CN116425145A - Preparation method of horizontal array carbon nano tube - Google Patents
Preparation method of horizontal array carbon nano tube Download PDFInfo
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- CN116425145A CN116425145A CN202310402166.5A CN202310402166A CN116425145A CN 116425145 A CN116425145 A CN 116425145A CN 202310402166 A CN202310402166 A CN 202310402166A CN 116425145 A CN116425145 A CN 116425145A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 48
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 54
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 229910052786 argon Inorganic materials 0.000 claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 230000008569 process Effects 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 24
- 239000007789 gas Substances 0.000 description 22
- 229910052799 carbon Inorganic materials 0.000 description 11
- 238000001704 evaporation Methods 0.000 description 9
- 230000008020 evaporation Effects 0.000 description 8
- 230000002159 abnormal effect Effects 0.000 description 7
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000002109 single walled nanotube Substances 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/02—Single-walled nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/36—Diameter
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
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Abstract
The invention relates to a preparation method of a horizontal array carbon nano tube in the technical field of carbon nano tube preparation, which comprises the following steps: 1) Selecting graphite columns as an anode and a cathode, and forming shallow grooves on the side wall of the cathode; 2) The shallow groove of the cathode is filled with a catalyst, the cathode and the anode are horizontally arranged in a closed reaction container, the anode is positioned above the cathode, and the cathode and the anode are connected with a discharge device; 3) After the reaction vessel is vacuumized, sequentially adding methane and argon into the reaction vessel; 4) And electrifying to react, and collecting the carbon nano tubes in the reaction container to obtain the horizontal array. The invention can simplify the process equipment for preparing the horizontal array carbon nano tube and reduce the preparation cost of the horizontal array carbon nano tube.
Description
Technical Field
The invention belongs to the technical field of carbon nanotube preparation, and particularly relates to a preparation method of a horizontal array carbon nanotube.
Background
The carbon nanotube, also called bucky tube, is a one-dimensional quantum material with a special structure (the radial dimension is in the order of nanometers, the axial dimension is in the order of micrometers, and both ends of the tube are basically sealed). Carbon nanotubes mainly consist of layers to tens of layers of coaxial round tubes of carbon atoms arranged in a hexagonal manner. The layer-to-layer distance is kept constant, about 0.34nm, and the diameter is typically 2-20 nm. And the carbon hexagons can be divided into three types of zigzag, armchair and spiral according to different orientations of the carbon hexagons along the axial direction. The spiral carbon nano tube has chirality, the zigzag and armchair carbon nano tube has no chirality, the carbon nano tube is used as a one-dimensional nano material, the weight is light, the hexagonal structure is perfectly connected, and the spiral carbon nano tube has a plurality of abnormal mechanical, electrical and chemical properties. The wide application prospect of the carbon nano tube and the nano material is continuously shown in recent years along with the deep research of the carbon nano tube and the nano material.
In patent CN201910533219.0, a device and a method for preparing carbon nanotubes are disclosed, the device connects a catalyst evaporation cavity through a pipeline chemical vapor deposition cavity in a sealing way, so as to realize the combination of high-temperature physical evaporation and chemical vapor deposition, the catalyst directly enters the chemical vapor deposition cavity through a connecting channel, meanwhile, a gas circuit system respectively introduces carrier gas and carbon source gas from the catalyst evaporation cavity and the chemical vapor deposition cavity, so that the catalyst reacts with high-temperature cracked organic carbon sources to generate carbon nanotubes, and then the carbon nanotubes are separated and collected through a gas-solid separation cavity. The device has a complex structure, the evaporated gaseous catalyst is difficult to completely transfer to the chemical vapor deposition cavity, and the yield is low. Moreover, the reaction needs to be carried out under a closed condition, and the sealing difficulty of the structure is great.
The existing horizontal array carbon nanotube preparation process is complicated, the preparation equipment is complex, the preparation cost of the carbon nanotube is greatly improved, and the existing carbon nanotube preparation precision and efficiency are low.
Therefore, we propose a method for preparing a carbon nanotube in a horizontal array.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a preparation method of a horizontal array carbon nano tube, which comprises the following steps:
a preparation method of a horizontal array carbon nano tube comprises the following steps:
1) Selecting graphite columns as an anode and a cathode, and forming shallow grooves on the side wall of the cathode;
2) The shallow groove of the cathode is filled with a catalyst, the cathode and the anode are horizontally arranged in a closed reaction container, the anode is positioned above the cathode, and the cathode and the anode are connected with a discharge device;
3) After the reaction vessel is vacuumized, sequentially adding methane and argon into the reaction vessel;
4) And electrifying to react, and collecting the carbon nano tubes in the reaction chamber to obtain the horizontal array.
