CN109734075A - A method of carbon nano pipe array is prepared using solution catalyst - Google Patents
A method of carbon nano pipe array is prepared using solution catalyst Download PDFInfo
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- CN109734075A CN109734075A CN201910226660.4A CN201910226660A CN109734075A CN 109734075 A CN109734075 A CN 109734075A CN 201910226660 A CN201910226660 A CN 201910226660A CN 109734075 A CN109734075 A CN 109734075A
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Abstract
The invention discloses a kind of methods for preparing carbon nano pipe array using solution catalyst.One smooth substrate is put into plasma generator, hydrophilic treated is carried out with plasma to the surface of smooth substrate；Then after substrate being taken out, match the catalyst solution postponed in the drop of surface, then uniform with sol evenning machine spin coating；Substrate is put into reaction chamber after finally drying and is passed through reaction gas and grows carbon nano pipe array from substrate using chemical vapour deposition technique under the conditions of certain temperature.The carbon nano pipe array surface that the method for the present invention is prepared is completely smooth, and superficial density is high, and process is simple, and preparation cost is very low, is suitble to industrial volume production.
Description
Technical field
The present invention relates to a kind of methods for preparing aligned carbon-nanotubes, use solution spin coating more particularly, to a kind of
Carbon nano pipe array preparation method of the method as catalyst.
Background technique
Due to the unique electricity and heat property of carbon nanotube, have in fields such as Nanometer integrated circuit, single molecules apparatus
This wide application prospect.Prepare the method for carbon nanotube comparative maturity, large area carbon nanotube in the lab at present
There has also been remarkable progress for the synthesis of array.But in the large-scale industrial production of demand low cost, current preparation method still has
It is insufficient.
The main method of preparation carbon nanotube mainly has arc discharge method, pulse laser evaporation and chemical vapor deposition at present
Area method etc..But these preparation methods are primarily present following several disadvantages: (1) low output, are not suitable for industrial production；(2) cost
It is high；(3) the bad control of the direction of growth, it is difficult to industrially apply.
Wherein solid catalyst is prepared by magnetron sputtering or electron beam evaporation method, and which greatly enhances production costs.
It the use of liquid catalyst is mostly to use ferrocene, liquid catalyst is easy to distillation volatilization, it is difficult to rest on substrate surface.
Summary of the invention
In order to solve the problems, such as background technique, the invention proposes a kind of preparation method of carbon nano pipe array,
It grows simultaneously in substrate upper and lower surface, and the carbon nano pipe array surface grown is completely smooth, strong with substrate caking power, and makes
Standby cost is very low.
The technical solution adopted by the present invention is that:
The method of the present invention is the following steps are included: be put into the table in plasma generator to smooth substrate for a smooth substrate
Face carries out hydrophilic treated with plasma；Then after substrate being taken out, with the catalyst solution that postpones in the drop of surface, then with even
Glue machine spin coating is uniform；Substrate is put into reaction chamber after finally drying and is passed through reaction gas under the conditions of certain temperature using chemistry
Vapour deposition process grows carbon nano pipe array from substrate.
The smooth substrate is silicon wafer, and the plasma power to silicon chip surface hydrophilic treated is 50W.
The catalyst solution is ferric chloride solution, concentration 0.8-1.2mol/L；Spin coating process is 1000r/
Min, the time 1 minute.
The chemical vapour deposition technique is plasma chemical vapor deposition, and certain temperature condition is that 580-620 is Celsius
Temperature is spent, the plasma power of plasma chemical vapor deposition is 150W, the pressure of plasma chemical vapor deposition
Strong range is 300-330Pa.
The reaction gas is the mixed gas of carbon source gas and carrier gas, and the carbon source gas is acetylene, and the carrier gas is hydrogen
The mixed gas of gas and argon gas.
The gas flow is respectively argon gas 200SCCM, hydrogen 60SCCM, acetylene 20SCCM.
It is passed through reaction gas in the reaction chamber, specifically: the argon gas of 200sccm, discharge are first passed through into reaction chamber
Then air in reaction chamber starts to warm up and is passed through the hydrogen of 60sccm simultaneously as reducibility gas, when temperature reaches temperature
Argon gas is closed after 580-620 degrees Celsius of degree, the acetylene gas of 20sccm is passed through as carbon source gas, opens simultaneously plasma.
After the present invention prepares catalyst coat using the method for solution of ferrous chloride method spin coating, plasma chemistry gas is used
Phase deposition growing carbon nano pipe array.
The beneficial effects of the present invention are:
Existing method provides catalyst source gas or growth catalyst layer, these method costs using spraying, sputtering method
Height, complex procedures.
Compared with prior art, the method and process provided by the invention for preparing carbon nano pipe array is simple, carbon nano-pipe array
List face is completely smooth, and cost is very low, easily operated, and the carbon nano pipe array pattern quality and conventional method phase grown
Closely, it is suitble to large-scale industrial production.
