CN114267492B - Uniform transparent conductive film with long tube bundle carbon nano tubes and preparation method thereof - Google Patents
Uniform transparent conductive film with long tube bundle carbon nano tubes and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a uniform transparent conductive film with long tube bundle carbon nanotubes and a preparation method thereof, belonging to the technical field of transparent conductive films. The invention adopts a floating catalytic chemical vapor deposition method, ethanol, toluene and acetonitrile are used as carbon sources, sulfur-containing compounds are used as growth promoters, ferrocene, nickel dichloride and cobalt dichloride are used as catalysts, a sample injection system is used for injecting a mixed solution of the carbon sources, the growth promoters and the catalysts into a high-temperature tube furnace at a certain speed under the action of inert gas and hydrogen, and carbon nanotubes growing in a vapor phase are collected on a filter membrane, so that a uniform and transparent conductive film with long tube bundle carbon nanotubes is obtained. The carbon nano tube prepared by the method has longer length, and effectively reduces the number of contact junctions in the film, thereby obviously improving the conductivity of the carbon nano tube film.
Description
Technical Field
The invention belongs to the technical field of transparent conductive films, and particularly relates to a uniform transparent conductive film with long tube bundle carbon nanotubes and a preparation method thereof.
Background
The carbon nanotube transparent conductive film has very wide application in the field of modern electronics, including the fields of photovoltaics, touch screens, liquid crystal displays, organic light emitting diodes and the like. The carbon nanotube transparent conductive film is a potential for replacing the traditional indium tin oxide film. The current method for preparing the carbon nano tube transparent conductive film is mainly divided into dry method preparation and wet method preparation. In general, the wet process for preparing the carbon nanotube film comprises dispersing carbon nanotubes in a surfactant, and performing ultrasonic treatment, centrifugation, suction filtration and the like to prepare the film (H. -Z.Geng, K.K.Kim, K.P.So, Y.S.H.Lee, Y.Chang and Y.S.H.Lee, J.Am.Chem.Soc.,2007,129,7758-7759). However, during the wet preparation, the carbon nanotubes are cut or impurities are introduced due to the influence of solvents, ultrasound and the like, and finally, the conductivity of the carbon nanotubes cannot be fully exerted. On the other hand, the dry-process thin film does not need to be subjected to subsequent treatments such as solution or ultrasound, and the prepared carbon nanotube maintains intrinsic physicochemical properties, so that the carbon nanotube thin film with excellent conductivity can be obtained. The floating catalytic chemical vapor deposition method is a representative dry method for preparing carbon nanotube films (A.Kaskela, A.G.Nasibulin, M.Y.Timmermans, B.Aitchison, A.Papadimitratos, Y.Tian, Z.Zhu, H.Jiang, D.P.Brown, A.Zakhidov and E.I. Kauppien, nano Lett.,2010,10,4349-4355.). The method not only can obtain the film with excellent conductivity, but also can transfer the carbon nano tube film to any substrate, and is a continuous production process.
At present, the surface resistance of the carbon nanotube film prepared by using a floating catalytic chemical vapor deposition method is far higher than a theoretical value, and the main reason is that the length of the produced carbon nanotubes is insufficient, so that the contact junction between the carbon nanotubes is increased, and finally, the resistance of the film is increased. In addition, since the carbon nanotubes grown in the vapor phase have a characteristic of flowing arbitrarily with the gas flow, the prepared carbon nanotube film is not uniform enough. Thus, obtaining a highly conductive and uniform carbon nanotube film is a significant challenge.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a uniform transparent conductive film having long tube bundles of carbon nanotubes and a method for preparing the same. Solves the problems of too short and uneven length of the carbon nano tube prepared under the normal condition, so as to obtain the carbon nano tube film with high conductivity.
