CN103663411B - A kind of high yield synthetic method of double-helix carbon nanotube - Google Patents
A kind of high yield synthetic method of double-helix carbon nanotube Download PDFInfo
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Abstract
The invention discloses a kind of high yield synthetic method of double-helix carbon nanotube, it is characterized in that: comprise following steps: (1) is by FeCl
24H
2o, citric acid particle and dehydrated alcohol mix according to the quantitative proportion of 1mol:1.5mol:100mL, after stirring in water bath, by gained colloidal sol in an oven thermal treatment until obtain xerogel; (2) by the thermal treatment of gained xerogel, required catalyst precursor powder is obtained; (3) gained powder is laid in little porcelain boat, under the protection of argon gas, temperature of reaction is increased to 450 DEG C by room temperature; close argon gas and switch immediately and pass into hydrogen 1 hour; close hydrogen and switch immediately and pass into acetylene and water vapour 2 hours, be cooled to room temperature, collect black sample.Transmission electron microscope and the field emission microscopy observation result of sample show: synthesized sample is the double-helix carbon nanotube of highly selective.Compared with current International reporting data (8.3), the double-helix carbon nanotube productive rate that the program obtains has had large increase.
Description
Technical field
The invention belongs to carbon nanotube preparation technology, particularly relate to a kind of high yield preparation method of double-helix carbon nanotube.
Background technology
Spirrillum carbon nanomaterial can regard that introducing portion carbon pentagon and carbon heptagon are formed in carbon hexagonal mesh as, is a kind of chiral material.If theoretical investigation shows there is electric current by single spiral carbon nanomaterial, inducedmagnetic field can be produced.Thus, spiral carbon nanomaterial also exists very large potentiality application in micro electric magnetic wave nanometer transmodulator and nanotube switch.In addition, a large amount of theoretical investigation work shows that spiral carbon nanomaterial not only possesses the process based prediction model of carbon nanomaterial intrinsic, but also has the advantage that himself spirane structure brings.The electrons transport property of its helicity to carbon nanomaterial has decisive role, along with the change of helicity, it can show metal, semi-conductor, or even semi-metal characteristic, nanometer spring, miniature antenna, biologically active agent or passivator, energy converter, microsensor and nanometer telefault etc. can be used as.The physics of spiral carbon nanomaterial excellence, chemical property and huge using value, make the synthesis of this kind of material enjoy paying close attention to of domestic and international researcher in recent years always, up to the present, although had much about the report of spiral carbon nanomaterial synthesis technique.But lower experiment productive rate has seriously fettered its applied research and product development.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of method that highly selective double-helix carbon nanotube high yield synthesizes, to solve the problem such as applied research and product development that prior art is brought in double-helix carbon nanotube low-yield.
Technical scheme of the present invention is: a kind of high yield synthetic method of double-helix carbon nanotube, comprises following steps: (1) is by FeCl
24H
2o, citric acid particle and dehydrated alcohol mix according to the quantitative proportion of 1mol:1.5mol:100mL, after stirring in water bath, by gained colloidal sol in an oven thermal treatment until obtain xerogel; (2) by the thermal treatment of gained xerogel, required catalyst precursor powder is obtained; (3) gained powder is laid in little porcelain boat, under the protection of argon gas, temperature of reaction is increased to 450 DEG C by room temperature; close argon gas and switch immediately and pass into hydrogen 1 hour; close hydrogen and switch immediately and pass into acetylene and water vapour 2 hours, be cooled to room temperature, collect black sample.
In step (1), bath temperature is 60 DEG C, and the time is 6 hours.
Thermal treatment temp in step (2) is 450 DEG C, thermal treatment 4 hours.
Beneficial effect of the present invention: the object of the invention is the experimental analysis by system and summary, designs the high yield synthetic schemes of a set of highly selective double-helix carbon nanotube, for basic substance is established in the real application research of this kind of advanced function material and exploitation.The present invention utilizes sol-gel method to prepare ferric oxide nanometer particle, is assisted the high yield synthetic technological condition of the technique study duplex carbon nanomaterial of iron nano-particle In-stiu catalysis acetylene by hydrogen reduction method and distilled water.Result of study shows: the introducing of water vapour greatly enhances the catalytic performance of iron nano-particle, compared with value reported before, the productive rate of synthesized double-helix carbon nanotube (
) be greatly improved.
Advantage of the present invention utilizes distilled water as the auxiliary of catalyzer iron nano-particle, both greatly increased the productive rate of double-helix carbon nanotube, and ensure that again the highly selective of double-helix carbon nanotube well.Thus, compared with processing condition reported before, this synthetic schemes ensure that high yield and the highly selective of double-helix carbon nanotube well simultaneously.
Method of the present invention is the productive rate that the catalytic chemical vapor deposition technique utilizing distilled water to assist improves double-helix carbon nanotube.By regulating and controlling the processing parameters such as the introducing speed of water vapour, realize the high yield synthesis of highly selective double-helix carbon nanotube.Compare with the report of patent with pertinent literature before, great advantage of the present invention is the auxiliary having used distilled water as transition group metal catalyst dexterously, the regulation and control of parameter by experiment, under the highly selective prerequisite ensureing double-helix carbon nanotube, greatly increase the productive rate of this kind of functional materials, for the real application research of the type functional materials and exploitation provide experiment basis.
