CN109748261A - The continuous preparation method and preparation facilities of carbon nano pipe array - Google Patents

The continuous preparation method and preparation facilities of carbon nano pipe array Download PDF

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Publication number
CN109748261A
CN109748261A CN201910228712.1A CN201910228712A CN109748261A CN 109748261 A CN109748261 A CN 109748261A CN 201910228712 A CN201910228712 A CN 201910228712A CN 109748261 A CN109748261 A CN 109748261A
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CN
China
Prior art keywords
carbon nano
pipe array
nano pipe
substrate
heating sheet
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Pending
Application number
CN201910228712.1A
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Chinese (zh)
Inventor
高建超
马春印
李文康
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Shenzhen Meishan Energy Technology Co Ltd
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Shenzhen Meishan Energy Technology Co Ltd
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Priority to CN201910228712.1A priority Critical patent/CN109748261A/en
Publication of CN109748261A publication Critical patent/CN109748261A/en
Pending legal-status Critical Current

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Abstract

The present invention relates to the continuous preparation method technical fields of carbon nano pipe array, refer in particular to the continuous preparation method and preparation facilities of carbon nano pipe array;1) preparation method is the following steps are included: provide a growing carrier, surface sputters one layer of catalyst layer on this carrier, and catalyst is nanometer iron ion;2) substrate of one layer of catalyst is placed on heating sheet upper surface sputtering;3) start computer heating control power supply, directly substrate is heated using heating sheet as heating device;4) carrier gas and carbon source gas are passed through;5) it along gas flow direction, draws carrier and passes sequentially through heating sheet;6) by adjusting hauling speed, the carbon nano pipe array of different length is produced;7) after the growth for completing carbon nano pipe array, power supply is closed, takes out product.The present invention allows continuous production, and does not need replacement substrate, and production efficiency and product quality can be improved.

Description

The continuous preparation method and preparation facilities of carbon nano pipe array
Technical field
The present invention relates to the continuous preparation method technical fields of carbon nano pipe array, refer in particular to the continuous system of carbon nano pipe array Preparation Method and preparation facilities.
Background technique
Due to the performance that carbon nano pipe array is excellent, make it that there is more extensive application prospect, from synthesis, Global scientific research personnel, which expands, largely to study and attempts to be applied to various fields.But it is constrained to high-volume carbon nanotube The wide application of the preparation of array, carbon nano pipe array does not occur.More than ten years in past, people have paid the effort gram of hardships The shortcomings that taking conventional chemical vapor sedimentation, to realize the industrialized production of carbon nano pipe array, for example, passing through replacement substrate Method, continuous production carbon nano pipe array.But substrate is replaced in high temperature furnace still certain difficulty.
Therefore, the defect of the continuous preparation method based on above-mentioned existing carbon nano pipe array needs to receive existing carbon The continuous preparation method of mitron array improves.
Summary of the invention
The purpose of the present invention is to solve the shortcomings of the prior art providing the continuous preparation method of carbon nano pipe array, the system Preparation Method solves present in existing preparation method: being unable to quantity-produced defect.
To achieve the above object, the present invention is achieved by the following technical solutions: the continuous preparation of carbon nano pipe array Method, comprising the following steps:
1) growing carrier is provided, surface sputters one layer of catalyst layer on this carrier, and catalyst is nanometer iron ion;
2) substrate of one layer of catalyst is placed on heating sheet upper surface sputtering;
3) start computer heating control power supply, directly substrate is heated using heating sheet as heating device;
4) carrier gas and carbon source gas are passed through;
5) it along gas flow direction, draws carrier and passes sequentially through heating sheet;
6) by adjusting hauling speed, the carbon nano pipe array of different length is produced;
7) after the growth for completing carbon nano pipe array, power supply is closed, takes out product.
The substrate is silicon wafer, sheet metal or other graphite shoestring.
The catalyst is nano-iron particle.
The carrier gas is the gaseous mixture or inert gas of nitrogen and hydrogen and the gaseous mixture or argon gas and hydrogen of hydrogen Gaseous mixture.
The carbon source is methane, ethylene or acetylene.
The preparation facilities of carbon nano pipe array, including glass reaction chamber, glass reaction chamber is interior to have the heating for placing substrate Piece, is furnished with microcell heater outside glass reaction chamber, and microcell heater is electrically connected heating sheet, glass reaction chamber also have air inlet pipe, Escape pipe also has the traction pump for drawing substrate in glass reaction chamber.
Microcell heater has step-up/step-down circuit and control circuit using 48V power supply;Heating sheet is silicon wafer;Glass tube is Quartz ampoule.
The beneficial effects of the present invention are: it allows continuous production, and does not need replacement substrate, production can be improved Efficiency and product quality.
Detailed description of the invention
Fig. 1 is preparation facilities schematic diagram of the invention.
Fig. 2 is the carbon nano pipe array that hauling speed of the invention is 3mm/min growth.
Fig. 3 is the transmission electron microscope picture of carbon nano pipe array of the invention.
Label title of the invention is as follows: microcell heater 1, glass reaction chamber 2, gas 3, on heating sheet 4, substrate 5.
Specific embodiment
The present invention will be further described below with reference to the drawings.
Embodiment 1:
As shown in Figure 1, the present invention provides a kind of continuous method grown of carbon nano pipe array, comprising:
In glass reaction chamber 2, a strip plating iron substrate 5 is placed on the heating sheet 4 of microcell heater 1 first;It is passed through The mixed gas 3 of argon gas, hydrogen and acetylene, gas flow are respectively 560 ml/mins, 200 ml/mins and 30 ml/mins Clock;After steady air current, start microcell computer heating control power supply, growth temperature needed for heating sheet is rapidly brought up to carbon nano pipe array Degree;It is slided on silicon heating sheet with traction pump traction plating iron substrate 5 along airflow direction;When plating iron substrate slides on heating sheet When, carbon nano pipe array starts to grow, and controls certain sliding speed, the carbon nano pipe array of available different height.Instead After answering, microcell heater is closed, surface is taken out and tested with the substrate of carbon nano pipe array.In the present embodiment, Heating sheet is silicon wafer, having a size of 2cm × 0.75cm × 0.05cm, meanwhile, use silicon wafer as substrate, in its shiny surface, magnetic control splashes One layer of 2nm simple substance iron layer is penetrated, the sputtering rate of iron layer is 0.029nm/s, and hauling speed is 3 mm/mins.
Shown in Fig. 2, hauling speed is the carbon nano pipe array of 3 mm/mins growth, and a in Fig. 2, b, c are respectively difference The scanning electron microscope (SEM) photograph of position carbon nano pipe array.
Embodiment 2:
In glass reaction chamber, a strip plating iron substrate is placed on the heating sheet of microcell heater first;Be passed through argon gas, Hydrogen and acetylene, gas flow are respectively 190 ml/mins, 70 ml/mins and 10 ml/mins;After steady air current, Start 1 power supply of microcell heater, growth temperature needed for heating sheet is rapidly brought up to carbon nano pipe array;Plating iron is drawn with traction pump Substrate slides on heating sheet along airflow direction;When plating iron substrate slides on heating sheet, carbon nano pipe array starts to give birth to It is long, control certain sliding speed, the carbon nano pipe array of available different height.After reaction, microcell heating is closed Device takes out on surface with the substrate of carbon nano pipe array.In the present embodiment, heating sheet is silicon wafer, having a size of 2cm × 0.75cm × 0.05cm, meanwhile, use graphite flake as substrate, in its shiny surface, one layer of 2nm simple substance iron layer of magnetron sputtering, traction Speed is 2 mm/mins.
Embodiment 3:
In glass reaction chamber, a strip plating iron substrate is placed on the heating sheet of microcell heater first;Be passed through argon gas, Hydrogen and methane, gas flow are respectively 560 ml/mins, 200 ml/mins and 20 ml/mins;After steady air current, Start microcell heater, growth temperature needed for heating sheet is rapidly brought up to carbon nano pipe array;Plating iron substrate is drawn with traction pump It is slided on heating sheet along airflow direction;When plating iron substrate slides on heating sheet, carbon nano pipe array starts to grow, control Make certain sliding speed, the carbon nano pipe array of available different height.After reaction, microcell heater is closed, it will It is taken out with the substrate of carbon nano pipe array on surface.In the present embodiment, heating sheet is silicon wafer, having a size of 4cm × 1cm × 0.05cm, meanwhile, use silicon wafer as substrate, in its shiny surface, one layer of 2nm simple substance iron layer of magnetron sputtering, hauling speed is 3 millis M/min.
Preparation method of the invention is simple, solves the problems, such as that carbon nano pipe array is continuously grown, and improves carbon nano-pipe array The speed of growth of column.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details and legend shown and described herein.

