CN101062765A - Preparation method of quasi one-dimensional boron nitride nanostructure - Google Patents
Preparation method of quasi one-dimensional boron nitride nanostructure Download PDFInfo
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Abstract
The invention discloses a controlled preparing method of pseudo one-dimensional boron nitride nanometer structure through adjusting preparation parameter to control diverse pseudo one-dimensional boron nitride nanometer structure, which comprises the following steps: choosing bis nickel, bis ferrum, bio cobalt or the mixture as suspended activator forerunner body; volatilizing in the low temperature region; carrying through gas-carrier to high-temperature region; disintegrating to metallic catalyst; accelerating B2O2 vapour generated through mixing boron powder and boron oxide to react with ammonia gas; generating the product; getting boron nitride nanometer thread and bamboo joint state boron nitride nanometer pipe with diverse diameter and outlook through controlling component, time, temperature of the activator. The structure of the boron nitride nanometer thread and pipe possesses essential difference, which the front (0002) face grow vertically and the back (0002) face parallel-grows.
Description
Technical field:
The present invention relates to the controllable method for preparing of boron nitride quasi-one dimensional nanostructure, be applicable to the quasi one-dimensional boron nitride nanotube and the nano wire of control preparation different-shape and structure, the output of product is big, purity is high.
Background technology:
Since carbon nanotube in 1991 was found, the preparation of various system one dimension Nano structures and application have caused widely to be paid close attention to.The structure of hexagonal boron nitride and graphite are very approaching, can be regarded as carbon atom formation sp in the alternate replacement graphite with the boron atom of nitrogen-atoms
2The class graphite flake layer structure of hydridization.The electrical properties of carbon nanotube (band gap width) changes with diameter, chirality, is difficult to control, thereby has increased the difficulty of practical application.Relative c-based nanomaterial, the electronic structure of hexagonal boron nitride is more stable, and its excellent oxidation-resistance in addition makes that the boron nitride-base nano material is potential more early to obtain practical application.Can predict, be with a wide range of applications in nano-device that the boron nitride one dimension Nano structure is worked under mal-conditions such as high temperature, oxidizing atmosphere and the product.For example its stable broad-band gap and high temperature superior oxidation resistance make it to become excellent high temperature wide bandgap semiconductor materials; The B-N key is one of the strongest key of nature, make the boron nitride nanometer one-dimensional material have can be suitable with the carbon pipe excellent mechanical property, make it might become mal-condition composite applications wild phase material; And for example, emission tip may produce high temperature or arc-over effect in the emission process on the scene, the negative electron affinity (NEA) on boron nitride surface, and its high chemical stability, high thermal stability make it to become the panel display material of practical application.Though nineteen ninety-five boron nitride nano-tube successfully preparation for the first time, and had a lot of methods to prepare boron nitride nano-tube, for example arc process, laser splash method, chemical vapour deposition, solid state reaction etc., but up to the present, the output of boron nitride tube is very low, and purity is also very poor.As the important boron nitride one dimension Nano structure of another kind, the boron nitride nanometer line, successful synthetic report is still less; Also there are defectives such as the low and productive rate of the poor or purity of degree of crystallinity is very low in only several pieces of reports.In a word, since the intrinsic performance research that this bottleneck of specimen preparation difficulty has obviously restricted the boron nitride one dimension Nano structure with and the realization of potential application.
Summary of the invention:
The purpose of this invention is to provide a kind of novel method that can prepare the quasi one-dimensional boron nitride nano material of high purity, different-shape and structure in a large number.This method can realize the quasi one-dimensional boron nitride nano material's structure, as the control of diameter, surface topography, atomic arrangement mode etc.