The technical scheme of the invention is as follows:
a process for preparing the uniform transparent conducting film with long tube bundle of carbon nanotubes includes such steps as floating catalytic chemical vapor deposition, taking alcohol, toluene and acetonitrile as carbon source, taking sulfur-contained compound (including thiophene, thiourea and thiol) as growth promoter, taking ferrocene, nickel-dicyclopentadienyl and cobalt as catalyst, loading the mixed solution of carbon source, growth promoter and catalyst in high-temp tube furnace, regulating the flow rate of hydrogen, regulating the size and activity of catalyst, regulating the growth condition of carbon nanotubes, and collecting the carbon nanotubes growing in gas phase in high-temp tube furnace onto filter membranes.
Further, the equipment used in the preparation method mainly comprises a sample injection system, a carrier gas system, a high-temperature tube furnace, a 1/8 inch plus 1/4 inch combined stainless steel gas tube, a filter membrane collector and a vacuum pump, wherein the sample injection system, the high-temperature tube furnace, the 1/8 inch plus 1/4 inch combined stainless steel gas tube, the filter membrane collector and the vacuum pump are sequentially connected, and carrier gas (inert gas and hydrogen) of the carrier gas system enters the high-temperature tube furnace from between the sample injection system and the high-temperature tube furnace.
Further, the high-temperature tube furnace is a horizontal high-temperature tube furnace, the length is 100-150 cm, the effective heating area is 70-90 cm, and the inner diameter of a quartz tube in the high-temperature tube furnace is 2.5-3.5 cm.
Further, a container for containing a precursor solution of the catalyst, the growth promoter and the carbon source is arranged in the sample injection system, and the precursor solution is conveyed by a microinjection pump.
Further, the preparation method comprises the following steps:
(1) At 200-400sccm (cm) 3 Under the protection of inert gas, gradually heating the high-temperature tube furnace to 950-1050 ℃, and injecting the precursor solution in the sample injection system into the high-temperature tube furnace at 5-20 mu L/min through a microinjection pump; the mass concentration of the catalyst is 0.2-0.4%, and the mass concentration of the growth promoter is 0.03-0.06%;
(2) The flow rate of inert gas is regulated to be 200-500sccm, the flow rate of hydrogen is regulated to be 50-400 sccm, a carbon source and a catalyst are cracked into atomic carbon and catalyst nano particles in a high temperature area of a tube furnace, and the carbon nano tubes grow in the high temperature area of the high temperature tube furnace under the action of a growth assisting agent and high temperature;
(3) The grown carbon nano tube is taken out of the high-temperature tube furnace along with carrier gas, is uniformly deposited on a filter membrane in a filter membrane collector after passing through a 1/8 inch and 1/4 inch combined stainless steel gas tube, and carbon nano tube conductive films with different thicknesses are obtained by controlling deposition time.
Further, the temperature rising rate of the high-temperature tube furnace in the step (1) is 5-10 ℃/min.
Further, in the step (3), the carbon nanotubes are uniformly deposited on the filter membrane by means of vacuum pump filtration.
Further, in order to obtain a large-sized carbon nanotube film, the diameter of the filter membrane in the step (3) is 4-10cm.
Further, the diameter of the tube bundles of the carbon nanotubes in the step (3) is 1.5-60 nm, and the length of the tube bundles is 10-80 mu m.
The invention also provides a uniform transparent conductive film with long tube bundle carbon nanotubes prepared by the preparation method.
Further, the Raman spectrum I of the conductive film G /I D The ratio of (2) is 80-100.
Further, the conductive film can be directly transferred to a glass or plastic substrate by a pressing method.
Compared with the prior art, the invention has the following beneficial effects:
1. the carbon nano tube obtained by the invention has longer length, and effectively reduces the number of contact junctions in the film, thereby obviously improving the conductivity of the carbon nano tube film.
2. The invention uses lower sample injection rate and smaller hydrogen carrier gas, thereby reducing the cost.
3. The invention adopts the combined stainless steel gas pipe of 1/8 inch and 1/4 inch to collect the sample, so that the film is more uniform.
