CN103030120A - Fabrication method of boron-carbon-nitrogen nanotube - Google Patents
Fabrication method of boron-carbon-nitrogen nanotube Download PDFInfo
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- CN103030120A CN103030120A CN2012105931091A CN201210593109A CN103030120A CN 103030120 A CN103030120 A CN 103030120A CN 2012105931091 A CN2012105931091 A CN 2012105931091A CN 201210593109 A CN201210593109 A CN 201210593109A CN 103030120 A CN103030120 A CN 103030120A
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Abstract
The invention relates to a compound containing boron and nitrogen, and discloses a fabrication method for synthesizing a boron-carbon-nitrogen nanotube with a chemical vapour deposition method. The fabrication method comprises the steps that a nickel oxide-sodium chloride catalyst precursor is prepared and placed in a quartz boat; the quartz boat is placed in a constant temperature area of a horizontal tube furnace; hydrogen is supplied; the temperature is raised and kept; hydrogen is shut down; a gas mixture of nitrogen, methyl borate vapour and methane is continuously supplied to the tube furnace; a chemical vapour deposition reaction is conducted; boron-carbon-nitrogen nanotube-sodium chloride composite powder is prepared; the powder is put into a deionized water solution of sodium dodecyl benzene sulfonate; sodium chloride is dissolved completely through ultrasonic dispersion; a precipitate in the solution is filtered; washing and drying are conducted; and the purified boron-carbon-nitrogen nanotube is fabricated. The fabrication method overcomes the defects in the prior art that the boron and nitrogen doped carbon nanotube is poor in crystal form, and low in doping efficiency and purity, and the boron-carbon-nitrogen nanotube is difficult in purification and dispersion.
Description
Technical field
Technical scheme of the present invention relates to boracic and nitrogen compound, specifically the preparation method of boron-carbon nanotube.
Background technology
Boron-carbon nanotube can be regarded the product that part carbon atom in the graphite network is replaced by boron or nitrogen-atoms as, and the B-C-N ternary compound is between hexagonal boron nitride and graphite-structure.Though its morphological structure and carbon nanotube have similarity, it has mechanical property and the electric property more excellent than carbon nanotube, and higher resistance of oxidation is arranged, and mechanical property and electric property be not subjected to the impact of its diameter, and is only relevant with its composition.Therefore, boron-carbon nanotube has physics and the mechanical property better than carbon nanotube, has a wide range of applications at matrix material, magneticsubstance, luminescent material and electronic material numerous areas.Although boron-carbon nanotube has many advantageous properties, the bottleneck that the restriction boron-carbon nanotube is used is its preparation difficulty, and synthetic yield is lower, and building-up process is difficult to control.
In the prior art, the main method of preparation boron-carbon nanotube has arc discharge method, plasma evaporation method, heated filament vapour deposition process and pyrolysis method, under different preparation conditions, by catalyzer, carbon source, boron source and nitrogenous source, prepared and come in every shape and the element different boron-carbon nanotube that distributes.CN101718731B discloses boron-carbon nanotube/semiconductor oxide composite and preparation method thereof, wherein boron-carbon nanotube by catalyzer, contain boron material and carbon nanotube is made in ammonia atmosphere; CN100354202C has reported a kind of method for preparing at low temperatures boron-carbon nanotube, with KBH
4, NH
4Cl, ZnBr
2With benzene be that starting material prepare boron-carbon nanotube in stainless steel cauldron; CN101718732B has disclosed carbon doped boron-nitrogen nanotube/semiconductor oxide matrix material and preparation method thereof, wherein adopts catalyzer, synthetic in ammonia after containing boron material and carbon nanotube and grinding, and purifies, obtains carbon doped boron-nitrogen nanotube after the roasting.Although above-mentioned prior art adopts the whole bag of tricks to realize the synthetic and control of boron-carbon nanotube, the shortcoming that exists is: the boron-carbon nanotube crystal formation that prepare (1) is relatively poor, doping efficiency and purity are low; (2) synthesis condition is relatively harsher, is unsuitable for the volume production of boron-carbon nanotube; (3) purification of boron-carbon nanotube is large with the dispersion difficulty.Therefore, seek that a kind of synthesis route is simple, crystal formation good, productive rate and purity are high, purify and disperse easy boron-carbon nanotube preparation method significant for its widespread use of promotion.
Summary of the invention
Technical problem to be solved by this invention is: the preparation method that boron-carbon nanotube is provided, a kind of preparation method by the synthetic boron-carbon nanotube of chemical Vapor deposition process, on preparation nickel oxide-sodium-chlor catalyzer precursor basis, prepare boron-carbon nanotube-sodium-chlor powder by chemical vapor deposition method, and then the acquisition boron-carbon nanotube of purifying, boron and nitrogen-doped carbon nanometer pipe poor crystal form in the prior art have been overcome, doping efficiency and purity are low, and the shortcoming that boron-carbon nanotube is purified and the dispersion difficulty is large.
