry 4～10h in baking oven;
B. the scatter stage of CNT
Add the CNT of 0.2～10g/L in the ethanol solution of 2～3g/L of neopelex, the concussion time is 1.5～2.5h;
C. the scatter stage of phenolic resins
It is 10～30% absolute ethyl alcohol system that phenolic resins is made into resin quality concentration, then the solution for preparing is put into the ultrasonic concussion 1.5～2.5h of supersonic wave cleaning machine;
D. the implantation stage of CNT
The coating of carbon paper billet surface CNT refers to first apply phenolic resins, the CNT that rear coating ethanol disperses; Or first apply the CNT that ethanol disperses, rear coating phenolic resins; Or first carbon nanotube dispersed in phenol resin solution, after be coated on the carbon paper billet surface; The mass ratio of phenolic resins and carbon paper base substrate is controlled at 6～8:2～4; The carbon paper base substrate dries the dry 1.5～2.5h of processing in the baking oven of 65～75 ℃ afterwards; Then hot-press solidifying moulding on vulcanizer, condition of cure are 3～5MPa, 170～190 ℃, 1.5～2.5h; Then charing in retort, carbonization condition are first to vacuumize below 10Pa, are warming up to 850-1000 ℃, and inflated with nitrogen is naturally cooling to the atmospheric pressure charing 2-10h; Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 1.5～2.5h under 1800～2200 ℃; Or
The mass ratio of phenolic resins and carbon paper base substrate is controlled at 6～8:2～4; The carbon paper base substrate dries the dry 1.5～2.5h of processing in the baking oven of 65～75 ℃ afterwards; Then hot-press solidifying moulding on vulcanizer, condition of cure is 3～5MPa, 170～190 ℃, 1.5～2.5h, the moulding carbon paper is placed in cvd furnace, first be evacuated under 10Pa, then be warming up to 800～1000 ℃ with the programming rate of 5-10 per minute ℃, insulation 1～2h, then pass into the mist of carbon-source gas and diluent gas, volume ratio both is 1:1, reaction gas flow 0.1～5L/ minute; To atmospheric furnace pressure condition, carbon-source gas is implemented continous mode or discontinuous is supplied gas at 1kPa, vacuumizes nature after deposition 0.2～2h cooling; Then the moulding carbon paper is carried out graphitization processing, the graphitization condition is to be incubated 1.5～2.5h under 1800～2200 ℃.
2. the manufacturing technique of modified carbon fiber paper by adopting carbon nanotube implanting according to claim 1, it is characterized in that: described carbon-source gas is methane, propylene or oil liquefied gas, described diluent gas is nitrogen or argon gas.
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| CN103600517B (en) * | 2013-11-27 | 2016-09-07 | 苏州芳磊蜂窝复合材料有限公司 | A kind of preparation method of the honeycomb core with nano material specific performance |
| CN108755279B (en) * | 2018-07-06 | 2020-07-31 | 江西克莱威纳米碳材料有限公司 | Aramid fiber porous conductive paper and preparation method thereof |
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| CN109256564B (en) * | 2018-09-10 | 2021-07-09 | 江西克莱威纳米碳材料有限公司 | Carbon nanotube-graphite composite material, lithium-sulfur battery positive electrode material and lithium-sulfur battery |
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| CN113105242B (en) * | 2021-03-15 | 2022-07-15 | 嘉寓氢能源科技(辽宁)有限公司 | Carbon paper for proton exchange membrane hydrogen fuel cell and preparation method thereof |
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