4. The invention provides a method for continuously growing a high-conductivity carbon nano tube film, which brings help to actual production and has wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention, the drawings to which the embodiments relate will be briefly described.
FIG. 1 is a schematic diagram of a system for preparing a uniform transparent conductive film of carbon nanotubes with bundles of long tubes.
Fig. 2. Carbon nanotube conductive films (a) of different sizes and different thicknesses prepared in example 1 and carbon nanotube conductive films can be transferred to a flexible transparent substrate (b).
FIG. 3 shows a scanning electron microscope (a), a carbon nanotube length distribution graph (b), a transmission electron microscope (c) and a Raman spectrum (d) of a carbon nanotube conductive film of the carbon nanotube prepared in example 1.
Fig. 4 is a graph showing transmittance and area resistance of the conductive thin film of carbon nanotubes prepared in example 1.
FIG. 5 is a graph of a sample of the carbon nanotube film collected in comparative example 2 using a 1/4 inch gas tube alone.
Detailed Description
The following detailed description of the invention is provided in connection with examples, but the implementation of the invention is not limited thereto, and it is obvious that the examples described below are only some examples of the invention, and that it is within the scope of protection of the invention to those skilled in the art to obtain other similar examples without inventive faculty.
As shown in figure 1, the equipment for preparing the uniform and transparent conductive film with the long tube bundle of carbon nanotubes mainly comprises a sample injection system, a carrier gas system, a high-temperature tube furnace, a 1/8 inch and 1/4 inch combined stainless steel gas tube, a filter membrane collector and a vacuum pump, wherein the sample injection system, the high-temperature tube furnace, the 1/8 inch and 1/4 inch combined stainless steel gas tube, the filter membrane collector and the vacuum pump are sequentially connected, the carrier gas of the carrier gas system enters from the space between the sample injection system and the high-temperature tube furnace, the precursor solution of a catalyst, a growth promoter and a carbon source is filled in the sample injection system, the precursor solution is loaded into the high-temperature tube furnace for reaction and growth of the carbon nanotubes under the action of inert gas and hydrogen, and the carbon nanotubes are deposited into the filter membrane collector at the tail part along with the carrier gas, so that the carbon nanotube film is finally obtained.
In the specific implementation process, the invention selects a horizontal high-temperature tube furnace and utilizes a floating catalytic chemical vapor deposition method to prepare the large-size and uniform carbon nanotube transparent conductive film. The method comprises the steps of taking metal organic matters such as ferrocene, nickel dichloride, cobalt dichloride and the like as catalysts, taking sulfur-containing matters as growth aids, taking liquid organic matters such as ethanol, toluene, acetone and the like as carbon sources, adding a certain amount of hydrogen into inert gas (argon or nitrogen) as carrier gas, growing carbon nano tubes at 1000 ℃, and depositing the carbon nano tubes in the carrier gas into a filter membrane collector through a 1/8 inch and 1/4 inch combined stainless steel gas pipeline to obtain a uniform film; the method comprises the following specific steps:
(1) Gradually heating the tube furnace to 1000 ℃ under the protection of 200-400sccm nitrogen, and then injecting the precursor in the microinjection pump into the tube furnace at the concentration of 5-20 mu L/min;
(2) The flow rate of carrier gas nitrogen is adjusted to 500sccm, and the flow rate of hydrogen is adjusted to 50-300 sccm (2-8L/min is generally required in the prior art). The carbon nano tube grows in a high temperature area;
(3) The grown carbon nano tube is taken out of the tube furnace along with carrier gas, the carbon nano tube is deposited on the filter membrane by adopting a 1/8 inch and 1/4 inch combined stainless steel gas tube, carbon nano tube films with different thicknesses can be obtained by controlling different deposition time, and the carbon nano tube films with different sizes can be obtained by adopting filter membranes with different sizes.
