CN102583456A - DC (direct-current)-plasma-jet CVD (chemical vapor deposition) method for preparing magnesia nanobelts - Google Patents
DC (direct-current)-plasma-jet CVD (chemical vapor deposition) method for preparing magnesia nanobelts Download PDFInfo
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- CN102583456A CN102583456A CN2012100534993A CN201210053499A CN102583456A CN 102583456 A CN102583456 A CN 102583456A CN 2012100534993 A CN2012100534993 A CN 2012100534993A CN 201210053499 A CN201210053499 A CN 201210053499A CN 102583456 A CN102583456 A CN 102583456A
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Abstract
The invention discloses a DC (direct-current)-plasma-jet CVD (chemical vapor deposition) method for preparing magnesia nanobelts. The DC-plasma-jet CVD method comprises the following steps that: mixed solution of magnesium nitrate and nickel nitrate is adopted as a precursor and then drops on substrates of molybdenum, zirconium and the like, the dried substrates are placed on a deposit table in DC-plasma-jet CVD equipment, a DC arc discharges to enable protective gas and hydrogen to generate high-temperature plasmas which are then jetted on the substrates, and the precursor solution is resolved and reduced to generate the magnesia nanobelts by the high-temperature plasmas. The DC-plasma-jet CVD method has the advantages that the high-purity magnesia nanobelts can be directly prepared by the DC-plasma-jet CVD system, the process is simple, the method is easy to implement, the purity of the prepared magnesia nanobelts is higher, the crystallinity of the magnesia nanobelts is better, the preparation rate is high, and the mass-production of the magnesia nanobelts can be realized, so that the method has a wide application prospect in the field of catalysts and catalyst supports.
Description
Technical field
The present invention relates to the preparation method of bitter earth nano band, particularly a kind of dc plasma jet chemical Vapor deposition process (CVD) prepares the method for bitter earth nano band.
Background technology
Natural manganese dioxide is a kind of functional materials that important use is arranged, and can be widely used in rubber, plastics, electric wire, glass, pottery, chemical reagent, medicine and other fields.Especially the Natural manganese dioxide of nanometer scale is expected in electron device, pottery and catalyzer and support of the catalyst field performance enormous function thereof because its unique geometrical dimension and surface effects have electricity, light, magnetic, the chemical property that is different from bulk material.The Natural manganese dioxide of nanostructure is compared with nano-powder and is had the more crystalline degree, and especially the particular performances and the application prospect that are had of nano strip structure and cross network structure thereof more and more receives people's attention.
The nano magnesia preparation method mainly contains three types at present, i.e. solid phase method, liquid phase method and vapor phase process.In recent years, usefulness Co such as Zhu have gone out the magnesium oxide nanometer rod and the nano belt [Chemical Physics Letters, 2001,347 (4-6): 337-343] of herring-bone form as Preparation of Catalyst; Li etc. are through chemical Vapor deposition process, i.e. ir radiation Mg/Al target has in a vacuum been prepared the bitter earth nano band of cubic structure; Its width can reach 200nm; Flakiness ratio is about 1-2 [Chemical Physics Letters, 2002,359 (1-2): 141-145]; Fang Xiaosheng etc. on silicon substrate with the magnesium powder as starting material, under water vapor and certain condition, synthesized the bitter earth nano floral structure of forming by many nanofibers [functional materials 2004, supplementary issue 35:2709-2712] of regular distribution with chemical Vapor deposition process.But these methods are difficult to a large amount of synthetic in industry, and the realization industrialization is had got long long way to go, and the Natural manganese dioxide of preparing the higher nanostructure of a large amount of purity has very important meaning.
Preparing the bitter earth nano band with the dc plasma jet chemical gas-phase deposition system, to have preparation speed fast, the product purity advantages of higher.Document and the patent of utilizing this method to prepare the bitter earth nano band are not also seen public reported.The bitter earth nano of this method preparation has prestige and brings into play enormous function in fields such as electronic industrial material, catalysis, insulating material and high temperature materials.
Summary of the invention
The objective of the invention is provides a kind of dc plasma jet CVD legal system to be equipped with the method for bitter earth nano band to above-mentioned existing problems, and this method has that preparation speed is fast, the product purity advantages of higher, helps realizing industrialization.
Technical scheme of the present invention:
A kind of dc plasma jet CVD legal system is equipped with the method for bitter earth nano band, and step is following:
1) magnesium nitrate crystal and nickelous nitrate dissolution of crystals are made mixing solutions as precursor in absolute ethyl alcohol;
2) the above-mentioned mixing solutions that makes is evenly dropped on the substrate, dry naturally;
3) with tin silk pad under above-mentioned substrate, be positioned on the deposition table in the dc plasma jet chemical vapor depsotition equipment chamber;
4) close Vakuumkammer and open vacuum pump and water pump vacuumizes, during less than 3kpa, open lobe pump, when pressure in the chamber during less than 0.1Pa etc. pump pressure; Feed shielding gas and hydrogen to Vakuumkammer, shield gas flow rate is 1-3L/min, and hydrogen flowing quantity is 6-15L/min; Start direct current arc, arc current is 75-150A, regulates vent valve and chamber and presses variable valve; Pressure is that 2500-7000Pa, underlayer temperature are under the 750-1200 ℃ of condition in the chamber, reacts 5-30 minute, makes the bitter earth nano band.