The present invention solves this technical problem the technical scheme that adopts: the preparation method of boron-carbon nanotube is a kind of preparation method by the synthetic boron-carbon nanotube of chemical Vapor deposition process, and concrete steps are as follows:
The first step, preparation nickel oxide-sodium-chlor catalyzer precursor
It is nickelous nitrate by weight: the ratio of sodium-chlor=0.02～0.55:1, take by weighing Nickelous nitrate hexahydrate and the sodium-chlor of institute's expense, under the induction stirring state, the sodium-chlor that takes by weighing is dissolved in the deionized water by the concentration of 50～80g/L, then the Nickelous nitrate hexahydrate that takes by weighing is dissolved in the above-mentioned deionized water, continue induction stirring until sodium-chlor and Nickelous nitrate hexahydrate dissolve fully, place Constant Temp. Oven in 60～90 ℃ of drying 48～96h mentioned solution, evaporate fully to moisture, then nickelous nitrate and the sodium-chlor crystalline mixture that obtains after the drying placed ball grinder, adopt planetary ball mill with speed ball milling 3～6h of 500～1000r/min, above-mentioned mixture after ball-milling processing is placed quartzy Noah's ark, should place the horizontal pipe furnace flat-temperature zone by the quartz Noah's ark, flow velocity with 180～240ml/min continues to pass into nitrogen and is warming up to 350～600 ℃ in this tube furnace, insulation 2～4h, make this tube furnace till cool to room temperature under the nitrogen atmosphere of 180～240ml/min flow velocity, make nickel oxide-sodium-chlor catalyzer precursor;
Second step, preparation boron-carbon nanotube-sodium-chlor composite powder
The nickel oxide that the first step is made-sodium-chlor catalyzer precursor places quartzy Noah's ark, should place the horizontal pipe furnace flat-temperature zone by the quartz Noah's ark, flow velocity with 180～240ml/min passes into hydrogen and is warming up to 550～750 ℃ in this tube furnace, insulation 1.5～3.5h, then close hydrogen, be nitrogen with volume ratio again: methyl-borate steam: the gas mixture of methane=4～8:0.5～1:1 continues to pass in this tube furnace with the flow velocity of 330～600ml/min, under 550～750 ℃, carry out chemical vapour deposition reaction 0.5～1.5h, close afterwards methyl-borate steam and methane and adjust nitrogen flow, make above-mentioned tube furnace till cool to room temperature under the nitrogen atmosphere of 180～240ml/min flow velocity, make thus boron-carbon nanotube-sodium-chlor composite powder, wherein the quality percentage composition of boron-carbon nanotube is 5.1～17.6%;
The 3rd step, the purification boron-carbon nanotube
The boron-carbon nanotube that second step is made by the concentration of 2～5g/L-sodium-chlor composite powder is put into the deionized water solution that mass percent concentration is 0.3～1.0% Sodium dodecylbenzene sulfonate, place the ultra-sonic dispersion instrument to disperse 10～20min that sodium-chlor is dissolved fully with the ultrasonic wave of 30kHz～40kHz in the beaker that mentioned solution is housed, throw out in the solution is filtered, with washed with de-ionized water 3～4 times, then use Constant Temp. Oven in 80～90 ℃ of drying 2～4h, namely make the boron-carbon nanotube after the purification.
The preparation method of above-mentioned boron-carbon nanotube, related starting material are all by commercially available, and used equipment and process all is that those skilled in the art are known.
The invention has the beneficial effects as follows:
Compared with prior art, the preparation method of boron-carbon nanotube of the present invention has outstanding substantive distinguishing features and is:
(1) because the boron-carbon nanotube length-to-diameter ratio is large, specific surface energy is high, in liquid phase thermal decomposition method building-up process, be subjected to strong van der Waals interaction, the boron-carbon nanotube that is synthesized is unavoidably reunited in liquid phase and is difficult to disperse together in subsequent processes; In the solid-phase pyrolysis building-up process, can indirectly play the effect that disperses boron-carbon nanotube though be used for the carrier of dispersed catalyst, but often be difficult to remove, the technique of removing carrier by strong acid, highly basic can cause damage to the structure of boron-carbon nanotube itself, and follow-up dispersing technology is complicated, dispersion effect is poor.The inventive method is by the carrier of sodium-chlor as the support nickel catalyzator, can play dissemination in early stage to synthetic boron-carbon nanotube in the building-up process, and can realize the removal of carrier and the dispersion of boron-carbon nanotube by the method for synthetic product being put into the aqueous solution that contains dispersion agent, thereby the inventive method propose on the sodium-chlor carrier by the preparation thinking of the synthetic boron-carbon nanotube of technology controlling and process, efficiently solve that boron-carbon nanotube in the existing synthetic method is reunited and the problem of follow-up dispersion, purifying technique complexity and weak effect.