The method relates to the evaporation of the catalyst and the pyrolytic deposition of the carbon source on the surface of the catalyst particles during the preparation of the carbon nano-tubes. In the invention, the catalyst is loaded in the shallow grooves of the cathode graphite rod by arranging the cathode graphite rod with the shallow grooves, so that the evaporation of the catalyst can be realized. The evaporation of the catalyst and the pyrolysis deposition of the carbon source are carried out in the same reaction vessel, so that the structure of the device is simplified. In addition, the process of generating the carbon nano tube by pyrolysis and deposition of the carbon source is greatly affected by the air pressure condition, and the method is easy to realize the accurate control of the air pressure condition during the reaction.
In step 2), the catalyst may be a single substance of various transition metals and salts thereof or a mixture thereof, and preferably, in step 2), the catalyst is elemental iron.
Preferably, in step 2), the cathode and the anode are arranged vertically. The arrangement method is beneficial to improving the evaporation efficiency of the electric arc on the simple substance iron in the shallow groove and is beneficial to the generation of the horizontal array carbon nano tube.
Preferably, methane is added to the reaction vessel at 13.33 kPa.
Preferably, argon is added to the reaction vessel at 53.32 Pa.
When the pressure is higher or lower than the pressure, the amount of the horizontally-arrayed carbon nanotubes produced in the reaction vessel is relatively small or the horizontally-arrayed carbon nanotubes are not produced after the reaction.
Preferably, the condition of the energizing reaction is current 200A and voltage 20V. The magnitude of the current and voltage affects the arc generation between the cathode and anode, thereby affecting the vaporization of the catalyst and the pyrolytic deposition of the carbon source gas.
According to the invention, the catalyst is directly loaded on the cathode graphite rod, and the evaporation of the catalyst and the vapor deposition of the carbon nano tube are carried out in the same reaction chamber, so that the structure of the device is simplified. The arc generated between the cathode and anode provides the high temperature conditions required for catalyst vaporization while providing the heat required for pyrolytic deposition of the carbon source gas.
Drawings
The invention will be further described with reference to the drawings and examples.
FIG. 1 is a schematic flow chart of the method of the present invention.
Fig. 2 is a SEM image of a horizontal array of carbon nanotubes prepared by the method of the present invention.
FIG. 3 is a graph of the dimensions of a horizontal array of carbon nanotubes prepared by the method of the present invention.
Detailed Description
The present invention will now be described more fully hereinafter with reference to the accompanying drawings, in which embodiments of the invention are shown, and in which embodiments of the invention are shown. All other embodiments, modifications, equivalents, improvements, etc., which are apparent to those skilled in the art without the benefit of this disclosure, are intended to be included within the scope of this invention.
Examples
As shown in fig. 1, the steps for preparing the horizontal array carbon nanotubes in this embodiment include:
s1, preparing experimental equipment;
the experimental facilities that need to be prepared are: a reaction vessel and a discharge device.
S2, preparing experimental raw materials;
the experimental raw materials to be prepared are as follows:
an anode and a cathode; the anode is a graphite carbon rod with the diameter of 10 mm; the cathode is a graphite carbon rod with a shallow groove, and a small amount of iron is filled in the shallow groove.
The anode and cathode mounting steps are as follows:
a1, placing an anode and a cathode at the central position of a reaction container;
a2, connecting the anode and the cathode with the discharge equipment correspondingly.
The mounting modes of the anode and the cathode are as follows:
the anode and the cathode are mutually perpendicular; the anode is at the top and the cathode is at the bottom.
S3, adding mixed gas;
the mixed gas to be added is as follows:
methane, argon.
Wherein methane is added to the reaction vessel at 13.33 kPa; argon must be added to the reaction vessel at 53.32 Pa.
S4, electrifying;
starting a discharge device, electrifying an anode and a cathode, melting iron in the shallow groove to form small liquid drops, and then evaporating to serve as a catalyst; the discharge device had a voltage of 20V and a current of 200A.
