CN102534571A - Method for preparing magnesium oxide nanoribbon by radio-frequency plasma enhanced CVD (Chemical Vapor Deposition) - Google Patents
Method for preparing magnesium oxide nanoribbon by radio-frequency plasma enhanced CVD (Chemical Vapor Deposition) Download PDFInfo
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- CN102534571A CN102534571A CN2012100535360A CN201210053536A CN102534571A CN 102534571 A CN102534571 A CN 102534571A CN 2012100535360 A CN2012100535360 A CN 2012100535360A CN 201210053536 A CN201210053536 A CN 201210053536A CN 102534571 A CN102534571 A CN 102534571A
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Abstract
The invention provides a method for preparing a magnesium oxide nanoribbon by using radio-frequency plasma enhanced CVD (Chemical Vapor Deposition); the method comprises the following steps of: by using a mixing solution of magnesium nitrate and nickel nitrate as a precursor, dropping the mixing solution on a substrate such as silicon, glass and the like, placing the substrate on a deposition platform inside the cavity of a radio-frequency plasma enhanced chemical vapor deposition device after drying the substrate, carrying out heating decomposition, and then restoring high-temperature plasmas formed by a protected gas and hydrogen under the action of radio-frequency to form the magnesium oxide nanoribbon. The method has the advantages that the prepared magnesium oxide nanostructure comprises a rectangular banded structure, a crossed reticular nanostructure, a T-shaped structure and the like and has better crystallinity, and particularly, the reticular nanomstructure changes in the growing crystal orientation at a crossing place and shows certain elastic deformability; and the method is simple in technology and easy to implement, is beneficial to the realization of industrialization and can be widely applied to the fields such as electronics, catalysis, ceramics, electrical insulating materials, high temperature resistant materials and the like.
Description
Technical field
The present invention relates to the preparation method of bitter earth nano band, particularly a kind of radio-frequency plasma strengthens the method that chemical Vapor deposition process (CVD) prepares the bitter earth nano band.
Background technology
Monodimension nanometer material is because its unique small-size effect, surface effects and quantum size effect have the new features such as electricity, calorifics and mechanics that are different from conventional material.The Natural manganese dioxide of nanostructure is compared with nano-powder and is had the more crystalline degree, and especially characteristics such as the band shape of its high firmness, HMP, uniqueness and network nano structure make its application in fields such as high temperature material, ceramic insulating material and support of the catalyst more and more receive people's attention.
In recent years, the existing more report of preparation bitter earth nano band.Zhang etc. are through heating MgCl in oxygen
2Prepared the higher bitter earth nano band [Appl.Phys.A, 2001,73:773-775] of purity; Chen Chen etc. are based on MgCO
33H
2The oriented growth characteristic of O with ammoniacal liquor and the two precipitation agent co-precipitation chemosynthesis approach of volatile salt, has at first been synthesized MgCO
33H
2O nano belt structure has been synthesized bitter earth nano band [Chinese Journal of Inorganic Chemistry, 2005,21 (6): 859-862] through calcining then in a large number; Ma etc. are earlier with the N of MAGNESIUM METAL 99 at 650 ℃
2Middle evaporation forms Mg
3N
2Precursor, Mg then
3N
2N at 800 ℃
2And O
2Decompose in the atmosphere and formation bitter earth nano band [Chemical Physics Letters, 2003,370 (5-6): 770-773].But owing to reasons such as production technique and production costs, bitter earth nano band industrialization at present also is difficult to realize that preparing the higher nano magnesia of a large amount of purity will have important meaning.
Strengthen the chemical gas-phase deposition system advantages such as to have speed fast, and technology is simple that prepare the bitter earth nano band with radio-frequency plasma.The bitter earth nano of this method preparation has prestige and brings into play enormous function in fields such as electronics, catalysis, pottery, electrically insulating material and high temperature materials.
Summary of the invention
The objective of the invention is to above-mentioned existing problems, provide a kind of radio-frequency plasma to strengthen the method that chemical Vapor deposition process prepares the bitter earth nano band, this method technology is simple, preparation speed is fast, helps realizing industrialization.
Technical scheme of the present invention:
A kind of radio-frequency plasma strengthens the method that the CVD legal system is equipped with the bitter earth nano band, and step is following:
1) with Mg (NO
3)
26H
2O crystal and Ni (NO
3)
26H
2The O dissolution of crystals makes mixing solutions as precursor in absolute ethyl alcohol;
2) above-mentioned mixing solutions evenly is sprayed on the substrate, after oven dry under the 50-100 ℃ of temperature, places radio-frequency plasma to strengthen on the sample table of chemical vapour deposition (RF-PECVD) equipment Vakuumkammer;
3) close vacuum chamber and vacuumizing; When pressure in the chamber during less than 0.1Pa; Feed protective gas and hydrogen to vacuum chamber; Shield gas flow rate is 10-100mL/min; Hydrogen flowing quantity is 20-200mL/min; When pressure reaches 100-2000Pa, be to heat 0.5-2 hour under the 700-1200 ℃ of condition sample stage in temperature, the predecessor on the substrate is decomposed and formation MgO and NiO;
4) apply the radio frequency power of 50-500W, under the hydrogen plasma effect, NiO is reduced to the Ni nano-metal particle, the reaction times is 0.5-2 hour, can make 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/mL.
