CN103086406A - Preparation method of magnesium oxide nanobelt-carbon nanotube composite material - Google Patents

Preparation method of magnesium oxide nanobelt-carbon nanotube composite material Download PDF

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CN103086406A
CN103086406A CN2013100300482A CN201310030048A CN103086406A CN 103086406 A CN103086406 A CN 103086406A CN 2013100300482 A CN2013100300482 A CN 2013100300482A CN 201310030048 A CN201310030048 A CN 201310030048A CN 103086406 A CN103086406 A CN 103086406A
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preparation
mgo
nanobelts
nitrate hexahydrate
carbon nano
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李明吉
王秀锋
李红姬
狄海荣
曲长庆
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Tianjin University of Technology
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Tianjin University of Technology
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Abstract

The invention relates to a preparation method of a magnesium oxide nanobelt-carbon nanotube composite material. The preparation method comprises the following steps of: dissolving magnesium nitrate hexahydrate and nickel nitrate hexahydrate in ethanol as a precursor for catalyzing the growth of a magnesium oxide nanobelt-carbon nanotube composite material; uniformly dripping and coating a mixed solution on a substrate, drying under an infrared lamp, placing on a deposition platform in a direct current plasma jet CVD (chemical vapor deposition) chamber, introducing argon and hydrogen, starting arc initiation, performing heating decomposition under the action of plasma to form NiO and MgO, and reducing the NiO to Ni nano-metal particles under the action of the plasma to obtain an Ni-MgO catalytic system; and introducing gas of a carbon source, and growing the magnesium nanobelt-carbon nanotube composite material in a plasma atmosphere. The preparation method disclosed by the invention has the advantages of simple preparation process, high efficiency, low energy consumption, low cost, huge industrial batch production potential and wide application prospects in light, electricity, magnetic and chemical fields, such as catalysts, biochemical sensors, microwave absorption and the like.