Detailed description of the invention
Fig. 1-Fig. 2 is the SEM figure of carbon nano pipe array made of embodiment 1 under a scanning electron microscope；
Fig. 3 is the SEM figure of carbon nano pipe array made of embodiment 2 under a scanning electron microscope.
Specific embodiment
The embodiment of the present invention will be described in further detail with reference to the accompanying drawing.
The embodiment of the present invention is as follows:
Embodiment 1
There is provided a smooth silicon wafer substrate, surface smoothness is less than 300 nanometers, so that subsequent carbon nano tube growth is with urging
Agent layer can be uniformly adhered to substrate surface.
A catalyst layer is formed on the smooth substrate surface, catalyst layer is uniformly applied to substrate by solution spin-coating method
Surface, then drying is made.Solution uses ferric chloride in aqueous solution, concentration 0.8mol/L.After solution drop is entreated in the substrate
With sol evenning machine spin coating, speed of rotation 1000r/min, the time is 1 minute.After smearing uniformly, substrate is placed in 200 degrees Celsius
It is dried on drying table.
The silicon wafer substrate for being formed with catalyst layer is placed into reaction chamber, reaction gas is passed through in reaction chamber, predetermined
Using plasma chemical vapour deposition technique makes carbon nano-pipe array be listed in substrate surface to grow under the conditions of temperature, specifically: it is first past
It is passed through the argon gas of 200sccm in reaction chamber five minutes, the air in chamber is discharged, then starts to warm up, while being passed through 60sccm's
Hydrogen is as reducibility gas.After temperature reaches 620 degrees Celsius of predetermined temperature, argon gas is closed, the acetylene gas of 20sccm is passed through
Body opens simultaneously plasma as carbon source gas.Plasma power is 150W, and intracavitary air pressure maintains 330Pa or so, and carbon is received
The mitron array growth time is 40 minutes.
In the present embodiment control reaction gas in the flow-ratio control of carbon source gas and carrier gas near 1:3.In this carbon
The carbon nano pipe array pattern grown under source gas concentration is best.
The present embodiment is tested by SEM, and carbon nano pipe array pattern is as depicted in figs. 1 and 2.It can be seen that from SEM figure
The carbon nano pipe array of solution catalyst method preparation of the present invention is very compact uniform, and carbon nanotube is collapsed almost without bending.It is raw
Long length of carbon nanotube reaches 32.6 microns, and same length.
Embodiment 2
There is provided a smooth silicon wafer substrate, surface smoothness is less than 300 nanometers, so that subsequent carbon nano tube growth is with urging
Agent layer can be uniformly adhered to substrate surface.
A catalyst layer is formed on the smooth substrate surface, catalyst layer is uniformly applied to substrate by solution spin-coating method
Surface, then drying is made.Solution uses ferric chloride in aqueous solution, concentration 1.2mol/L.After solution drop is entreated in the substrate
With sol evenning machine spin coating, speed of rotation 1000r/min, the time is 1 minute.After smearing uniformly, substrate is placed in 200 degrees Celsius
It is dried on drying table.
The silicon wafer substrate for being formed with catalyst layer is placed into reaction chamber, reaction gas is passed through in reaction chamber, predetermined
Using plasma chemical vapour deposition technique makes carbon nano-pipe array be listed in substrate surface to grow under the conditions of temperature, specifically: it is first past
It is passed through the argon gas of 200sccm in reaction chamber five minutes, the air in chamber is discharged, then starts to warm up, while being passed through 60sccm's
Hydrogen is as reducibility gas.After temperature reaches 620 degrees Celsius of predetermined temperature, argon gas is closed, the acetylene gas of 20sccm is passed through
Body opens simultaneously plasma as carbon source gas.Plasma power is 150W, and intracavitary air pressure maintains 330Pa or so, and carbon is received
The mitron array growth time is 40 minutes.
In the present embodiment control reaction gas in the flow-ratio control of carbon source gas and carrier gas near 1:3.In this carbon
The carbon nano pipe array pattern grown under source gas concentration is best.
The present embodiment is tested by SEM, and carbon nano pipe array pattern is as shown in Figure 3.As can be seen that this hair from SEM figure
The carbon nano pipe array of bright solution catalyst method preparation is very compact uniform, and carbon nanotube is collapsed almost without bending.Growth
Length of carbon nanotube reaches 34 microns, and same length.
Solution spin-coating method provided by the invention prepares the catalyst for growing carbon nano pipe array, splashes relative to traditional
Sedimentation and spray-on process are penetrated, process is simple, without using expensive equipment.And the catalyst that the embodiment of the present invention uses is molten
Liquid is solution of ferrous chloride, extremely cheap, and waste is few in use, this just considerably reduces production cost.
Therefore the method provided by the invention for preparing carbon nano pipe array using solution catalyst has inexpensive, efficient
Rate, easily operated and simple process advantage, are suitably applied large-scale industrial production.
