CN110040720A - High-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method - Google Patents
High-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method Download PDFInfo
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Abstract
The present invention relates to the structure control preparation field of carbon nanotube, specially a kind of high-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method.Using floating catalytic agent chemical vapour deposition technique, using toluene and ethylene as carbon source, ferrocene be catalyst precursor, sulphur is growth promoter, hydrogen is carrier gas growth carbon nanotube.Double-walled carbon nano-tube radical accounts for the 50~70% of the total radical of carbon nanotube in product, remaining is single-walled carbon nanotube.Product is heat-treated in air, unformed charcoal and single-walled carbon nanotube in oxidation removal product, the radical of double-walled carbon nano-tube accounts for 95% or more of the total radical of carbon nanotube after processing, and double-walled carbon nano-tube structural integrity, diameter integrated distribution concentrates oxidizing temperature to be greater than 800 DEG C in 1.8~2.3nm.Finally, high-purity, narrow diameter distribution, the preparation of minor diameter double-walled carbon nano-tube are realized.
Description
Technical field
The present invention relates to the structure control preparation field of carbon nanotube, specially a kind of high-purity, narrow diameter are distributed, are small straight
The preparation method of diameter double-walled carbon nano-tube.
Background technique
Double-walled carbon nano-tube is considered as one-dimensional hollow tubular structure made of coaxially being crimped as bilayer graphene, has
Good flexibility, the specific surface area of superelevation, excellent mechanics, electrical properties.Also, due to distinctive double-layer tube wall structure,
Compared to single-walled carbon nanotube, double-walled carbon nano-tube has higher mechanical strength, mass transfer diversification of forms between inside and outside wall, tool
There is the application field of richer multiplicity.Moreover, the outer wall of double-walled carbon nano-tube plays a protective role to inner layer tube wall, even if
Outer wall is functionalized to a certain degree, and the intact inner wall of structure still can keep good mechanical performance and electron transport performance (document
1Yao Zhao,Jinquan Wei,Robert Vajtai,Pulickel M.Ajayan&Enrique
V.Barrera.SCIENTIFIC REPORTS.1 (83): SEP 6 (2011)).Thus, double-walled carbon nano-tube can be to its outer wall
It is functionalized the compatibility to improve itself with other substances, and the excellent mechanical of single-walled carbon nanotube, electricity, heat can be kept
Etc. properties have tempting application potential.Therefore, it is necessary to develop the structure control technology of preparing of double-walled carbon nano-tube.
Chemical vapour deposition technique (document 2Guoqing Ning, Yi Liu, Fei Wei, Qian are supported currently, generalling use
Wen, Guohua Luo.J Phys Chem C, 2007,111:1969-1975) and floating catalytic agent chemical vapour deposition technique (text
Offer 3Jinquan Wei, Hongwei Zhu, Yi Jia, Qinke Shu, Chuangang Li, Kunlin Wang, Bingqing
Wei, Yanqiu Zhu, Zhicheng Wang, JianbinLuo, Wenjin Liu, Dehai Wu.CARBON.45 (11):
2152-2158 (2007), document 4Xiaohua Zhong, Yali Li, Jianmin Feng, Yanru Kang and
Shuaishuai Han.NANOSCALE.4 (18): 5614-5618 (2012)) double-walled carbon nano-tube is prepared.Support chemical gas
Phase sedimentation is needed catalyst loading on porous matrix, it is therefore desirable to which last handling process removes the carrying body in product, deposits
The problems such as introducing fault of construction during preparation process complexity, removal carrying body.Floating catalytic agent chemical vapour deposition technique is (floating
Dynamic method) it is that catalyst precursor is carried along into reaction zone, metallocene using carrier gas using organic luxuriant compound as catalyst precursor
Metal nanoparticle is decomposed and formed to compound in high-temperature region, and under optimum conditions, carbon source is decomposed on metallic particles, permeates, analysed
Double-walled carbon nano-tube out.Whole preparation process does not introduce other impurities, and can continuously prepare, thus be expected to prepare high quality,
The magnanimity double-walled carbon nano-tube of high-purity.However, that there are purity is lower, knot for the double-walled carbon nano-tube sample of floating current method growth
The problems such as structure homogeneity is poor, be relatively large in diameter (> 3nm), product is mostly the mixture of double-walled and other wall number carbon nanotubes, limit into
The performance and application study of one step.Currently, high-purity, the controllable preparation technology of minor diameter double-walled carbon nano-tube at home and abroad still belong to
Blank.Therefore it provides a kind of high-purity, high crystalline, high quality, diameter are uniform, minor diameter double-walled carbon nano-tube it is controllable
Standby technology has important academic significance and application value.