(4) After the preparation is finished, the tube furnace is cooled to room temperature, and the sample preparation is finished.
The following describes in detail the method for preparing a uniform transparent conductive film having long tube bundle carbon nanotubes according to the present invention by combining examples with the accompanying drawings.
Example 1
In this example, under the protection of 200sccm nitrogen, the tube furnace is gradually heated to 1000 ℃, then the precursor in the microinjection pump, including 100ml of ethanol, ferrocene (with a mass concentration of 0.3%) and thiophene (with a mass concentration of 0.03%), is injected into the tube furnace at 5 μl/min, then the flow rate of carrier gas nitrogen is adjusted to 500sccm, the flow rate of hydrogen is adjusted to 150sccm, carbon nanotubes are grown in a high temperature region, the grown carbon nanotubes are carried out of the tube furnace along with the carrier gas, and the carbon nanotubes are deposited on the filter membrane by adopting a 1/8 inch and 1/4 inch combined stainless steel gas tube, carbon nanotube films with different thicknesses can be obtained by controlling different deposition times, carbon nanotube films with different sizes can be obtained by adopting filter membranes with different sizes, see fig. 2 (a), and the carbon nanotube films on the filter membrane can be transferred to a flexible transparent substrate, such as polyethylene terephthalate (PET), see fig. 2 (b).
As shown in fig. 3 (a), the prepared carbon nanotubes are uniform and compact, have no other impurities, and are arranged in a disordered and crossed manner as shown in a scanning electron microscope; as shown in FIG. 3 (b), the length distribution of the prepared carbon nanotube bundles is in the range of 5-45 μm and the average length is 18.39 μm; as shown in the transmission electron microscope result of fig. 3 (c), the prepared carbon nanotubes are clean and have few impurities, and the diameter of the tube bundle is about 10nm; as can be seen from FIG. 3 (d), the prepared carbon nanotube film has I G /I D The value is 96.4, which indicates that the prepared carbon nano tube has high crystallinity.
As shown in fig. 4, carbon nanotube films with different thicknesses are transferred onto a quartz substrate by a dry method, the light transmittance and the surface resistance of the carbon nanotube films are tested to obtain light transmittance of 95%,91%,90%,85%,76% and 60%, the corresponding surface resistances of the carbon nanotube films are 2015, 736, 530, 300, 208 and 106 Ω/sq (the surface resistances of the carbon nanotube films are tested by adopting four probes), the surface resistance can be further reduced by doping gold chloride, a pre-prepared acetonitrile solution of gold chloride with the concentration of 16mmol/L is adopted, 100 μl of gold chloride solution is taken and is dripped on the carbon nanotube films, the carbon nanotube films are left stand for 3min and then washed by pure acetonitrile solution, doping is completed after drying, then the surface resistances of the doped carbon nanotubes are further tested, and the surface resistances of the carbon nanotube films after doping are respectively 438, 151, 121, 80, 56 and 35 Ω/sq.
Example 2
In this embodiment, under the protection of 400sccm nitrogen, the tube furnace is gradually heated to 1000 ℃, then the precursor in the microinjection pump, including 100ml of ethanol, ferrocene (mass fraction is 0.4%) and thiophene (mass fraction is 0.04%), is injected into the tube furnace at 10 μl/min, then the flow rate of carrier gas nitrogen is adjusted to 500sccm, the flow rate of hydrogen is adjusted to 300sccm, carbon nanotubes are grown in a high temperature region, the grown carbon nanotubes are carried out of the tube furnace along with the carrier gas, and the carbon nanotubes are deposited on the filter membrane by adopting a 1/8 inch and 1/4 inch combined stainless steel gas tube, carbon nanotube films with different thicknesses can be obtained by controlling different deposition times, and carbon nanotube films with different sizes can be obtained by adopting filter membranes with different sizes.