S5, monitoring experimental conditions;
the monitoring of the experimental conditions in S5 is specifically as follows:
the device is respectively provided with methane pressure detection equipment, argon pressure detection equipment and voltage and current detection equipment;
the device comprises a methane pressure detection device, an argon gas pressure detection device, a voltage and current detection device and a discharge device, wherein the methane pressure detection device is used for detecting the pressure of methane, the argon gas pressure detection device is used for detecting the pressure of argon, and the voltage and current detection device is used for detecting the voltage and current of the discharge device;
the methane pressure detection equipment, the argon gas pressure detection equipment and the voltage and current detection equipment are respectively and electrically connected with the data equipment, the display screen and the alarm equipment.
The detection steps of the methane gas pressure detection equipment are as follows:
a1, detecting methane added into a reaction container by methane pressure detection equipment and sending detected data to data equipment;
a2, reasonable data are built in the data equipment, the specific data value of the data equipment is that the air pressure of methane is 13.33kPa, the data equipment can compare the reasonable data 13.33kPa with the methane pressure data after receiving the methane pressure data, if the comparison data are inconsistent, the data equipment can send a comparison result to a display screen for experimenters to refer, meanwhile, the data equipment can also send a signal to an alarm device, and the alarm device gives an alarm, so that the experimenters are reminded of abnormal methane pressure.
The detection steps of the argon gas pressure detection equipment are as follows:
a1, an argon gas pressure detection device detects argon gas added into a reaction container and sends detected data to a data device;
a2, reasonable data are built in the data equipment, the specific data value is 53.32Pa of argon gas pressure, the data equipment can compare the reasonable data 53.32Pa with the argon gas pressure data after receiving the argon gas pressure data, if the comparison data are inconsistent, the data equipment can send a comparison result to a display screen for experimenters to refer to, meanwhile, the data equipment can also send a signal to an alarm device, and the alarm device gives an alarm, so that the experimenters are reminded of abnormal argon gas pressure.
The detection steps of the voltage and current detection equipment are as follows:
a1, the voltage and current detection equipment detects the voltage and current in the discharge equipment and sends detected data to the data equipment;
a2, the data equipment is internally provided with reasonable data, the specific data value of the data equipment is current 200A and voltage 20V, the reasonable data can be compared with the voltage and current data of the discharge equipment at the moment after the data equipment receives the voltage and current data, if the comparison data are inconsistent, the data equipment can send a comparison result to a display screen for experimenters to refer to, meanwhile, the data equipment can also send a signal to alarm equipment, and the alarm equipment gives an alarm, so that the experimenters are reminded of abnormal discharge equipment.
S6, adjusting experimental conditions;
the experimenter can adjust the pressure of methane, the pressure of argon and the voltage and current of the discharge equipment according to the display screen, so that the normal data value can be met.
S7, observing;
the viewing device required to be used is a transmission electron microscope. As shown in FIGS. 2 and 3, the anode product was observed under a transmission electron microscope, and found that the product was mostly clustered into bundles, each bundle consisting of several single-walled tubes with diameters of 0.7-1.6 nm, and a small number of single-walled carbon nanotubes could be observed.
S8, cleaning experimental equipment.
After the preparation of the carbon nano tube is finished, the reaction vessel needs to be cleaned, so that the influence of impurities in the reaction vessel on the next preparation work of the carbon nano tube is avoided.
The invention is characterized in that an anode and a cathode are placed in a reaction container, the anode and the cathode are mutually vertical, the anode and the cathode are correspondingly connected with a discharge device, methane and argon are added into the reaction container, the discharge device is started, the anode and the cathode are electrified, iron in a shallow groove is melted to form small liquid drops, then the small liquid drops are evaporated to serve as a catalyst, an anode product is observed under a transmission electron microscope, most of the product is clustered, each cluster is formed by a plurality of single-layer tubes with the diameter of 0.7-1.6 nm, a small quantity of single-wall carbon nanotubes can be observed, and the preparation work of the carbon nanotubes is completed. Compared with the prior art, the method has the advantages that less equipment is used when the carbon nano tube is prepared, and the preparation process is simple, so that the preparation cost of the carbon nano tube is reduced.
According to the invention, methane added into the reaction container is detected through the methane pressure detection equipment, detected data are sent to the data equipment, reasonable data are arranged in the data equipment, the specific data value is that the methane pressure is 13.33kPa, the data equipment can compare the reasonable data 13.33kPa with the methane pressure data after receiving the methane pressure data, if the comparison data are inconsistent, the data equipment can send a comparison result to the display screen for reference of experimenters, meanwhile, the data equipment can also send a signal to the alarm equipment, and the alarm equipment sends an alarm, so that the experimenters are reminded that the methane pressure is abnormal.