Summary of the invention
The object of the present invention is to provide a kind of high-purity, narrow diameters to be distributed, the preparation method of minor diameter double-walled carbon nano-tube,
Pass through thermodynamics and kinetics condition optimizing, growth course control and the subsequent weak oxide grown to minor diameter double-walled carbon nano-tube
The means that combine are handled, realize that high-purity, high crystalline, diameter be uniform, enrichment of minor diameter double-walled carbon nano-tube.
The technical scheme is that
A kind of high-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method, using floating catalytic agent chemistry
Vapour deposition process, using hydrogen as carrier gas, toluene and ethylene be carbon source, ferrocene is catalyst precursor, sulphur is that promotor carries out
The growth of carbon nanotube, double-walled carbon nano-tube radical accounts for the 50~70% of the total radical of carbon nanotube in products therefrom, remaining is single
Wall carbon nano tube；Then As-deposited state product is laid in horizontal tube furnace, in air in heat-treatment oxidation removal product
Agraphitic carbon and single-walled carbon nanotube, thus realize high-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube enrichment.
The high-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method, prepare the tool of carbon nanotube
Steps are as follows for body: under hydrogen protection, chemical vapor deposition horizontal tube furnace being warming up to 1100~1300 DEG C, by hydrogen stream
Amount is adjusted to 1000~3000sccm, is passed through 0.5~30sccm of ethylene, at the same with the rate of 0.5~1ml/h at the uniform velocity inject toluene,
The mixed solution that ferrocene, sulphur powder are formulated, mixed solution quality proportioning are 100:(3~5): (0.1~1) carries out carbon and receives
The growth of mitron, 0.5~5h of growth time.
The high-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method, it is preferred that protected in hydrogen
Under shield, chemical vapor deposition horizontal tube furnace is warming up to 1150~1250 DEG C, hydrogen flowing quantity is adjusted to 1700~
2400sccm is passed through 3~15sccm of ethylene, while at the uniform velocity injecting toluene, ferrocene, sulphur powder with the rate of 0.5~0.8ml/h and matching
Mixed solution made of system, mixed solution quality proportioning are 100:(3~5): (0.25~0.65) carries out the life of carbon nanotube
It is long, 0.5~2h of growth time.
The high-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method, by floating catalytic agent chemistry
The product of vapour deposition process preparation is placed in the horizontal tube furnace of air at room temperature atmosphere, then by horizontal tube furnace with 10~
The rate of 20 DEG C/min is warming up to 500~540 DEG C and constant temperature 0.5~3 hour, and product is with furnace cooled to room temperature.
The high-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method, double wall carbon nano-tubes in product
Manage highly enriched, radical accounts for 95% or more of the total radical of carbon nanotube, and diameter is uniform, and 85% or more is straight in double-walled carbon nano-tube
Diameter integrated distribution is in 1.8~2.3 nanometer ranges.
The high-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method, double-walled carbon nano-tube crystallization
Property it is high, defect is few, and oxidizing temperature is concentrated to be greater than 800 DEG C.
Design philosophy of the invention is:
The present invention has this intrinsic physical property of higher reactivity using minor diameter single-walled carbon nanotube, proposes double-walled
What carbon nano tube growth condition optimizing was combined with weak oxide processing in air opens one's minds to prepare high-purity minor diameter double-walled
Carbon nanotube.That is: it first passes through control thermodynamics and kinetics condition and prepares minor diameter single-walled carbon nanotube and double wall carbon nano-tubes
The mixture of pipe, then weak oxide handles oxidation removal single-walled carbon nanotube through the air, and does not destroy double-walled carbon nano-tube
Structure.While the present invention finally realizes minor diameter double-walled carbon nano-tube controllable preparation, the purity of double-walled carbon nano-tube is improved, is protected
The intrinsic carbon-coating structural intergrity of double-walled carbon nano-tube is held, acquisition high-purity, outer wall is pure, carbon impurity content is few and diameter is equal
One minor diameter double-walled carbon nano-tube.