Above-mentioned specific embodiment is used to illustrate the present invention, rather than limits the invention, of the invention
In spirit and scope of protection of the claims, to any modifications and changes that the present invention makes, protection model of the invention is both fallen within
It encloses.
Claims (7)
1. a kind of method for preparing carbon nano pipe array using solution catalyst, it is characterised in that: method will be the following steps are included: will
One smooth substrate, which is put into plasma generator, carries out hydrophilic treated with plasma to the surface of smooth substrate；Then base
After bottom is taken out, match the catalyst solution postponed in the drop of surface, then uniform with sol evenning machine spin coating；Substrate is put into after finally drying
Reaction gas is passed through in reaction chamber makes carbon nano pipe array from substrate under the conditions of certain temperature using chemical vapour deposition technique
It grows.
2. a kind of method for preparing carbon nano pipe array using solution catalyst according to claim 1, it is characterised in that:
The smooth substrate is silicon wafer, and the plasma power to silicon chip surface hydrophilic treated is 50W.
3. a kind of method for preparing carbon nano pipe array using solution catalyst according to claim 1, it is characterised in that:
The catalyst solution is ferric chloride solution, concentration 0.8-1.2mol/L；Spin coating process is 1000r/min, and the time 1 divides
Clock.
4. a kind of method for preparing carbon nano pipe array using solution catalyst according to claim 1, it is characterised in that:
The chemical vapour deposition technique is plasma chemical vapor deposition, and certain temperature condition is 580-620 degree celsius temperature, etc.
The plasma power of gas ions chemical vapour deposition technique is 150W, and the pressure range of plasma chemical vapor deposition is
300-330Pa。
5. a kind of method for preparing carbon nano pipe array using solution catalyst according to claim 1, it is characterised in that:
The reaction gas is the mixed gas of carbon source gas and carrier gas, and the carbon source gas is acetylene, and the carrier gas is hydrogen and argon gas
Mixed gas.
6. a kind of method for preparing carbon nano pipe array using solution catalyst according to claim 1, it is characterised in that:
The gas flow is respectively argon gas 200SCCM, hydrogen 60SCCM, acetylene 20SCCM.
7. a kind of method for preparing carbon nano pipe array using solution catalyst according to claim 1, it is characterised in that:
It is passed through reaction gas in the reaction chamber, specifically: it is first passed through the argon gas of 200sccm into reaction chamber, is discharged in reaction chamber
Air, then start to warm up and be passed through simultaneously the hydrogen of 60sccm, close argon after temperature reaches 580-620 degrees Celsius of temperature
Gas is passed through the acetylene gas of 20sccm as carbon source gas, opens simultaneously plasma.
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| CN201910226660.4A CN109734075A (en) | 2019-03-25 | 2019-03-25 | A method of carbon nano pipe array is prepared using solution catalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113788474A (en) * | 2021-11-04 | 2021-12-14 | 航天特种材料及工艺技术研究所 | Graphene nanoribbon horizontal array and preparation method and application thereof |
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| US20030064169A1 (en) * | 2001-09-28 | 2003-04-03 | Hong Jin Pyo | Plasma enhanced chemical vapor deposition apparatus and method of producing carbon nanotube using the same |
| CN1919728A (en) * | 2006-09-18 | 2007-02-28 | 北京大学 | Preparation method of reducing single-wall carbon nano-tube |
| CN1978315A (en) * | 2005-12-09 | 2007-06-13 | 清华大学 | Method for preparing carbon nano tube array |
| CN101077773A (en) * | 2007-06-15 | 2007-11-28 | 清华大学 | Method for preparing carbon nano-tube array on the basis of chemical vapour deposition |
| CN102320591A (en) * | 2011-06-22 | 2012-01-18 | 天津大学 | Method for directly growing mesh carbon nanotubes on copper substrate |
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2019
- 2019-03-25 CN CN201910226660.4A patent/CN109734075A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030064169A1 (en) * | 2001-09-28 | 2003-04-03 | Hong Jin Pyo | Plasma enhanced chemical vapor deposition apparatus and method of producing carbon nanotube using the same |
| CN1978315A (en) * | 2005-12-09 | 2007-06-13 | 清华大学 | Method for preparing carbon nano tube array |
| CN1919728A (en) * | 2006-09-18 | 2007-02-28 | 北京大学 | Preparation method of reducing single-wall carbon nano-tube |
| CN101077773A (en) * | 2007-06-15 | 2007-11-28 | 清华大学 | Method for preparing carbon nano-tube array on the basis of chemical vapour deposition |
| CN102320591A (en) * | 2011-06-22 | 2012-01-18 | 天津大学 | Method for directly growing mesh carbon nanotubes on copper substrate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113788474A (en) * | 2021-11-04 | 2021-12-14 | 航天特种材料及工艺技术研究所 | Graphene nanoribbon horizontal array and preparation method and application thereof |
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