Description

A kind of preparation method of MgO nanobelts-carbon nano tube compound material
Technical field
The present invention relates to the preparation method of the preparation of metal oxide composite, particularly a kind of MgO nanobelts-carbon nano tube compound material.
Background technology
Since 1991, since Iijima prepares carbon nanotube, owing to having unique mechanics, calorifics and electric property, the aspects such as toughener of line, photoconductive fiber and the matrix material of its needle point at scanning tunnel microscope, nano-device and super large-scale integration are had broad application prospects.
MgO is as the broad-band gap isolator, characteristics with high-melting-point (approximately 2830 ℃) and low heat capacity, high secondary electron emission field has a wide range of applications in the photoelectricity such as plasmadisplay panel (PDP), Photoelectrochemistry, metal-oxide semiconductor (MOS) grid controllable devices and high-temperature superconductor mixing material sustainable field.After size is refined to nanometer scale, because of the peculiar volume effect of nano material and surface effects, the bitter earth nano material presents many heat, light, electricity, mechanics and chemical propertys that are different from bulk material at low-temperature sintering, microwave absorbing, catalytic performance etc. aspect numerous.Therefore, the MgO nano material also can have broad application prospects at aspects such as electrochemica biological sensor, sterilant, refractory materialss.In recent years, the preparation method of many MgO nano belt is proposed in succession, for example: adopt simple CVD method Infrared Heating Mg/Al target, finally synthesized netted MgO nano belt on the Si substrate; Adopt simple thermal evaporation, high-purity magnesium powder thermostatically heating (650 ℃) in Ar/O2 atmosphere was obtained wire MgO nano belt in one hour; Take prefabricated ZnO nano-band as template and Mg steam generation replacement(metathesis)reaction (650 ℃) obtain the MgO nano belt.But these methods exist complex process, and efficient is low, and energy consumption is high, and high in cost of production is not enough.
The researchs such as Maldonado-Hodar are found can embody well collaborative or cooperative effect between metal oxide and carbon are mutually, these characteristics make CNTs be applied in metal oxide composite, can well improve the various performances of matrix material, to reach the purpose of combination among the strong ones.
Summary of the invention
The object of the invention is to provides a kind of preparation method of MgO nanobelts-carbon nano tube compound material for above technical Analysis, and the method technique is simple, efficient is high, cost is low, be expected to realize the industrialization volume production.
Technical solution of the present invention:
A kind of preparation method of MgO nanobelts-carbon nano tube compound material adopts the preparation of DC arc plasma jet CVD system, and step is as follows:
1) Nickelous nitrate hexahydrate and magnesium nitrate hexahydrate are dissolved in ethanol, make mixing solutions as catalyst precursor;
2) even the dripping of mixing solutions is coated in substrate, after oven dry, is placed on the water-cooled deposition platform of DC arc plasma jet CVD system sediment chamber under infrared lamp;
3) close the sediment chamber, the open water cooling system also vacuumizes, and presses and pump pressure when being 0.01Pa when the chamber, passes into the H that flow is 500-20000mL/min 2With the Ar of 500-20000mL/min, press to the chamber and pump pressure is gone up respectively to 1000-10000Pa and 10000-20000Pa;
4) remain on 1000-10000Pa and 10000-20000Pa in chamber pressure and pump pressure, temperature remains under the condition of 500-1205 ℃, apply magnetic control voltage 1-20V, arc voltage 50-200V, start direct current arc, reaction times 0.5-15 minute, then pass into the carbon-source gas that flow is 10-600mL/min, reaction times 0.5-15 minute, directly make MgO nanobelts-carbon nano tube compound material by carrying out plasma reaction at catalyst surface.
In described mixing solutions, the mol ratio of Nickelous nitrate hexahydrate and magnesium nitrate hexahydrate is 10-1:1-10, and the total amount of Nickelous nitrate hexahydrate and magnesium nitrate hexahydrate and the amount ratio of ethanol are 0.1-2mol/L.
Described substrate is molybdenum, zirconium or graphite.
Described carbon-source gas is methane, acetylene or ethene.
Sediment chamber in described DC arc plasma jet CVD system comprises deposit cavity and plasma torch, deposit cavity is comprised of cavity body wall, cavity deposition table and bleeding point, substrate is put on the cavity deposition table, cavity body wall and cavity deposition table all through water quench suppressing the deposit cavity temperature rise, bleeding point is located at the deposit cavity bottom and is connected with the vacuum pump air-bleed system; Plasma torch comprises that working gas entrance, discharge channel from top to bottom, the anode spout of bottom, the current-carrying screwed pipe magnet coil that is looped around the torch outer wall and the cooling-water duct on shaft-like tungsten cathode, the tubular red copper anode that surrounds negative electrode, top form, tungsten cathode, red copper anode and current-carrying screwed pipe magnet coil are connected with DC power distribution cabinet respectively, and the working gas entrance is connected with gas bottle by mass-flow gas meter.
Technical Analysis of the present invention:
In the DC arc plasma jet CVD system, volts DS is added between the negative electrode and anode of plasma torch, when the Ar as striking gas of easily ionizable flows through between negative electrode and anode, form plasma body, and then ionization hydrogen, form hydrogen plasma, reduction forms the Ni nano-metal particle to the NiO that is formed by the nickelous nitrate thermolysis through hydrogen plasma, with MgO jointly as the catalyst system of carbon nano-tube, carbon nano-tube under hydrogen, carbon-source gas plasma atmosphere, simultaneously, MgO forms the nano belt pattern under plasma effect.