Technical scheme of the present invention is:
A kind of preparation method of quasi one-dimensional boron nitride nanostructure, this method adopts nickelocene, ferrocene, dicyclopentadienylcobalt or its to be mixed into floating catalytic agent presoma, in the cold zone volatilization, be carried to the high-temperature zone by carrier gas and be decomposed into metal catalyst, promote boron powder and boron oxide to mix the B that generates
2O
2Steam and ammonia gas react generate the boron nitride one dimension Nano structure of different-shape.
Wherein:
Floating catalytic agent (mixtures of ferrocene, nickelocene, dicyclopentadienylcobalt or its different proportionings) vaporization temperature is 100～300 ℃.
Nitrogenous source is an ammonia, and carrier gas is nitrogen or argon gas, and the flow proportional of nitrogenous source and carrier gas is between 0.25-4; The gas flow of nitrogenous source is 50～500sccm.
Boron powder and boron oxide are as the boron source, and weight ratio is between 1: 1～1: 7; It is 0.1～1 that the part by weight of floating catalytic agent and reactant (boron powder, boron oxide) summation closes.
The end reaction temperature is between 1200～1500 ℃, and used temperature rise rate is between 20-45 ℃/min, and the reaction times is 15～90 minutes.
Quasi-one dimensional nanostructure of the present invention comprises ring shape boron nitride nano-tube, folded cup-shaped boron nitride nanometer line etc.
Wherein, the structure of gained boron nitride nanometer line and nanotube has essential distinction, and the former grows the parallel axial growth of the latter (0002) face by (0002) face vertical axial.
Advantage of the present invention and beneficial effect are:
1, the present invention proposes to adopt the floating catalytic method, by processing parameters such as control catalyst proportioning, vaporization temperature, boron powder and boron oxide proportioning, temperature of reaction, ammonia and nitrogen flow ratios, may command prepares the boron nitride quasi-one dimensional nanostructure of high purity different-shape and structure, as ring shape boron nitride nano-tube, folded cup-shaped boron nitride nanometer line etc.The structure of gained boron nitride nanometer line and nanotube has essential distinction, and the former grows the parallel axial growth of the latter (0002) face by (0002) face vertical axial.
2, the present invention as floating catalytic agent presoma, in cold zone volatilization and be carried to the high-temperature zone by carrier gas and be decomposed into metal catalyst, promotes boron powder and boron oxide to mix the B that generates with nickelocene, ferrocene, dicyclopentadienylcobalt or its mixture
2O
2Steam and ammonia gas react generate the boron nitride one dimension Nano structure of different-shape.Advantages such as this method has good reproducibility, cost is low, processing parameter is easy to control and product production is big, even, pure adopt the inventive method purity to reach more than 90%.The present invention has established good basis for the controlled preparation and the application thereof of boron nitride one dimension Nano structure.
Description of drawings:
Fig. 1. prepared ring shape boron nitride nano-tube stereoscan photograph and corresponding transmission electron microscope photo, high resolution photo among the embodiment one.Among the figure, (a) be stereoscan photograph; (b), (c) is transmission electron microscope photo; (d) be the high resolution photo of (c) figure.
Fig. 2. prepared folded cup-shaped boron nitride nanometer line sweep electromicroscopic photograph and corresponding transmission electron microscope photo, high resolution photo among the embodiment two.Among the figure, (a) be stereoscan photograph; (b) be transmission electron microscope photo; (c) be the high resolution photo of (b) figure.
Fig. 3. prepared folded cup-shaped boron nitride nanometer line (there is the lamella of a lot of diauxic growths on the surface) stereoscan photograph and corresponding transmission electron microscope photo, selected area electron diffraction spectrum among the embodiment three.Among the figure, (a) be stereoscan photograph; (b) be transmission electron microscope photo and selected area electron diffraction spectrum (upper right corner illustration).
Fig. 4. prepared diameter homogeneous boron nitride nanometer line (there is the lamella and the minor diameter nanofiber of a lot of diauxic growths on the surface) stereoscan photograph among the embodiment four.Among the figure, (a) be the low power stereoscan photograph; (b) be the high power stereoscan photograph.