The scanning electron microscope shows that the prepared carbon nanotubes are uniform and compact, have no other impurities, and are in disordered cross arrangement. The length distribution range of the prepared carbon nanotube bundles is 8-76 mu m, and the average length is 26.4 mu m. As can be seen from the transmission electron microscope result, the prepared carbon nano tube is clean and has few impurities, and the diameter of the tube bundle is about 18.4nm. As can be seen from the Raman spectrum result, the prepared carbon nanotube film has I G /I D The value is 101.5, which indicates that the prepared carbon nano tube has high crystallinity.
The carbon nanotube films with different thicknesses were transferred onto a quartz substrate by dry method, and the light transmittance and the surface resistance thereof were tested, to obtain 94%,92%,90%,83%,77%,64% light transmittance, and the corresponding surface resistances thereof were 1421, 644, 481, 299, 179, 99 Ω/sq., respectively, and the surface resistances of the carbon nanotube films (gold chloride concentration 16mmol/L, doping amount 100 μl) after gold chloride doping were 401, 112, 101, 72, 49, 29 Ω/sq., respectively.
Comparative example 1
In this embodiment, under the protection of 400sccm nitrogen, the tube furnace is gradually heated to 1000 ℃, then the precursor in the microinjection pump, including 100ml of ethanol, ferrocene (mass fraction is 0.6%) and thiophene (mass fraction is 0.06%), is injected into the tube furnace at 30 μl/min, then the flow rate of carrier gas nitrogen is adjusted to 500sccm, the flow rate of hydrogen is adjusted to 50sccm, carbon nanotubes are grown in a high temperature region, the grown carbon nanotubes are carried out of the tube furnace along with the carrier gas, and the carbon nanotubes are deposited on the filter membrane by adopting a 1/8 inch and 1/4 inch combined stainless steel gas tube, carbon nanotube films with different thicknesses can be obtained by controlling different deposition times, and carbon nanotube films with different sizes can be obtained by adopting filter membranes with different sizes.
The scanning electron microscope shows that the prepared carbon nanotubes are uniform and compact, and the carbon nanotubes are arranged in a disordered and crossed mode. The length distribution range of the prepared carbon nanotube bundles is 4-35 mu m, and the average length is 9.2 mu m. As can be seen from the transmission electron microscope result, the prepared carbon nano tube has more amorphous carbon, and the diameter of the tube bundle is about 40.6nm. As can be seen from the Raman spectrum result, the prepared carbon nanotube film has I G /I D The value was 45.2.
Carbon nanotube films with different thicknesses are transferred onto a quartz substrate through a dry method, and the light transmittance and the surface resistance of the carbon nanotube films are tested to obtain light transmittance of 96%,92%,90%,85%,74% and 67%, the corresponding surface resistances are 3061, 1145, 984, 877, 692 and 501 Ω/sq respectively, and the surface resistances of the carbon nanotube films (gold chloride concentration is 16mmol/L and doping amount is 100 μl) after gold chloride doping are 1083, 501, 392, 301, 252 and 169 Ω/sq respectively.
Comparative example 2
In this example, under the protection of 200sccm nitrogen, the tube furnace was gradually heated to 1000 ℃, then the precursor in the microinjection pump, including 100ml of ethanol, ferrocene (mass concentration of 0.3%) and thiophene (mass concentration of 0.03%), was injected into the tube furnace at 5 μl/min, then the flow rate of carrier gas nitrogen was adjusted to 500sccm, the flow rate of hydrogen was adjusted to 150sccm, carbon nanotubes were grown in the high temperature zone, the grown carbon nanotubes were carried out of the tube furnace with the carrier gas, and the carbon nanotubes were deposited on the filter membrane using only 1/4 inch stainless steel gas tube, and the uniformity of the prepared carbon nanotube film was poor, as shown in fig. 5.