Mg (NO in the said mixing solutions
3)
2And Ni (NO
3)
2Mol ratio be 1-10: 1, Mg (NO
3)
2Volumetric molar concentration be 0.05-2mol/L.
Said substrate is molybdenum, zirconium or graphite.
Said tin silk twines the 6-10 circle in the form of a ring.
Said shielding gas is argon gas or helium.
Technical Analysis of the present invention:
Dc arc plasma jet is with the direct current arc discharge, makes hydrogen and argon gas mixed gas form high-temperature plasma, and the heat that arc-over produces makes the complex catalyst precursor thing on the substrate decompose and formation NiO and MgO; Under the hydrogen plasma effect; NiO is reduced to the Ni nano-metal particle,, can't be reduced into Mg to MgO with hydrogen plasma because the specific activity H atom of Mg atom is strong; Wherein Ni plays dissemination, labile Mg (NO under the low temperature
3)
2And Ni (NO
3)
2Precursor decomposes under the effect of high temperature hydrogen plasma body and is reduced, and forms the bitter earth nano band.
Advantage of the present invention is: adopt the dc plasma jet chemical gas-phase deposition system can directly prepare highly purified bitter earth nano band; This method technology is simple, easy to implement; The bitter earth nano band purity of preparation is higher, and crystallinity is better, and preparation speed is fast; Can be mass-produced, have broad application prospects at catalyzer and support of the catalyst field.
Description of drawings
Fig. 1 is the TEM figure of the bitter earth nano band for preparing under the processing condition of embodiment 1.
Fig. 2 is the HRTEM figure of the bitter earth nano band for preparing under the processing condition of embodiment 1.
Fig. 3 is the TEM figure of the bitter earth nano band for preparing under the processing condition of embodiment 2.
Fig. 4 is the EDS figure of the bitter earth nano band for preparing under the processing condition of embodiment 2.
Embodiment
Below in conjunction with specific embodiment the present invention is elaborated, provided detailed embodiment and concrete operating process.The equipment of used preparation bitter earth nano band is the dc plasma jet chemical gas-phase deposition system that Hebei Institute of Laser produces among the embodiment.
Embodiment 1:
A kind of dc plasma jet CVD legal system is equipped with the method for bitter earth nano band, and step is following:
1) 13g magnesium nitrate crystal and 14.5g nickelous nitrate dissolution of crystals are made mixing solutions as the complex catalyst precursor thing in the 100mL absolute ethyl alcohol, be made into Mg (NO
3)
2And Ni (NO
3)
2Concentration be 0.5mol/L, Mg (NO
3)
2With Ni (NO
3)
2Mol ratio is 1: 1 a mixing solutions;
2) solution of step (1) being processed drops on the molybdenum platform equably, dries naturally;
3) the tin silk is twined 8 circles in the form of a ring and fill up under the molybdenum platform, be positioned over together on the deposition table in the dc plasma jet chemical vapor depsotition equipment chamber;
4) close Vakuumkammer and open vacuum pump and water pump vacuumizes, during less than 3kpa, open lobe pump, when pressure in the chamber during less than 0.1Pa etc. pump pressure; Feed argon gas and hydrogen to Vakuumkammer, argon flow amount is 1.5L/min, and hydrogen flowing quantity is 12L/min, starts direct current arc; The adjusting arc current is 110A, regulates vent valve and chamber and presses variable valve, and pressure is 3000Pa in the chamber; Underlayer temperature is under 1050 ℃ of conditions, reacts 8 minutes, prepares the bitter earth nano band.
Fig. 1 is the TEM photo of the bitter earth nano band for preparing under these processing condition, and show among the figure: the bitter earth nano bandwidth of preparation is about 30～70nm, and in bifurcation stronger netted syndeton is arranged.
Fig. 2 is the HRTEM photo of the bitter earth nano band for preparing under these processing condition, and show among the figure: the bitter earth nano band crystallinity of preparation is good, and this spacing is 021nm, is face centered cubic (200) crystal face corresponding to MgO.Fig. 2 lower right corner accompanying drawing is the HRTEM photo of reticulated structure junction, is presented at magnesian growth crystal orientation, decussate texture place among the figure and changes, and demonstrates stronger stress.