Fig. 5. prepared diameter homogeneous boron nitride nanometer line (there is the lamella of the very thin thickness of a lot of diauxic growths on the surface) stereoscan photograph among the embodiment five.Among the figure, (a) and (b) are the low power stereoscan photograph; (c) be the high power stereoscan photograph.
Fig. 6. the apparatus structure synoptic diagram that preparation process of the present invention adopted.Among the figure, 1 resistance heading furnace; 2 thermopairs; 3 alundum tubes; 4 boron powder, boron oxide powder are placed boat; 5 presomas are placed boat.
Embodiment:
As shown in Figure 6, the apparatus structure that the present invention adopts is as follows: heating unit is a conventional, electric-resistance process furnace 1, and reaction vessel is the alundum tube 3 of 30mm diameter, and temperature control and thermometric are by inserting thermopair 2 realizations in the stove.Place boat 5 at the presoma of cold zone A and place floating catalytic agent presoma, the boron powder of high-temperature zone B (being reaction zone), boron oxide powder are placed boat 4 and are placed boron powder and boron oxide powder (boron powder and boron oxide powder size range are at the 1-10 micron), enter ammonia and carrier gas by cold zone after heating up, transport to the high-temperature zone reaction decomposing the catalyzer that produces.The present invention adopts the preparation of floating catalytic method, be to be nitrogenous source with the ammonia, nitrogen or argon gas are carrier gas, ferrocene, nickelocene, dicyclopentadienylcobalt or its mixture are floating catalytic agent presoma, amorphous boron powder and boron oxide powder are mixed into the boron source, and by the processing parameter of control growing process, floating catalytic agent presoma volatilizees at cold zone, be carried to high-temperature zone (1200～1500 ℃) by carrier gas and be decomposed into metal catalyst, promote boron powder and boron oxide to mix the B that generates
2O
2Steam and ammonia gas react 15～90 minutes cool to room temperature again with the furnace, thus the control preparation pattern boron nitride quasi-one dimensional nanostructure different with structure.
Embodiment one
The floating catalytic agent is a ferrocene, it is 0.1 that the part by weight of its usage quantity and reactant (boron powder, boron oxide) summation closes, vaporization temperature is 150 ℃, ammonia flow is 100sccm, nitrogen flow is 300sccm, boron powder and boron oxide weight ratio 1: 4,1300 ℃ of temperature of reaction, 25 ℃/min of temperature rise rate, 1 hour reaction times.Obtain about about 50 nanometers of diameter, length is tens of microns ring shape boron nitride nano-tube, sees Fig. 1.Can be clearly seen that from high resolution picture (0002) is parallel to axial arrangement, its purity is 95%.
Embodiment two
The floating catalytic agent is a nickelocene, it is 0.2 that the part by weight of its usage quantity and reactant (boron powder, boron oxide) summation closes, the evaporation temperature is 200 ℃, ammonia flow is 50sccm, nitrogen flow is 150sccm, boron powder and boron oxide weight ratio 1: 4,1400 ℃ of temperature of reaction, 35 ℃/min of temperature rise rate, 1 hour reaction times.Obtain about about 100 nanometers of diameter, length is tens of microns folded cup-shaped boron nitride nanometer line, sees Fig. 2.Can be clearly seen that the arrangement perpendicular to axial direction of (0002) face from high resolution picture, its purity is 90%.
Embodiment three
The floating catalytic agent is a dicyclopentadienylcobalt, it is 0.2 that the part by weight of its usage quantity and reactant (boron powder, boron oxide) summation closes, the evaporation temperature is 300 ℃, ammonia flow is 50sccm, nitrogen flow is 200sccm, boron powder and boron oxide weight ratio 1: 7,1380 ℃ of temperature of reaction, 40 ℃/min of temperature rise rate, 1 hour reaction times.Obtain diameter Distribution in tens to 100 nanometers, length is tens of microns folded cup-shaped boron nitride nanometer line, and lamella and little nanotube that the surface has a lot of diauxic growths to come out are seen Fig. 3.Can verify the arrangement mode of said the embodiment two (0002) vertical axial from selected area electron diffraction, its purity is 90%.