Advantage of the present invention: adopt the DC arc plasma jet CVD system, direct fast growth of magnetisum oxide nano belt-carbon nano tube compound material in substrate, catalyzer forms to synchronize with Material growth and completes, and this preparation method's technique is simple, efficient is high, energy consumption is low, cost is low, commercial scale production has a high potential.
Description of drawings
Fig. 1 is the structural representation of DC arc plasma jet CVD of the present invention sediment chamber.
In figure: 1. deposit cavity 2. plasma torch 3. cavity body wall 4. cavity deposition table 5. bleeding point 6. substrate 7. tungsten cathode 8. red copper anode 9. working gas entrance 10. discharge channel 11 anode spout 12. current-carrying screwed pipe magnet coil 13. cooling-water ducts
Fig. 2 is the MgO nanobelts for preparing under the processing condition of embodiment 1-carbon nano tube compound material SEM photo.
Fig. 3 is the HRTEM photo of carbon nanotube in the MgO nanobelts-carbon nano tube compound material for preparing under the processing condition of embodiment 2.
Fig. 4 is the HRTEM photo of MgO nanobelts in the MgO nanobelts-carbon nano tube compound material for preparing under the processing condition of embodiment 2.
Embodiment
The below elaborates to embodiments of the invention, and the present embodiment is implemented under take technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
a kind of MgO-nanobelts/CNTs composite manufacture method based on DC arc plasma jet CVD, the DC arc plasma jet CVD system that adopts is that Hebei Institute of Laser produces, sediment chamber's structure of this system as shown in Figure 1, sediment chamber in the DC arc plasma jet CVD system comprises deposit cavity 1 and plasma torch 2, deposit cavity 1 is by cavity body wall 3, cavity deposition table 4 and bleeding point 5 form, substrate 6 is put on cavity deposition table 4, cavity body wall 3 and cavity deposition table 4 all through water quench to suppress the deposit cavity temperature rise, bleeding point 5 is located at deposit cavity 1 bottom and is connected with the vacuum pump air-bleed system, plasma torch 2 comprises that working gas entrance 9, discharge channel from top to bottom 10, the anode spout 11 of bottom, the current-carrying screwed pipe magnet coil 12 that is looped around the torch outer wall and the cooling-water duct 13 on shaft-like tungsten cathode 7, the tubular red copper anode 8 that surrounds negative electrode, top form, tungsten cathode 7, red copper anode 8 and current-carrying screwed pipe magnet coil 12 are connected with DC power distribution cabinet respectively, and working gas entrance 9 is connected with gas bottle by mass-flow gas meter.
Embodiment 1:
A kind of preparation method of MgO nanobelts-carbon nano tube compound material adopts the preparation of DC arc plasma jet CVD system, and step is as follows:
1) Nickelous nitrate hexahydrate of 14.5g and the magnesium nitrate hexahydrate of 12.8g are dissolved in the ethanol of 100mL, making nickel nitrate solution concentration is that the 0.5mol/L(mol ratio is 1:1) mixing solutions;
2) even the dripping of mixing solutions is coated in the molybdenum substrate, after oven dry, is placed on the water-cooled deposition platform of DC arc plasma jet CVD sediment chamber under infrared lamp;
3) close the sediment chamber, the open water cooling system also vacuumizes, and presses and pump pressure when being 0.01Pa when the chamber, passes into the H that flow is 4000mL/min 2With the Ar of 1500mL/min, wait for that press in the chamber and pump pressure is gone up respectively to 3000Pa and 13000Pa;
4) remain on 3000Pa and 13000Pa in chamber pressure and pump pressure, temperature remains under the condition of 950 ℃, apply magnetic control voltage 8V, arc voltage 95V, start direct current arc, in 3 minutes reaction times, pass into afterwards the methane that flow is 138mL/min, in 2 minutes reaction times, directly prepare MgO nanobelts-carbon nano tube compound material by carrying out plasma reaction at catalyst surface.
Fig. 2 changes the MgO nanobelts for preparing under processing condition-carbon nano tube compound material SEM photo, shows in figure that in matrix material, the carbon nanotube caliber is 10-40nm, and MgO nano belt width is 10-30nm.
Embodiment 2:
A kind of preparation method of MgO nanobelts-carbon nano tube compound material adopts the preparation of DC arc plasma jet CVD system, and step is as follows:
1) Nickelous nitrate hexahydrate of 7.25g and the magnesium nitrate hexahydrate of 14.2g are dissolved in the ethanol of 100mL, making nickel nitrate solution concentration is that the 0.25mol/L(mol ratio is 1:3) mixing solutions;
2) even the dripping of mixing solutions is coated on graphite base, after oven dry, is placed on the water-cooled deposition platform of DC arc plasma jet CVD sediment chamber under infrared lamp;
3) close the sediment chamber, the open water cooling system also vacuumizes, and presses and pump pressure when being 0.01Pa when the chamber, passes into the H that flow is 6000mL/min 2With the Ar of 1600mL/min, wait for that press in the chamber and pump pressure is gone up respectively to 4000Pa and 14000Pa;
4) remain on 4000Pa and 14000Pa in chamber pressure and pump pressure, temperature remains under the condition of 1050 ℃, apply magnetic control voltage 6V, arc voltage 100V, start direct current arc, in 2.5 minutes reaction times, pass into afterwards the acetylene that flow is 140mL/min, in 3 minutes reaction times, directly prepare MgO nanobelts-carbon nano tube compound material by carrying out plasma reaction at catalyst surface.
Fig. 3 is the HRTEM photo of carbon nanotube in the MgO nanobelts-carbon nano tube compound material for preparing under these processing condition, shows in figure that prepared carbon nanotube is the multi-walled carbon nano-tubes of " Bamboo-shaped ", and caliber is about 15nm.
Fig. 4 is the HRTEM photo of MgO nanobelts in the MgO nanobelts-carbon nano tube compound material for preparing under these processing condition, show in figure that prepared bitter earth nano bandwidth is about 10nm, and overall width is even.
Conclusive evidence by experiment, in the present invention by controlling growth conditions: as processing condition such as complex catalyst precursor substrate concentration and concentration ratio, reaction pressure, gas flow, arc powers, can prepare the MgO nanobelts-carbon nano tube compound material of various demands.