The invention has the advantages and beneficial effects that:
1, the present invention uses floating catalytic agent chemical vapour deposition technique, prepares double-walled carbon nano-tube first and receives with single wall carbon
Mitron mix products, then under preference temperature, air atmosphere to product carry out weak oxide processing, remove product in carbon impurity and
Single-walled carbon nanotube, finally realize high-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube it is highly enriched, product carbon is received
Double-walled carbon nano-tube content is 95% or more in mitron.
2, the double-walled carbon nano-tube diameter that the present invention obtains is uniform, and 85% diameter above integrated distribution is in 1.8~2.3 nanometers
It is suitable with the diameter of single-wall carbon nano tube of general floating catalytic agent chemical vapour deposition technique preparation in range, but double-layer tube wall has
There are stronger mechanical strength, higher stability, richer functionalized form, more with potential applications, the present invention obtains double
Wall carbon nano tube structural integrity, crystallinity are high, defect is few.
3, the present invention is based on the preparations of floating catalytic agent chemical vapour deposition technique and low temperature weak oxide to post-process the side combined
Formula, entire process flow is simple, is easy to repetition and prepare with scale.
Detailed description of the invention
The stereoscan photograph of carbon nanotube prepared by Fig. 1 embodiment 1.Wherein, (a) figure is As-deposited state carbon nanotube；
(b) figure is weak oxide treated carbon nanotube.
The high-resolution-ration transmission electric-lens photo of carbon nanotube prepared by Fig. 2 embodiment 1.Wherein, (a) figure is that As-deposited state carbon is received
Mitron；(b) figure is weak oxide treated carbon nanotube.
1 weak oxide of Fig. 3 embodiment treated double-walled carbon nano-tube diameter distribution statistics figure.
The thermogravimetric curve of carbon nanotube prepared by Fig. 4 embodiment 1.Wherein, (a) figure is As-deposited state carbon nanotube；(b) figure
For weak oxide treated carbon nanotube.In figure, abscissa Temp is represented temperature (DEG C), left ordinate Mass representation quality percentage
Number (%), right ordinate DSC represent heat flow rate (mW/mg).
Specific embodiment
In the specific implementation process, before the present invention using hydrogen as carrier gas, toluene and ethylene is carbon source, ferrocene is catalyst
Body, sulphur are driven as growth promoter, the growth of carbon nanotube is carried out, then As-deposited state product is laid in horizontal tube furnace,
By the way of being heat-treated in air, in-situ oxidation removes the agraphitic carbon and single-walled carbon nanotube in product, to realize
High-purity, narrow diameter distribution, the enrichment of minor diameter double-walled carbon nano-tube.With optimal conditions, double-walled carbon is received in As-deposited state product
Mitron radical accounts for the 50~70% of the total radical of carbon nanotube, remaining is single-walled carbon nanotube；After weak oxide processing, double wall carbon nano-tubes
Pipe radical accounts for 95% or more of the total radical of carbon nanotube.Uniform (85% or more the double-walled carbon nano-tube of the diameter of double-walled carbon nano-tube
Diameter integrated distribution is in 1.8~2.3 nanometers), crystallinity is high, and defect is few, and oxidizing temperature is concentrated to be greater than 800 DEG C.
In the following, the present invention is described in further detail by embodiment and attached drawing.
Embodiment 1.
Toluene, ferrocene, the sulphur powder mixed solution that mass ratio is 100:3:0.25 are prepared first, and ultrasonic treatment 10 minutes standby
With.Under small flow hydrogen shield, chemical vapor deposition horizontal tube furnace is warming up to 1200 DEG C, then by hydrogen flowing quantity tune
To 1800sccm, and be passed through 7sccm ethylene, at the same with the rate of 0.6ml/h at the uniform velocity inject toluene, ferrocene, sulphur powder prepare and
At mixed solution, carry out the growth of carbon nanotube, growth time 1h.
The As-deposited state product that above-mentioned steps obtain is laid in the horizontal tube furnace flat-temperature zone center of both ends open, then
Horizontal tube furnace is warming up to 530 DEG C, and constant temperature 2 hours with the rate of 15 DEG C/min, weak oxide in situ removes in product
Amorphous carbon and single-walled carbon nanotube, sample is with furnace cooled to room temperature later.