Embodiment four
The floating catalytic agent is nickelocene and ferrocene mixture, it is 0.1 that the part by weight of its usage quantity and reactant (boron powder, boron oxide) summation closes, in the present embodiment, the two weight ratio of nickelocene and ferrocene is 1: 1, and the evaporation temperature is 300 ℃, ammonia flow is 150sccm, nitrogen flow is 50sccm, boron powder and boron oxide weight ratio 1: 7,1350 ℃ of temperature of reaction, 40 ℃/min of temperature rise rate, 1.5 hours reaction times.Obtain diameter Distribution in tens to 100 nanometers, length is the relative homogeneous boron nitride nanometer of tens of microns diameter line, and lamella and minor diameter nanofiber that the surface has a lot of diauxic growths to come out are seen Fig. 4, and its purity is 95%.
Embodiment five
The floating catalytic agent is dicyclopentadienylcobalt and ferrocene mixture, it is 0.4 that the part by weight of its usage quantity and reactant (boron powder, boron oxide) summation closes, in the present embodiment, the two weight ratio of dicyclopentadienylcobalt and ferrocene is 1: 5, and the evaporation temperature is 300 ℃, ammonia flow is 150sccm, nitrogen flow is 50sccm, boron powder and boron oxide weight ratio 1: 7,1350 ℃ of temperature of reaction, 40 ℃/min of temperature rise rate, 1.5 hours reaction times.Obtain diameter Distribution in tens to 100 nanometers, length is the relative homogeneous boron nitride nanometer of tens of microns diameter line, and the extremely thin lamella that the surface has a lot of diauxic growths to come out is seen Fig. 5, and its purity is 94%.
Claims (8)
1. the preparation method of a quasi one-dimensional boron nitride nanostructure, it is characterized in that: adopt the preparation of floating catalytic method, be to be nitrogenous source with the ammonia, nitrogen or argon gas are carrier gas, ferrocene, nickelocene, dicyclopentadienylcobalt or its mixture are floating catalytic agent presoma, amorphous boron powder and boron oxide powder are mixed into the boron source, processing parameter by the control growing process, floating catalytic agent presoma volatilizees at cold zone, be carried to the high-temperature zone by carrier gas and be decomposed into metal catalyst, promote boron powder and boron oxide to mix the B that generates
2O
2Steam and ammonia gas react, thereby the control preparation pattern boron nitride quasi-one dimensional nanostructure different with structure.
2. according to the described preparation method of claim 1, it is characterized in that: as the temperature range of the cold zone of evaporation floating catalytic agent at 100～300 ℃.
3. according to the described preparation method of claim 1, it is characterized in that: the weight ratio of boron powder and boron oxide between 1: 1～1: 7, finally in the temperature of reaction of high-temperature zone between 1200～1500 ℃.
4. according to the described preparation method of claim 1, it is characterized in that: it is 0.1～1 that the part by weight of floating catalytic agent and reactant boron powder, boron oxide summation closes.
5. according to the described preparation method of claim 1, it is characterized in that: the throughput ratio of carrier gas and nitrogenous source is between 4-0.25.
6. according to the described preparation method of claim 1, it is characterized in that: the gas flow of nitrogenous source is 50～500sccm.
7. according to the described preparation method of claim 1, it is characterized in that: at B
2O
2Constant temperature is 15～90 minutes under the temperature of reaction of steam and ammonia.
8. according to the described preparation method of claim 1, it is characterized in that: quasi-one dimensional nanostructure comprises ring shape boron nitride nano-tube, folded cup-shaped boron nitride nanometer line, and wherein the boron nitride nanometer line is along＜0001〉direction growth.
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