Said substrate is Si, glass, quartz or copper.
Said shielding gas is argon gas or helium.
Technical Analysis of the present invention:
It is through heated substrate the precursor mixing solutions to be decomposed that radio-frequency plasma strengthens chemical Vapor deposition process, apply radio frequency power after, the high-temperature plasma reduction that resolvent is formed by hydrogen and shielding gas, formation bitter earth nano band.Bring with chemical Vapor deposition process and prepared by other bitter earth nano than what reported, preparation speed is fast, and process step is simplified.
Advantage of the present invention is: adopt be soluble in ethanol and can labile at low temperatures magnesium nitrate and the nickelous nitrate mixing solutions as precursor; Strengthen chemical gas-phase deposition system with radio-frequency plasma and obtain nanostructures of magnesium oxide; The nanostructures of magnesium oxide of preparation comprises network nano structure and the T shape structure of rectangle zonal structure, intersection etc.; Crystallinity is better, and especially network nano structure changes in the growth crystal orientation of infall, demonstrates certain elastic deformation property; This method technology is simple, easy to implement, helps realizing industrialization, can be widely used in fields such as electronics, catalysis, pottery, electrically insulating material and high temperature material.
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 radio-frequency plasma of used preparation bitter earth nano band strengthens the single target high temperature of the PECVD400 type high vacuum filming equipment that chemical vapor depsotition equipment (RF-PECVD) is Shenyang Scientific Instrument Research & Mfg. Center Co., Ltd., C.A.S's production among the embodiment.
Embodiment 1:
A kind of radio-frequency plasma strengthens the method that the CVD legal system is equipped with the bitter earth nano band, and step is following:
1) with 13gMg (NO
3)
26H
2O crystal and 14.5g Ni (NO
3)
26H
2The O dissolution of crystals makes mixing solutions as precursor in 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) above-mentioned mixing solutions evenly is sprayed on the Si substrate, after oven dry under 80 ℃ of temperature, places radio-frequency plasma to strengthen on the sample table of chemical vapour deposition (RF-PECVD) system vacuum chamber;
3) close vacuum chamber and vacuumizing; When pressure in the chamber during less than 0.1Pa; Feed argon gas and hydrogen to vacuum chamber; Wherein argon flow amount is 20mL/min; Hydrogen flowing quantity is 120mL/min, when pressure reaches 1000Pa, with sample stage heating 0.5 hour; Heating-up temperature is 1050 ℃, and the predecessor on the substrate is decomposed and formation MgO and NiO;
4) apply the radio frequency power of 150W, under the hydrogen plasma effect, NiO is reduced to the Ni nano-metal particle, because the specific activity H atom of Mg atom is strong, can't be reduced into Mg to MgO with hydrogen plasma, the reaction times is 0.5 hour, forms 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: mostly the nano magnesia of preparation is rectangular configuration, and width is 30-70nm, and length is about 1-2nm, also has a spot of cross network structure to occur.
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.
Embodiment 2:
A kind of radio-frequency plasma strengthens the method that the CVD legal system is equipped with the bitter earth nano band, and step is following:
1) with 7.68g Mg (NO
3)
26H
2O crystal and 2.91g Ni (NO
3)
26H
2The O dissolution of crystals makes mixing solutions as precursor in 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) above-mentioned mixing solutions evenly is sprayed on the glass substrate, after oven dry under 60 ℃ of temperature, places radio-frequency plasma to strengthen on the sample table of chemical vapour deposition (RF-PECVD) system vacuum chamber;
3) close vacuum chamber and vacuumizing; When pressure in the chamber during less than 0.1Pa; Feed helium and hydrogen to vacuum chamber; Wherein argon flow amount is 10mL/min; Hydrogen flowing quantity is 80mL/min, when pressure reaches 1200Pa, with sample stage heating 1 hour; Heating-up temperature is 850 ℃, and the predecessor on the substrate is decomposed and formation MgO and NiO;
4) apply the radio frequency power of 300W, under the hydrogen plasma effect, NiO is reduced to the Ni nano-metal particle, because the specific activity H atom of Mg atom is strong, can't be reduced into Mg to MgO with hydrogen plasma, the reaction times is 1 hour, forms 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 nano magnesia of preparation is a rectangular configuration, and width is about 20～70nm, has formed the cross network structure simultaneously, wherein has a spot of nickel particle.