Using scanning electron microscope and transmission electron microscope, to As-deposited state and weak oxide, treated that sample characterizes.As shown in Figure 1,
(Fig. 1 b) sample is all very pure after scanning electron microscope characterization display As-deposited state (Fig. 1 a) and weak oxide processing, and carbon pipe surface is without particle
Shape impurity.As shown in Fig. 2, transmission electron microscope characterization discovery, As-deposited state sample (Fig. 2 a) are the mixing of single wall and double-walled carbon nano-tube
Object counts the wall number and radical of carbon nanotube under transmission electron microscope, and double-walled carbon nano-tube radical accounts for carbon and receives as the result is shown
Total 65% or more the radical of mitron；After weak oxide processing (Fig. 2 b), single-walled carbon nanotube is greatly decreased, and double-walled carbon nano-tube accounts for carbon and receives
97% or more of the total radical of mitron, double-walled carbon nano-tube all has complete carbon-coating structure to weak oxide before and after the processing.Such as Fig. 3 institute
Show, 100 double-walled carbon nano-tube diameters are measured under transmission electron microscope and draws diameter distribution profile, the distribution of double-walled carbon nano-tube diameter
In in 1.7~3.1 nanometer ranges, wherein 88% double-walled carbon nano-tube diameter integrated distribution is in 1.8~2.3 nanometers, double-walled carbon
The concentration oxidizing temperature of nanotube is 805 DEG C.
Thermogravimetric analysis is carried out to As-deposited state and weak oxide treated sample, with characterize magnanimity sample crystallinity variation and
Purity.As shown in figure 4, the mass percent curve of As-deposited state carbon nanotube (Fig. 4 a) is in 450~550 DEG C and 750~820 DEG C two
There is obvious weightless, the weightlessness of corresponding mass percentage curve in a temperature range, and the multiple discrete exothermic peaks of DSC curve appearance are right
Answer the oxidative decomposition of carbonaceous product.Wherein, under lower temperature (450~550 DEG C) generation oxidative decomposition be reaction
The higher amorphous carbon of activity and minor diameter single-walled carbon nanotube, (750~820 DEG C) generation oxidative decompositions under higher temperature
Be double-walled carbon nano-tube；The mass percent curve of sample (Fig. 4 b) goes out in 750~820 DEG C of temperature ranges after weak oxide processing
Existing weightlessness, the weightlessness of corresponding mass percentage curve, DSC curve is in 805 DEG C or so appearance, one obvious exothermic peak, corresponding double-walled
The decomposition reaction of carbon nanotube illustrates the high crystalline and structural homogeneity of double-walled carbon nano-tube.Compare As-deposited state and weak oxide
Treated carbon nanotube thermal gravimetric analysis results, the oxygenolysis temperature of double-walled carbon nano-tube and weak oxygen in As-deposited state carbon nanotube
Change treated double-walled carbon nano-tube oxygenolysis temperature without significant difference, shows weak oxide treatment process to double-walled carbon nano-tube
Structure destroy it is minimum, this is consistent with transmission electron microscope characterization result.In addition, carbon nanotube-sample after As-deposited state and weak oxide processing
Impurity residual quantity be respectively 4.5wt% and 7wt%, show the high-purity of sample, this is consistent with the characterization result of scanning electron microscope.
Embodiment 2.
Toluene, ferrocene, the sulphur powder mixed solution that mass ratio is 100:3:0.19 are prepared first, and ultrasonic treatment 10 minutes standby
With.Under small flow hydrogen shield, chemical vapor deposition horizontal tube furnace is warming up to 1100 DEG C, then by hydrogen flowing quantity tune
To 1500sccm, and be passed through 8sccm ethylene, at the same with the rate of 0.6ml/h at the uniform velocity inject toluene, ferrocene, sulphur powder prepare and
At mixed solution, carry out the growth of carbon nanotube, growth time 2h.
The As-deposited state product that above-mentioned steps obtain is laid in the horizontal tube furnace flat-temperature zone center of both ends open, then
Horizontal tube furnace is warming up to 530 DEG C of constant temperature 1.5 hours with the rate of 10 DEG C/min, the nothing in weak oxide removal product in situ
Shape carbon and single-walled carbon nanotube, and sample is with furnace cooled to room temperature later.
