Production of material based on carbon nanotubes

FIELD: process engineering.

SUBSTANCE: invention can be used for production of articles operated in aggressive media and at high temperatures, such as membranes, filters, coatings. Proposed material is produced in vertical CVD-reactor 1 by gas phase deposition. Said reactor id pre-evacuated, blown with argon for 10-12 minutes and heated to 900-1150°C. Then, hydrogen carrier gas is forced via channel 2 at flow rate of about 1000 ml/min along with a three-component mix fed at the rate of 4.5-5.0 ml/min the contains the following elements in wt %: 1.0-10.0 - ferrocene, 0.5-1.5 - thiophen and 93.5-98.5 - ethanol.

EFFECT: production of porous films with pore size of 10-300 nm composed by carbon nanotubes 2.5-30 nm in diameter without application of substrate or carcass.

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The present invention relates to functional materials, in particular the production of porous films used for the fabrication of membranes, filters, coatings, etc., Carbon materials, in connection with chemical inertness, can be used when working in corrosive environments and at high temperatures the working area, including as containers for storing various objects, such as metal powders catalysts.

Currently, there are many known methods of preparation and applications of thin porous films.

Known (patent RF 2305632 C2, IPC B32B 5/18, published 10.09.2005) a method of manufacturing a multilayer microporous films of polyethylene and polypropylene. Films made by this method, suitable for semi-permeable membranes for the filtration of liquids, but they need to get on the substrate and cannot be used in aggressive environments and at elevated temperatures of the working area.

Known thin film of α,α,α',α'-tetrafluoropropylene (RF patent 2268900, IPC C08G 61/02, C08J 5/18, published 27.01.2006). Method implemented by a sequential implementation in a three-zone reactor, consisting of zones of sublimation, pyrolysis and condensation. Sublimation and pyrolysis subjected to cyclic dimer 1,1,2,2,9,9,10,10-acceptor[2,2]paracyclophane, the products of pyrolysis condense and combine the Menno polymerized on the substrate in the film tetrafluoroethylene. To obtain porous films spend two-stage heat treatment of the resulting product. This material is resistant and inert, but made the film attached to the substrate, and it requires getting scarce reagents and careful control of the synthesis that leads to a significant rise in the cost of the product.

Known holonomically film cathode and method thereof (patent RF 2194328, IPC H01J 1/30, 9/02, published 10.12.2002). This cathode obtained by the method of gas-phase synthesis, including the ignition glow DC discharge in a mixture of hydrogen with carbon-containing additive and deposition on located on the anode substrate for carbon film. When this carbon film precipitated sequentially, maintaining the appropriate temperature and pressure.

A known method of obtaining films based on carbon nanotubes (patent US 2009211901, IPC C01B 31/02, H01B 13/00, H01B 5/14, H01L 33/00, H01M 4/96, published 12.02.2009). In the described method proposed various ways of getting films optimum thickness and porosity. The method includes several steps: dispersing carbon nanotubes in surfactant, filtering the suspension of nanotubes with the formation of the film material on the membrane filter, the removal of the surfactant. However, this method of obtaining porous thin films also require a substrate or to the RCAS, which is a membrane filter.

A method of obtaining carbon films by the method of gas-phase deposition (CVD) (patent JP 2001192829, IPC C01B 31/02; C23C 16/26; C23C 16/511; H01J 9/02, published 05.01.2000). In this case, it is proposed to use a modified CVD method, namely plasma chemical vapor deposition. The disadvantage is the need for the use of the substrate.

Also known is a method of obtaining single-walled carbon nanotubes by the method of gas-phase deposition (CVD) (WO 2012-059716, IPC C01B 1/02, B01J 37/08, B01J 23/745, D01F 9/12, published on 10.05.2012). In this way I propose to use the method of synthesis of carbon nanotubes, in which the catalyst (composed of ferrocene) is introduced into the reactor together with the carbon-containing substance is methane. At this point the process parameters under which predpodtitelno the formation of catalyst particles less than 10 nm in diameter. The resulting aerogel of single-walled nanotubes, which pulled and twisted into a fiber by winding on the spindle.