Claims (6)

1. the continuous preparation method of carbon nano pipe array, it is characterised in that: the following steps are included:
1) growing carrier is provided, surface sputters one layer of catalyst layer on this carrier, and catalyst is nanometer iron ion;
2) substrate of one layer of catalyst is placed on heating sheet upper surface sputtering;
3) start computer heating control power supply, directly substrate is heated using heating sheet as heating device;
4) carrier gas and carbon source gas are passed through;
5) it along gas flow direction, draws carrier and passes sequentially through heating sheet;
6) by adjusting hauling speed, the carbon nano pipe array of different length is produced;
7) after the growth for completing carbon nano pipe array, power supply is closed, takes out product.
2. the continuous preparation method of carbon nano pipe array according to claim 1, it is characterised in that: the substrate is silicon Piece, sheet metal or other graphite shoestring.
3. the continuous preparation method of carbon nano pipe array according to claim 1, it is characterised in that: the catalyst is Nano-iron particle.
4. the continuous preparation method of carbon nano pipe array according to claim 1, it is characterised in that: the carrier gas is nitrogen The gaseous mixture of the gaseous mixture or inert gas of gas and hydrogen and the gaseous mixture or argon gas of hydrogen and hydrogen.
5. the continuous preparation method of carbon nano pipe array according to claim 1, it is characterised in that: the carbon source is first Alkane, ethylene or acetylene.
6. the preparation facilities of carbon nano pipe array, it is characterised in that: including glass reaction chamber, have in glass reaction chamber and place base The heating sheet at bottom, glass reaction chamber are furnished with microcell heater outside, and microcell heater is electrically connected heating sheet, and glass reaction chamber also has Air inlet pipe, escape pipe also have the traction pump for drawing substrate in glass reaction chamber.
CN201910228712.1A 2019-03-25 2019-03-25 The continuous preparation method and preparation facilities of carbon nano pipe array Pending CN109748261A (en)

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Application Number Priority Date Filing Date Title
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101372327A (en) * 2008-09-26 2009-02-25 厦门大学 Growth method of carbon nano-tube array
CN102388171A (en) * 2009-04-10 2012-03-21 应用纳米结构方案公司 Apparatus and method for the production of carbon nanotubes on a continuously moving substrate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101372327A (en) * 2008-09-26 2009-02-25 厦门大学 Growth method of carbon nano-tube array
CN102388171A (en) * 2009-04-10 2012-03-21 应用纳米结构方案公司 Apparatus and method for the production of carbon nanotubes on a continuously moving substrate

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