Using scanning electron microscope and transmission electron microscope, to As-deposited state and weak oxide, treated that sample characterizes, scanning electron microscope table
Sign display, treated that sample is all very pure for As-deposited state and weak oxide, carbon pipe surface grainless impurity；Transmission electron microscope characterization
It has been shown that, weak oxide processing promote double-walled carbon nano-tube radical accounting in carbon nanotube to 95% or more by 58%.Double-walled carbon
Tube diameters are distributed in 1.7~2.5 nanometer ranges, wherein 85% double-walled carbon nano-tube diameter is distributed in 1.8~2.3 and receives
Rice.The concentration oxidizing temperature of double-walled carbon nano-tube is 801 DEG C.
Embodiment 3.
Toluene, ferrocene, the sulphur powder mixed solution that mass ratio is 100:5:0.35 are prepared first, and ultrasonic treatment 10 minutes standby
With.Under small flow hydrogen shield, chemical vapor deposition horizontal tube furnace is warming up to 1150 DEG C, then by hydrogen flowing quantity tune
To 1500sccm, and be passed through 8sccm ethylene, at the same with the rate of 0.6ml/h at the uniform velocity inject toluene, ferrocene, sulphur powder prepare and
At mixed solution, carry out the growth of carbon nanotube, growth time 2h.
The As-deposited state product that above-mentioned steps obtain is laid in the horizontal tube furnace flat-temperature zone center of both ends open, then
Horizontal tube furnace is warming up to 515 DEG C of constant temperature 2.5 hours with the rate of 15 DEG C/min, the nothing in weak oxide removal product in situ
Shape carbon and single-walled carbon nanotube, and sample is with furnace cooled to room temperature later.
Using scanning electron microscope and transmission electron microscope, to As-deposited state and weak oxide, treated that sample characterizes, scanning electron microscope table
Sign display, treated that sample is all very pure for As-deposited state and weak oxide, carbon pipe surface grainless impurity；Transmission electron microscope characterization
It has been shown that, weak oxide processing promote double-walled carbon nano-tube radical accounting in carbon nanotube to 96% or more by 62%.Double-walled carbon
Tube diameters are distributed in 1.7~3.0 nanometer ranges, wherein 85% double-walled carbon nano-tube diameter is distributed in 1.8~2.3 and receives
Rice.The concentration oxidizing temperature of double-walled carbon nano-tube is 802 DEG C.
Comparative example 1.
Toluene, ferrocene, the sulphur powder mixed solution that mass ratio is 100:2:0.95 are prepared first, and ultrasonic treatment 10 minutes standby
With.Under small flow hydrogen shield, chemical vapor deposition horizontal tube furnace is warming up to 1200 DEG C, then by hydrogen flowing quantity tune
To 1500sccm, and be passed through 5sccm ethylene, at the same with the rate of 0.9ml/h at the uniform velocity inject toluene, ferrocene, sulphur powder prepare and
At mixed solution, carry out the growth of carbon nanotube, growth time 2h.
Transmission electron microscope characterization display, products therefrom double-walled carbon nano-tube radical account for 35% or more of the total radical of carbon nanotube,
Remaining is single-walled carbon nanotube, and double-walled carbon nano-tube diameter is distributed in 2~3.5 nanometers, and carbon nano tube surface adheres to a large amount of impurity
Charcoal.The double-walled carbon nano-tube of high-purity can not be obtained by carrying out weak oxide processing to this sample.
Comparative example 2.
Toluene, ferrocene, the sulphur powder mixed solution that mass ratio is 100:2:0.38 are prepared first, and ultrasonic treatment 10 minutes standby
With.Under small flow hydrogen shield, chemical vapor deposition horizontal tube furnace is warming up to 1150 DEG C, then by hydrogen flowing quantity tune
To 2000sccm, and be passed through 5sccm ethylene, at the same with the rate of 1.2ml/h at the uniform velocity inject toluene, ferrocene, sulphur powder prepare and
At mixed solution, carry out the growth of carbon nanotube, growth time 1h.
Transmission electron microscope characterization shows that different wall number carbon nanotube radical accountings are respectively as follows: single in products therefrom
Pipe accounting 98%, double-walled carbon nano-tube accounting 1%, three wall carbon nano tube accountings 1%.