The closest in technical essence (prototype) is a method for braided carbon fibers of the nanotubes by the method of gas-phase deposition (CVD) (patent JP 2011-202338, IPC C01B 31/02, D01F 9/127, D02G 3/02, D02G 3/02, D02G 3/04, D01F 9/08, published on 13.10.2011). In this way of aerogel carbon nanotubes formed in the CVD-reactor: if you want the Ute fiber by winding on the spindle. Deposition of carbon nanotubes is carried out at a temperature of from 1000 to 1500°C in flowing hydrogen atmosphere from precursor containing the catalyst. As a precursor of carbon nanotubes using a three-component mixture composition: 0,23-2.3 wt.% ferrocene, 0.2 to 3.0 wt.% thiophene, 94,7-97,2 wt.% of ethanol. The feed rate of the mixture from 0.08 to 0.25 cm3/min Carrier gas is hydrogen which offers speeds ranging from 400 to 800 cm3/min. Minimum, the synthesis time is 30 min, and due to the fact that carbon nanotubes is continuously removed from the working zone, the deposition can be performed for a long time. In this way we obtain a material in the form of elongated braided fibers, and the use of the set of values of the process parameters is not possible to obtain a porous film.

Objective of the claimed invention is to develop ways to get the material in the form of a porous film composed of carbon nanotubes without using the substrate or frame.

To solve this problem, we offer to carry out the deposition of carbon nanotubes, schematically represented in Fig.1, in a flow-through tubular CVD reactor 1 vertical type with flow through channel 2 carrier gas is hydrogen and the reactive mixture in the direction of "top-down". The inner diameter of the rector 1 is 40 mm, the length of the reaction of the working area 300 is m The process parameters and conditions of the deposition is chosen experimentally in a series of experiments. As a carbon source for the formation of nanotubes using a three-component mixture consisting of 0.5 to 1.5 wt.% thiophene, 1.0 to 10.0 wt.% ferrocene, of 93.5-98.5 wt.% of ethanol. The mixture is fed at a speed ranging from 4.5 to 5.0 cm3/min. Ethanol acts as a solvent and the main source of carbon. Clusters of iron, formed by thermal decomposition of ferrocene, are the catalyst particles, which is the growth of nanotubes 4 (Fig.1). As a promoter of dissolution of carbon in the particles of iron is sulfur, which is contained in the thiophene. The deposition is carried out in the flow of carrier gas is hydrogen when its flow rate is not more than 1000 cm3/min. and the Temperature of the working area 6 (Fig.1) from 900 to 1150°C.

The pore size of the obtained film education controlled by the deposition parameters. Settling time of 25 min to 120 min In the resulting porous film education in the form of a sleeve 7 (Fig.1), consisting of carbon nanotubes. It should be emphasized that the final result is affected by all the parameters together, and changing any of them affects the contribution of the other, therefore, the selection of suitable conditions is a complex task, requiring a series of experiments to search for optimalnyh values. It should also be noted that an important role in the process of gas-phase deposition plays the geometry of the reactor, which in the present invention remains constant.

The used temperature range from 900 to 1150°C gives a positive result when the process of deposition of carbon nanotubes from the gas phase at a temperature below 900°C do not fully achieved problem solving, and the upper limit in the present invention was due to technical limitations of the installation.

The use of flow rate carrier gas near 1000 cm3/min due to the residence time of the carbon-containing mixture in the working zone of the reactor: at higher speeds the components of the mixture is not completely decomposed, and therefore dramatically decreases the yield of carbon nanotubes that do not allows to achieve a positive result - deposition of the porous film at a lower flow rate carrier gas target product is formed, but it is heavily contaminated with impurities.

Used a range of concentrations of thiophene 0.5 to 1.0 allows you to ensure a positive result, the use of lower concentrations leads to a decrease in the rate of formation of carbon nanotubes and increase the duration of the process, the use of higher concentrations of contaminates gray target product.

Use the series a range of concentrations of ferrocene 1,0-10,0 allows you to ensure a positive result, using a lower concentration leads to a decrease in the yield of carbon nanotubes and the formation of soot and pyrolytic carbon, the use of higher concentrations leads to contamination by iron carbide target product.