Embodiment 2:
A kind of dc plasma jet CVD legal system is equipped with the method for bitter earth nano band, and step is following:
1) 7.68g magnesium nitrate crystal and 2.91g nickelous nitrate dissolution of crystals are made mixing solutions as the complex catalyst precursor thing in the 100mL absolute ethyl alcohol, be made into Mg (NO
3)
2Concentration be 0.3mol/L, Mg (NO
3)
2With Ni (NO
3)
2Mol ratio is 3: 1 a mixing solutions;
2) solution of step (1) being processed drops on the graphite platform equably, dries naturally;
3) the tin silk is twined 10 circles in the form of a ring and fill up under the graphite platform, be positioned over together on the deposition table in the dc plasma jet chemical vapor depsotition equipment chamber;
4) close Vakuumkammer and open vacuum pump and water pump vacuumizes, during less than 3kpa, open lobe pump, when pressure in the chamber during less than 0.1Pa etc. pump pressure; Feed helium and hydrogen to Vakuumkammer, argon flow amount is 1.2L/min, and hydrogen flowing quantity is 10L/min, starts direct current arc; The adjusting arc current is 90A, regulates vent valve and chamber and presses variable valve, and pressure is 4000Pa in the chamber; Underlayer temperature is under 950 ℃ of conditions, reacts 10 minutes, prepares the bitter earth nano band.
Fig. 3 is the TEM photo of the bitter earth nano band for preparing under these processing condition, and show among the figure: the bitter earth nano bandwidth of preparation is about more than the 40nm, and length is about about 2 μ m, and interlaced formation network nano structure.
Fig. 4 is the EDS figure of the bitter earth nano band for preparing under these processing condition, and show among the figure: this nanostructure is made up of O and Mg element, and atomic ratio is about 1: 1 accordingly, explains and has prepared the higher bitter earth nano band of purity under this condition.
Through the experiment conclusive evidence, pass through the control preparation condition among the present invention: like the pilot-gas flow, underlayer temperature, reaction pressure, processing condition such as flame current and reaction times can grow the higher bitter earth nano band of a large amount of purity.
Claims (5)
1. a dc plasma jet CVD legal system is equipped with the method for bitter earth nano band, it is characterized in that step is following:
1) magnesium nitrate crystal and nickelous nitrate dissolution of crystals are made mixing solutions as precursor in absolute ethyl alcohol;
2) the above-mentioned mixing solutions that makes is evenly dropped on the substrate, dry naturally;
3) with tin silk pad under above-mentioned substrate, be positioned on the deposition table in the dc plasma jet chemical vapor depsotition equipment chamber;
4) close Vakuumkammer and open vacuum pump and water pump vacuumizes, during less than 3kpa, open lobe pump, when pressure in the chamber during less than 0.1Pa etc. pump pressure; Feed shielding gas and hydrogen to Vakuumkammer, shield gas flow rate is 1-3L/min, and hydrogen flowing quantity is 6-15L/min; Start direct current arc, arc current is 75-150A, regulates vent valve and chamber and presses variable valve; Pressure is that 2500-7000Pa, underlayer temperature are under the 750-1200 ℃ of condition in the chamber, reacts 5-30 minute, makes the bitter earth nano band.
2. be equipped with the method for bitter earth nano band according to the said dc plasma jet CVD of claim 1 legal system, it is characterized in that: Mg (NO in the said mixing solutions
3)
2And Ni (NO
3)
2Mol ratio be 1-10: 1, Mg (NO
3)
2Volumetric molar concentration be 0.05-2mol/L.
3. be equipped with the method for bitter earth nano band according to the said dc plasma jet CVD of claim 1 legal system, it is characterized in that: said substrate is molybdenum, zirconium or graphite.
4. be equipped with the method for bitter earth nano band according to the said dc plasma jet CVD of claim 1 legal system, it is characterized in that: said tin silk twines the 6-10 circle in the form of a ring.
5. be equipped with the method for bitter earth nano band according to the said dc plasma jet CVD of claim 1 legal system, it is characterized in that: said shielding gas is argon gas or helium.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086406A (en) * | 2013-01-25 | 2013-05-08 | 天津理工大学 | Preparation method of magnesium oxide nanobelt-carbon nanotube composite material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004299918A (en) * | 2003-03-28 | 2004-10-28 | National Institute For Materials Science | Method for manufacturing magnesium oxide nanobelt using magnesium nitride precursor |
| CN102162135A (en) * | 2011-03-09 | 2011-08-24 | 中国科学院理化技术研究所 | Preparation method of ZnS/Si nuclear-shell nanowires or nanobelts and polycrystal Si tubes |
| CN102330069A (en) * | 2011-10-18 | 2012-01-25 | 天津理工大学 | Preparation method of carbon nano tube |
-
2012
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004299918A (en) * | 2003-03-28 | 2004-10-28 | National Institute For Materials Science | Method for manufacturing magnesium oxide nanobelt using magnesium nitride precursor |
| CN102162135A (en) * | 2011-03-09 | 2011-08-24 | 中国科学院理化技术研究所 | Preparation method of ZnS/Si nuclear-shell nanowires or nanobelts and polycrystal Si tubes |
| CN102330069A (en) * | 2011-10-18 | 2012-01-25 | 天津理工大学 | Preparation method of carbon nano tube |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086406A (en) * | 2013-01-25 | 2013-05-08 | 天津理工大学 | Preparation method of magnesium oxide nanobelt-carbon nanotube composite material |
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Application publication date: 20120718 |