The argon gas pressure detection equipment can detect the argon gas added into the reaction container and send detected data to the data equipment, the data equipment is internally provided with reasonable data, the specific data value of the data is 53.32Pa, the data equipment can compare the reasonable data 53.32Pa with the argon gas pressure data after receiving the argon gas pressure data, if the comparison data are inconsistent, the data equipment can send a comparison result to a display screen for reference of experimental staff, meanwhile, the data equipment can also send a signal to the alarm equipment, and the alarm equipment sends an alarm to remind the experimental staff that the argon gas pressure is abnormal.
The voltage and current detection equipment detects the voltage and current in the discharge equipment and sends the detected data to the data equipment, the data equipment is internally provided with reasonable data, the specific data value is 200A and 20V, the reasonable data is compared with the voltage and current data of the discharge equipment when the data equipment receives the voltage and current data, if the comparison data are inconsistent, the data equipment sends a comparison result to a display screen for reference of experiment personnel, meanwhile, the data equipment also sends a signal to the alarm equipment, and the alarm equipment sends an alarm to remind the experiment personnel of abnormal discharge equipment.
Claims (6)
1. The preparation method of the horizontal array carbon nano tube is characterized by comprising the following steps of:
1) Selecting graphite columns as an anode and a cathode, and forming shallow grooves on the side wall of the cathode;
2) The shallow groove of the cathode is filled with a catalyst, the cathode and the anode are horizontally arranged in a closed reaction container, the anode is positioned above the cathode, and the cathode and the anode are connected with a discharge device;
3) After the reaction vessel is vacuumized, sequentially adding methane and argon into the reaction vessel;
4) And electrifying to react, and collecting the carbon nano tubes in the reaction container to obtain the horizontal array.
2. The method for preparing the horizontal array carbon nanotube according to claim 1, wherein: in the step 2), the catalyst is elemental iron.
3. The method for preparing the horizontal array carbon nanotube according to claim 1, wherein: in the step 2), the cathode and the anode are vertically arranged.
4. The method for preparing the horizontal array carbon nanotube according to claim 1, wherein: in step 3), methane was added to the reaction vessel at 13.33 kPa.
5. The method for preparing the horizontal array carbon nanotube according to claim 1, wherein: in step 3), argon was added to the reaction vessel at 53.32 Pa.
6. The method for preparing the horizontal array carbon nanotube according to claim 1, wherein: in the step 4), the condition of the electrifying reaction is that the current is 200A and the voltage is 20V.
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| CN202310402166.5A CN116425145A (en) | 2023-04-13 | 2023-04-13 | Preparation method of horizontal array carbon nano tube |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1579931A (en) * | 2004-05-17 | 2005-02-16 | 西安交通大学 | Method for batch type production of single-wall nano carbon tube suing temperature-controlled electric arc furnace |
| CN1987443A (en) * | 2006-11-27 | 2007-06-27 | 西南交通大学 | Method for preparing in-situ growing carbon nano tube chemical decoration electrode |
| CN103241725A (en) * | 2013-05-09 | 2013-08-14 | 中国石油大学(北京) | Method for preparing carbon nano tube by taking coke as raw material and prepared carbon nano tube |
| CN110217777A (en) * | 2019-06-19 | 2019-09-10 | 江西铜业技术研究院有限公司 | A kind of carbon nanotube preparing apparatus and method |
| CN112174113A (en) * | 2020-10-14 | 2021-01-05 | 宁波中乌新材料产业技术研究院有限公司 | Preparation method of bamboo-joint-type carbon nano tube |
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- 2023-04-13 CN CN202310402166.5A patent/CN116425145A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1579931A (en) * | 2004-05-17 | 2005-02-16 | 西安交通大学 | Method for batch type production of single-wall nano carbon tube suing temperature-controlled electric arc furnace |
| CN1987443A (en) * | 2006-11-27 | 2007-06-27 | 西南交通大学 | Method for preparing in-situ growing carbon nano tube chemical decoration electrode |
| CN103241725A (en) * | 2013-05-09 | 2013-08-14 | 中国石油大学(北京) | Method for preparing carbon nano tube by taking coke as raw material and prepared carbon nano tube |
| CN110217777A (en) * | 2019-06-19 | 2019-09-10 | 江西铜业技术研究院有限公司 | A kind of carbon nanotube preparing apparatus and method |
| CN112174113A (en) * | 2020-10-14 | 2021-01-05 | 宁波中乌新材料产业技术研究院有限公司 | Preparation method of bamboo-joint-type carbon nano tube |
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