Using high compared to the value of the corresponding parameter in the prototype, the speed of feeding the carbon-containing mixture of 4,5-5 cm3rpm provides a positive result, at lower speeds porous film of carbon nanotubes is formed slowly and only on the substrate at a higher speed of the target product is highly contaminated with impurities.

Thus, the total set of optimal parameter values to obtain gas-phase deposition of a porous film of carbon nanotubes to achieve the best possible result.

In Fig.1-7 shows a diagram and pictures explaining the claimed invention is:

in Fig.1 is a diagram of a flow CVD reactor vertical type;

1 - reactor;

2 - channel, for supplying carrier gas and a mixture of;

3 - dimensional vessel;

4 - area growth of carbon nanotubes;

5 - bake;

6 - the working zone of the reactor;

7 - closed tsilindricheskoi the formation of a porous film -"stocking";

in Fig.2 shows obtained in a transmission electron microscope micrograph of single-walled ug is rodnoy nanotubes;

in Fig.3 shows the obtained transmission electron microscope micrograph of the porous film deposited according to the present invention, as described in example 1;

in Fig.4 shows obtained in the scanning electron microscope micrograph of a porous film consisting of multiwalled carbon nanotubes;

in Fig.5 shows obtained in the scanning electron microscope micrograph of a porous film consisting of multiwalled carbon nanotubes;

in Fig.6 shows a photograph of a "grip" of the porous film obtained according to the present invention;

in Fig.7 shows a photograph of a "grip" of the layers of the porous film obtained according to the present invention.

Examples of implementation of the method.

The method of obtaining porous films based on carbon nanotubes, vapor deposition is carried out in a flow-through vertical CVD reactor 1 (Fig.1) equipped with a vacuum system and gas distribution, to clean the system from air and control the gas flow. The reactor 1 equipped with a system of inlet and exhaust gases, pressurized. The air is pumped out of the reactor and adjacent the supply system and exhaust gases. In the reactor 1 serves argon through the channel 2, then purge the reactor 1 with argon for 10 to 20 minutes, include heating furnace 5, which supports the working area of the reactor to the required temperature. Then stop feeding argon and allowed to pass through the channel 2 carrier gas is hydrogen with a bulk velocity of 1000 cm3/min. Receptacle 3, which is connected with the reactor, with measuring scale fill three-carbon mixture composition: 0.5 wt.% thiophene, 5.5 wt.% ferrocene, 94 wt.% of ethanol. When the temperature in the reactor reaches 1150°C using a peristaltic pump allowed carbon-containing mixture in the reactor 1 with a speed of 4.5 cm3/min. for 25 minutes in the zone of the reactor at the outlet from the working area, the formation of a closed cylindrical education 7, in appearance resembling a stocking, a porous film with a pore size of from 10 to 70 nm, consisting primarily of single-walled carbon nanotubes with a diameter of 2.5-4.0 nm, shown in Fig.2 and Fig.3.

Other examples of conduct similar to the first. They are different quantitative parameters.

Example 2. At a feed rate of the carbonaceous mixture of 3.0 cm3/min, the flow rate of carrier gas 1500 cm3/min, the temperature of the working area 800°C, deposition time 120 min and the composition of the carbon-containing mixture: 0.5% thiophene, 5.5% ferrocene, 94% of ethanol is deposited on the walls of the reactor porous film with a pore size of 50 to 300 nm, consisting of multiwalled carbon nanotubes with a diameter of 10-30 nm without education "stocking".

Example 3. When the speed n is giving carbon a mixture of 4.5 cm 3/min, the flow rate of carrier gas of 1000 cm /min, the temperature of the working area of 1150°C, deposition time 120 min and the composition of the carbon-containing mixture: 1.5 wt.% thiophene, 10 wt.% ferrocene, 88.5 wt.% ethanol - is the formation of "stocking" of the porous film with a pore size of 50 to 150 nm, consisting of multiwalled carbon nanotubes with a diameter of 25-30 nm, are heavily contaminated with mixture of sulfur and iron carbide.