Claims (5)

1. the preparation method of a MgO nanobelts-carbon nano tube compound material is characterized in that: adopt the preparation of DC arc plasma jet CVD system, step is as follows:
1) Nickelous nitrate hexahydrate and magnesium nitrate hexahydrate are dissolved in ethanol, make mixing solutions as catalyst precursor;
2) even the dripping of mixing solutions is coated in substrate, after oven dry, is placed on the water-cooled deposition platform of DC arc plasma jet CVD system sediment chamber under infrared lamp;
3) close the sediment chamber, the open water cooling system also vacuumizes, and presses and pump pressure when being 0.01Pa when the chamber, passes into the H that flow is 500-20000mL/min 2With the Ar of 500-20000mL/min, press to the chamber and pump pressure is gone up respectively to 1000-10000Pa and 10000-20000Pa;
4) remain on 1000-10000Pa and 10000-20000Pa in chamber pressure and pump pressure, temperature remains under the condition of 500-1205 ℃, apply magnetic control voltage 1-20V, arc voltage 50-200V, start direct current arc, reaction times 0.5-15 minute, then pass into the carbon-source gas that flow is 10-600mL/min, reaction times 0.5-15 minute, directly make MgO nanobelts-carbon nano tube compound material by carrying out plasma reaction at catalyst surface.
2. the preparation method of MgO nanobelts-carbon nano tube compound material according to claim 1, it is characterized in that: in described mixing solutions, the mol ratio of Nickelous nitrate hexahydrate and magnesium nitrate hexahydrate is 10-1:1-10, and the total amount of Nickelous nitrate hexahydrate and magnesium nitrate hexahydrate and the amount ratio of ethanol are 0.1-2mol/L.
3. the preparation method of MgO nanobelts-carbon nano tube compound material according to claim 1, it is characterized in that: described substrate is molybdenum, zirconium or graphite.
4. the preparation method of MgO nanobelts-carbon nano tube compound material according to claim 1, it is characterized in that: described carbon-source gas is methane, acetylene or ethene.
5. the preparation method of MgO nanobelts-carbon nano tube compound material according to claim 1, it is characterized in that: the sediment chamber in described DC arc plasma jet CVD system comprises deposit cavity and plasma torch, deposit cavity is comprised of cavity body wall, cavity deposition table and bleeding point, substrate is put on the cavity deposition table, cavity body wall and cavity deposition table all through water quench suppressing the deposit cavity temperature rise, bleeding point is located at the deposit cavity bottom and is connected with the vacuum pump air-bleed system; Plasma torch comprises that working gas entrance, discharge channel from top to bottom, the anode spout of bottom, the current-carrying screwed pipe magnet coil that is looped around the torch outer wall and the cooling-water duct on shaft-like tungsten cathode, the tubular red copper anode that surrounds negative electrode, top form, tungsten cathode, red copper anode and current-carrying screwed pipe magnet coil are connected with DC power distribution cabinet respectively, and the working gas entrance is connected with gas bottle by mass-flow gas meter.
CN2013100300482A 2013-01-25 2013-01-25 Preparation method of magnesium oxide nanobelt-carbon nanotube composite material Pending CN103086406A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103466667A (en) * 2013-09-10 2013-12-25 清华大学 Method for preparing nanometer magnesium oxide through plasma high temperature pyrolysis method
CN110508270A (en) * 2019-09-16 2019-11-29 中南大学 A kind of magnesia/carbon nano tube compound material and the preparation method and application thereof
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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CN102583456A (en) * 2012-03-03 2012-07-18 天津理工大学 DC (direct-current)-plasma-jet CVD (chemical vapor deposition) method for preparing magnesia nanobelts
CN102649547A (en) * 2011-02-25 2012-08-29 东京毅力科创株式会社 Carbon nanotube forming method and pre-treatment method therefor

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CN101660144A (en) * 2009-09-25 2010-03-03 河北普莱斯曼金刚石科技有限公司 Plasma torch for chemical vapor deposition
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103466667A (en) * 2013-09-10 2013-12-25 清华大学 Method for preparing nanometer magnesium oxide through plasma high temperature pyrolysis method
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CN110508270A (en) * 2019-09-16 2019-11-29 中南大学 A kind of magnesia/carbon nano tube compound material and the preparation method and application thereof
CN110508270B (en) * 2019-09-16 2020-09-08 中南大学 Magnesium oxide/carbon nanotube composite material and preparation method and application thereof
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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Application publication date: 20130508