Embodiment and comparative example the result shows that, the present invention can pass through regulation floating catalytic agent chemical vapor deposition growth carbon
The thermodynamics and kinetics condition of nanotube realizes high-purity, high level minor diameter double-walled carbon nano-tube (> 50%) and single wall
The controllable preparation of carbon nanotube mixture can largely prepare high-purity, narrow diameter is distributed, is small in conjunction with subsequent airoxidation
The double-walled carbon nano-tube of diameter, and the double-walled carbon nano-tube structural integrity, the crystallinity that finally obtain are high, purity is high.Work of the present invention
Skill process is simple, is easy to repetition and prepare with scale.
Claims (6)
1. the preparation method of the distribution of a kind of high-purity, narrow diameter, minor diameter double-walled carbon nano-tube, which is characterized in that using floating
Catalyst chemical gas phase deposition method, using hydrogen as carrier gas, toluene and ethylene be carbon source, ferrocene is catalyst precursor, sulphur is
Promotor carries out the growth of carbon nanotube, in products therefrom double-walled carbon nano-tube radical account for the total radical of carbon nanotube 50~
70%, remaining is single-walled carbon nanotube；Then As-deposited state product is laid in horizontal tube furnace, is heat-treated oxygen in air
Change the agraphitic carbon and single-walled carbon nanotube in removal product, to realize that high-purity, narrow diameter distribution, minor diameter double-walled carbon are received
The enrichment of mitron.
2. the preparation method of the distribution of high-purity described in accordance with the claim 1, narrow diameter, minor diameter double-walled carbon nano-tube, special
Sign is that preparing carbon nanotube, specific step is as follows: under hydrogen protection, chemical vapor deposition horizontal tube furnace being heated up
To 1100~1300 DEG C, hydrogen flowing quantity is adjusted to 1000~3000sccm, is passed through 0.5~30sccm of ethylene, while with 0.5~
The rate of 1ml/h at the uniform velocity injects the mixed solution that toluene, ferrocene, sulphur powder are formulated, and mixed solution quality proportioning is 100:
(3~5): (0.1~1) carries out the growth of carbon nanotube, 0.5~5h of growth time.
3. according to claim 2 high-purity, narrow diameter distribution, minor diameter double-walled carbon nano-tube preparation method, it is special
Sign is, it is preferred that under hydrogen protection, chemical vapor deposition horizontal tube furnace is warming up to 1150~1250 DEG C, by hydrogen
Throughput is adjusted to 1700~2400sccm, is passed through 3~15sccm of ethylene, while at the uniform velocity injecting first with the rate of 0.5~0.8ml/h
The mixed solution that benzene, ferrocene, sulphur powder are formulated, mixed solution quality proportioning are 100:(3~5): (0.25~0.65), into
The growth of row carbon nanotube, 0.5~2h of growth time.
4. the preparation method of the distribution of high-purity described in accordance with the claim 1, narrow diameter, minor diameter double-walled carbon nano-tube, special
Sign is, product prepared by floating catalytic agent chemical vapour deposition technique is placed in the horizontal tube furnace of air at room temperature atmosphere,
Horizontal tube furnace is then warming up to 500~540 DEG C and constant temperature 0.5~3 hour with the rate of 10~20 DEG C/min, product with
Furnace cooled to room temperature.
5. being distributed according to high-purity described in one of Claims 1-4, narrow diameter, the preparation side of minor diameter double-walled carbon nano-tube
Method, which is characterized in that double-walled carbon nano-tube is highly enriched in product, and radical accounts for 95% or more of the total radical of carbon nanotube, and straight
Diameter is uniform, and 85% diameter above integrated distribution is in 1.8~2.3 nanometer ranges in double-walled carbon nano-tube.
6. being distributed according to high-purity described in one of Claims 1-4, narrow diameter, the preparation side of minor diameter double-walled carbon nano-tube
Method, which is characterized in that double-walled carbon nano-tube crystallinity is high, and defect is few, and oxidizing temperature is concentrated to be greater than 800 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498833A (en) * | 2020-06-03 | 2020-08-07 | 中国科学院化学研究所 | Double-wall carbon nanoring material and preparation method and application thereof |
| WO2023173357A1 (en) * | 2022-03-14 | 2023-09-21 | 无锡东恒新能源科技有限公司 | Method for synthesizing thin-walled carbon nanotube |
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