Example 4. At a feed rate of the carbonaceous mixture of 10.0 cm3/min, the flow rate of carrier gas 600 cm3/min, the temperature of the working area 1000°C, deposition time 120 min and the composition of the carbon-containing mixture: 1.5 wt.% thiophene, 10 wt.% ferrocene, 88.5 wt.% ethanol - is deposited on the walls of the reactor porous film with a pore size of from 70 to 200 nm, consisting of multiwalled carbon nanotubes with a diameter of 25-30 nm, with the formation of pautinopodobnoj grid.

Example 5. At a feed rate of the carbonaceous mixture of 5.0 cm3/min, the flow rate of carrier gas 1000 cm3/min, the temperature of the working area 1000°C, deposition time 60 min and the composition of the carbon-containing mixture: 1.5% thiophene, 1.5% ferrocene, 97% of ethanol is deposited on the walls of the reactor outside of the working area of the porous film with a pore size of from 20 to 150 nm with the formation of "stocking", consisting mainly of single-walled carbon nanotubes with a diameter of 2.5-5 nm.

3/min, the flow rate of carrier gas 1000 cm3/min, the temperature of the working area of 1150°C, deposition time of 30 min and the composition of the carbon-containing mixture: 0.5 wt.% thiophene, 6.0 wt.% ferrocene, 93.5 wt.% ethanol - is the formation of "stocking" of the porous film with a pore size of from 70 to 250 nm, consisting of multiwalled carbon nanotubes with a diameter of 5-30 nm. The microstructure of the films is shown in Fig.4 and Fig.5.

Example 7. At a feed rate of the carbonaceous mixture of 4.5 cm3/min, the flow rate of carrier gas 1000 cm3/min, the temperature of the working area 900°C, deposition time 60 min and the composition of the carbon-containing mixture of 0.5 wt.% thiophene, 1.0 wt.% ferrocene, 98.5 wt.% ethanol - is the formation of "stocking" of the porous film with pore size from 20 to 120 nm, consisting primarily of single-walled carbon nanotubes with a diameter of 2.5-5 nm mixed with soot.

Example 8. At a feed rate of the carbonaceous mixture of 4.5 cm3/min, the flow rate of carrier gas 1000 cm3/min, the temperature of the working area of 1150°C, deposition time of 50 min and the composition of the carbon-containing mixture of 0.5 wt.% thiophene, 5.5 wt.% ferrocene, 94 wt.% ethanol - is the formation of multi-layered "stocking", shown in Fig.6 and Fig.7, the porous films with pore size from 20 to 100 nm, consisting preimushestvenno single-walled nanotubes with a diameter of 2.5-5 nm.

Thus, the proposed method allows to create a new type of porous films. The technical result is free from the substrate and a skeleton of a porous film of a carbon nanotube.

The given examples show that the claimed invention of the parameters is justified and allow you to get the material without the use of a substrate or frame, which is a porous carbon film consisting of nanotubes, free from the frame and the substrate. The structure of the film is a chaotic tangle - "the grid" - long carbon nanotubes with a diameter of from 2.5 to 30 nm. The average estimated pore diameter of the grid depending on the mode of obtaining film approximately ranges from 10 to 250 nm.

A method of producing material based on carbon nanotubes by gas-phase deposition in a CVD reactor in the flow of carrier gas is hydrogen and the decomposition products of carbon-containing three-component mixture consisting of ferrocene, thiophene and ethanol, wherein the deposition is carried out in a flow-through vertical CVD reactor, pre-vacuum, then rinsed with argon for 10-12 minutes, heat the reactor to the desired temperature of 900-1150°C and then transmit the carrier gas is hydrogen with a volume rate of about 1000 ml/min, simultaneously with the transmission of carrier gas of hydrogen in the reaction the PRS serves a three-component mixture with a speed of 4.5-5.0 ml/min, this three-component mixture taken in the following ratio of components, wt.%:

ferrocene1,0-10,0
thiophene0.5 to 1.5
ethanol93,5-98,5



 

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