Fig. 4 is the EDS figure of the bitter earth nano band for preparing under these processing condition; Fig. 4 is corresponding with Fig. 3; Show among the figure: this nanostructure is made up of O and Mg element; And corresponding atomic ratio is about 1: 1, only contains minor N i impurity, explains and has prepared quality bitter earth nano band preferably under this condition.
Embodiment 3:
A kind of radio-frequency plasma strengthens the method that the CVD legal system is equipped with the bitter earth nano band, and step is following:
1) with 25.6g Mg (NO
3)
26H
2O crystal and 2.91g Ni (NO
3)
26H
2The O dissolution of crystals makes mixing solutions as precursor in absolute ethyl alcohol, be made into Mg (NO
3)
2Concentration be 1mol/L, Mg (NO
3)
2With Ni (NO
3)
2Mol ratio is 10: 1 a mixing solutions;
2) above-mentioned mixing solutions evenly is sprayed on the copper substrate, after oven dry under 90 ℃ of temperature, places radio-frequency plasma to strengthen on the sample table of chemical vapour deposition (RF-PECVD) system vacuum chamber;
3) close vacuum chamber and vacuumizing; When pressure in the chamber during less than 0.1Pa; Feed argon gas and hydrogen to vacuum chamber; Wherein argon flow amount is 15mL/min; Hydrogen flowing quantity is 100mL/min, when pressure reaches 900Pa, with sample stage heating 0.5 hour; Heating-up temperature is 950 ℃, and the predecessor on the substrate is decomposed and formation MgO and NiO;
4) apply the radio frequency power of 200W, under the hydrogen plasma effect, NiO is reduced to the Ni nano-metal particle, because the specific activity H atom of Mg atom is strong, can't be reduced into Mg to MgO with hydrogen plasma, the reaction times is 1 hour, forms the bitter earth nano band.
Through the experiment conclusive evidence, the present invention is through controlling preparation condition: like pilot-gas flow, underlayer temperature; Reaction pressure; Processing condition such as radio frequency power and reaction times, and, can prepare the higher bitter earth nano band of a large amount of purity through allotment strength of solution and ratio etc.
Claims (4)
1. a radio-frequency plasma strengthens the method that the CVD legal system is equipped with the bitter earth nano band, it is characterized in that step is following:
1) with Mg (NO
3)
26H
2O crystal and Ni (NO
3)
26H
2The O dissolution of crystals makes mixing solutions as precursor in absolute ethyl alcohol;
2) above-mentioned mixing solutions evenly is sprayed on the substrate, after oven dry under the 50-100 ℃ of temperature, places radio-frequency plasma to strengthen on the sample table of chemical vapour deposition (RF-PECVD) equipment Vakuumkammer;
3) close vacuum chamber and vacuumizing; When pressure in the chamber during less than 0.1Pa; Feed protective gas and hydrogen to vacuum chamber; Shield gas flow rate is 10-100mL/min; Hydrogen flowing quantity is 20-200mL/min; When pressure reaches 100-2000Pa, be to heat 0.5-2 hour under the 700-1200 ℃ of condition sample stage in temperature, the predecessor on the substrate is decomposed and formation MgO and NiO;
4) apply the radio frequency power of 50-500W, under the hydrogen plasma effect, NiO is reduced to the Ni nano-metal particle, the reaction times is 0.5-2 hour, can make the bitter earth nano band.
2. strengthen the method that the CVD legal system is equipped with the bitter earth nano band according to the said radio-frequency plasma of claim 1, 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/mL.
3. strengthen the method that the CVD legal system is equipped with the bitter earth nano band according to the said radio-frequency plasma of claim 1, it is characterized in that: said substrate is Si, glass, quartz or copper.
4. strengthen the method that the CVD legal system is equipped with the bitter earth nano band according to the said radio-frequency plasma of claim 1, it is characterized in that: said shielding gas is argon gas or helium.
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|---|---|---|---|---|
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267693A (en) * | 2011-07-06 | 2011-12-07 | 天津理工大学 | Low-temperature preparation method of carbon nanotube |
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| CN102267693A (en) * | 2011-07-06 | 2011-12-07 | 天津理工大学 | Low-temperature preparation method of carbon nanotube |
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| Title |
|---|
| 《无机化学学报》 20060630 陈晨等 "新颖氧化镁纳米带共沉淀法合成与表征" 859-861 1-4 第21卷, 第6期 * |
| 陈晨等: ""新颖氧化镁纳米带共沉淀法合成与表征"", 《无机化学学报》 * |
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|---|---|---|---|---|
| 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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