Need to utilize following instrument to carry out thing phase and structural characterization, analysis with sample prepared by the present invention: D/Max-RA type rotary-anode X-ray diffractometer (XRD) that sample thing adopts Japanese Rigaku company to manufacture mutually carries out analyzing (CuK α); The Sirion field emission scanning electron microscope (FE-SEM) that product pattern adopts FEI Co. to produce and JEOL-2010 type high resolution transmission electron microscopy (HRTEM) characterize.
The present invention is on the basis utilizing iron nano-particle catalytic pyrolysis acetylene synthesis highly selective double-helix carbon nanotube, by the introducing of water vapour, make use of the auxiliary catalysis effect of distilled water dexterously, under the prerequisite ensureing double-helix carbon nanotube highly selective, improve the productive rate of this kind of spiral carbon nanomaterial, for the practical application of this kind of material has established solid experiment basis with exploitation.
In order to solve the problem that double-helix carbon nanotube low-yield is brought well, the catalystic pyrolysis that the present invention adopts distilled water auxiliary, improves the synthetic yield of double-helix carbon nanotube effectively.Compared with numerical value reported before, the yield value that the present invention reports has exceeded similar numerical value reported in the world at present.First the present invention focuses on the improvement of sample synthetic technological condition, and its innovation is, by using distilled water as auxiliary dexterously, effectively to promote the catalytic performance of catalyzer, thus improve the productive rate of synthesized double-helix carbon nanotube.Compared with current International reporting data (8.3), the double-helix carbon nanotube productive rate that the program obtains has had large increase.
Accompanying drawing explanation
Fig. 1 is field emission scanning electron microscope (FE-SEM) and transmission electron microscope (TEM) photo of synthesized sample.
Embodiment
Be below example of the present invention (in example, agents useful for same is chemical pure), this experimentation mainly completes in two steps:
The first step: first by 1molFeCl
24H
2o (Iron dichloride tetrahydrate), 1.5mol citric acid particle mix, add 100mL dehydrated alcohol wherein, gained mixture put into three-necked bottle 60 ° of C stirring in water bath after 6 hours, by the 80 ° of C thermal treatments after 6 hours in an oven of gained colloidal sol, then be warming up to 150 ° of C thermal treatments until obtain corresponding xerogel; Gained xerogel can be obtained required catalyst precursor powder 450 ° of C thermal treatments in atmosphere in High Temperature Furnaces Heating Apparatus after 4 hours;
Second step: a certain amount of catalyst precursor powder (50mg) to be laid in little porcelain boat and to push in tubular quartz pipe to tube furnace thermocouple location place, under the provide protection of argon gas, temperature of reaction being increased to 450 ° of C by room temperature; Close argon gas afterwards and switch immediately and pass into hydrogen, by ferric oxide nanometer particle after hydrogen atmosphere situ reduces 1 hour, close hydrogen and switch immediately and pass into acetylene and water vapour (distilled water 30 ° of C heating in water bath), iron nano-particle surface in situ catalytic pyrolysis acetylene 2 hours, after whole device is cooled to room temperature, a large amount of black sample (1.44g) can be collected in little porcelain boat.
Fig. 1 a is the FE-SEM photo of this sample, is the duplex carbon nanomaterial of highly selective by the known synthesized sample of the systematic observation of FE-SEM.Fig. 1 b gives the TEM photo of this sample, and the nanotubes structure of sample can clearly be observed.Thus, the scanning electron microscope of sample and transmission electron microscope show that synthesized sample is the double-helix carbon nanotube of highly selective.
Table 1: the repeatability of contrast experiment
Claims (3)
1. a high yield synthetic method for double-helix carbon nanotube, is characterized in that: comprise following steps:
(1) by FeCl
24H
2o, citric acid particle and dehydrated alcohol mix according to the quantitative proportion of 1mol:1.5mol:100mL, after stirring in water bath, by gained colloidal sol in an oven thermal treatment until obtain xerogel; (2) by the thermal treatment of gained xerogel, required catalyst precursor powder is obtained; (3) gained powder is laid in little porcelain boat, under the protection of argon gas, temperature of reaction is increased to 450 DEG C by room temperature; close argon gas and switch immediately and pass into hydrogen 1 hour; close hydrogen and switch immediately and pass into acetylene and water vapour 2 hours, be cooled to room temperature, collect black sample.
2. the high yield synthetic method of a kind of double-helix carbon nanotube according to claim 1, is characterized in that: in step (1), bath temperature is 60 DEG C, and the time is 6 hours.
3. the high yield synthetic method of a kind of double-helix carbon nanotube according to claim 1, is characterized in that: the thermal treatment temp in step (2) is 450 DEG C, thermal treatment 4 hours.
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| CN101885484A (en) * | 2010-07-14 | 2010-11-17 | 南京大学 | Method for synthesizing carbon nanobelts and spiral carbon nanotubes simultaneously |
| CN102424377A (en) * | 2011-09-15 | 2012-04-25 | 西南交通大学 | Method for preparing coiled carbon nanotube macroscopic body |
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| CN101885484A (en) * | 2010-07-14 | 2010-11-17 | 南京大学 | Method for synthesizing carbon nanobelts and spiral carbon nanotubes simultaneously |
| CN102424377A (en) * | 2011-09-15 | 2012-04-25 | 西南交通大学 | Method for preparing coiled carbon nanotube macroscopic body |
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