The results of comparative examples 1 to 2 and examples 1 to 2 show that the conductive film prepared by the method for preparing a uniform transparent conductive film with long bundle carbon nanotubes of the present invention has a long bundle and excellent conductivity, and the prepared film has a surface resistance of 481 Ω/sq. at 90% transmittance, and a gold chloride doping followed by 101 Ω/sq. The invention realizes the preparation of the transparent conductive film with large size and uniformity, and solves the problems of nonuniform film, poor conductivity and the like in the prior art.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (9)
1. A preparation method of a uniform transparent conductive film with long tube bundle carbon nanotubes is characterized in that a floating catalytic chemical vapor deposition method is adopted, ethanol, toluene and acetonitrile are used as carbon sources, sulfur-containing compounds are used as growth aids, ferrocene, nickel dicyclopentadienyl and cobalt are used as catalysts, a mixed solution of the carbon sources, the growth aids and the catalysts is injected into a high-temperature tube furnace at a certain speed under the carrying action of inert gas and hydrogen, and the carbon nanotubes growing in the gas phase in the high-temperature tube furnace are collected on a filter membrane to obtain the uniform transparent conductive film with long tube bundle carbon nanotubes;
the preparation method mainly comprises the following steps:
(1) Under the protection of 200-400sccm inert gas, heating the high-temperature tube furnace to 950-1050 ℃, and injecting the precursor solution in the sample injection system into the high-temperature tube furnace at 5-20 mu L/min through a microinjection pump; the mass concentration of the catalyst is 0.2-0.4%, and the mass concentration of the growth promoter is 0.03-0.06%;
(2) Regulating the flow rate of inert gas to 200-500sccm, regulating the flow rate of hydrogen to 50-400 sccm, and growing carbon nanotubes in a high temperature area in a high temperature tube furnace;
(3) The grown carbon nano tube is taken out of the high-temperature tube furnace along with carrier gas, is uniformly deposited on a filter membrane in a filter membrane collector after passing through a 1/8 inch and 1/4 inch combined stainless steel gas tube, and carbon nano tube conductive films with different thicknesses are obtained by controlling deposition time.
2. The preparation method according to claim 1, wherein the equipment used in the preparation method mainly comprises a sample injection system, a carrier gas system, a high-temperature tube furnace, a 1/8 inch plus 1/4 inch combined stainless steel gas tube, a filter membrane collector and a vacuum pump, wherein the sample injection system, the high-temperature tube furnace, the 1/8 inch plus 1/4 inch combined stainless steel gas tube, the filter membrane collector and the vacuum pump are sequentially connected, and the carrier gas of the carrier gas system enters the high-temperature tube furnace from between the sample injection system and the high-temperature tube furnace.
3. The preparation method according to claim 2, wherein the high-temperature tube furnace is a horizontal high-temperature tube furnace, the length is 100-150 cm, the effective heating area is 70-90 cm, and the inner diameter of a quartz tube in the high-temperature tube furnace is 2.5-3.5 cm; the sample injection system is provided with a container for containing a precursor solution of a catalyst, a growth promoter and a carbon source, and the precursor solution is conveyed by a microinjection pump.
4. The method according to claim 1, wherein the temperature rise rate of the high-temperature tube furnace in the step (1) is 5 to 10 ℃/min.
5. The method according to claim 1, wherein the carbon nanotubes are uniformly deposited on the filter membrane in the step (3) by means of vacuum pump filtration; the diameter of the filter membrane is 4-10cm.
6. The method according to claim 1, wherein the diameter of the tube bundles of the carbon nanotubes in the step (3) is 1.5 to 60nm, and the length of the tube bundles is 10 to 80 μm.
7. The electrically conductive film having long tube bundle carbon nanotubes and being uniformly transparent, which is produced by the production method according to any one of claims 1 to 6.
8. The conductive film according to claim 7, wherein the conductive film has a raman spectrum I G /I D The ratio of (2) is 80-100.
9. The conductive film according to claim 7 or 8, wherein the conductive film is directly transferred onto a glass or plastic substrate by a pressing method.
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