(2) to adopt boron source and nitrogenous source that carbon nanotube is mixed be the common method of preparation boron-carbon nanotube to prior art, but by the technique that boron source and nitrogenous source mix to carbon nanotube cause easily that the product crystal formation is unstable, the doping efficiency of B and N is low, boron-carbon nanotube purity is low and the boron-carbon nanotube productive rate is low; Simultaneously, be subjected to the effect of strong Van der Waals force, the reunion of carbon nanotube causes the purification of subsequent boron carbon-nitrogen nano tube very difficult with dispersion in the starting material.The inventive method makes B, C and N atom dissolve in catalyst metal particles, spread and separate out in reaction zone by boron source, Carbon and nitrogen sources, forms pentagonal class graphite linings structure, and then synthetic boron-carbon nanotube, so that it has stable crystal formation; B and N atom directly enter body inside in building-up process, thereby the doping efficiency of B and N, boron-carbon nanotube purity and boron-carbon nanotube synthetic yield all improve, so that the boron-carbon nanotube synthetic product has higher chemical stability and thermostability; Do purification and the dispersion of the easier realization boron-carbon nanotube of carrier by water-soluble chlorination sodium.
Compared with prior art, the marked improvement that the preparation method has of boron-carbon nanotube of the present invention is:
(1) compare with CN101718732B with prior art CN101718731B, more stable with the prepared boron-carbon nanotube crystal formation of preparation method of boron-carbon nanotube of the present invention, doping efficiency, purity and synthetic yield are higher, and are easy to purify and dispersion.
(2) compare with prior art CN100354202C, the inventive method has overcome the shortcoming that product that above-mentioned prior art makes is difficult to disperse, dispersion effect is poor in liquid phase, have the simple and easy to do characteristics of dispersing technology, and purification and dispersion effect are better.
(3) the inventive method processing method is easy, production cost is low.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is the high resolution scanning electron microscope photo of the embodiment of the invention 1 prepared boron-carbon nanotube-sodium-chlor composite powder.
Fig. 2 is the transmission electron microscope photo of the boron-carbon nanotube after the embodiment of the invention 1 prepared purification.
Fig. 3 is the high resolution transmission electron microscopy photo of the boron-carbon nanotube after the embodiment of the invention 1 prepared purification.
Embodiment
Embodiment 1
The first step, preparation nickel oxide-sodium-chlor catalyzer precursor
Be the ratio of nickelous nitrate: sodium-chlor=0.02:1 by weight, take by weighing Nickelous nitrate hexahydrate and the sodium-chlor of institute's expense, under the induction stirring state, the sodium-chlor that takes by weighing is dissolved in the deionized water by the concentration of 50g/L, then the Nickelous nitrate hexahydrate that takes by weighing is dissolved in the above-mentioned deionized water, continue induction stirring until sodium-chlor and Nickelous nitrate hexahydrate dissolve fully, place Constant Temp. Oven in 60 ℃ of dry 48h mentioned solution, evaporate fully to moisture, then nickelous nitrate and the sodium-chlor crystalline mixture that obtains after the drying placed ball grinder, adopt planetary ball mill with the speed ball milling 3h of 500r/min, above-mentioned mixture after ball-milling processing is placed quartzy Noah's ark, should place the horizontal pipe furnace flat-temperature zone by the quartz Noah's ark, flow velocity with 180ml/min continues to pass into nitrogen and is warming up to 350 ℃ in this tube furnace, insulation 2h makes this tube furnace till cool to room temperature under the nitrogen atmosphere of 180ml/min flow velocity, makes nickel oxide-sodium-chlor catalyzer precursor;
Second step, preparation boron-carbon nanotube-sodium-chlor composite powder
The nickel oxide that the first step is made-sodium-chlor catalyzer precursor places quartzy Noah's ark, should place the horizontal pipe furnace flat-temperature zone by the quartz Noah's ark, flow velocity with 180ml/min passes into hydrogen and is warming up to 550 ℃ in this tube furnace, insulation 1.5h, then close hydrogen, be nitrogen with volume ratio again: the gas mixture of methyl-borate steam: methane=4:0.5:1 continues to pass in this tube furnace with the flow velocity of 330ml/min, under 550 ℃, carry out chemical vapour deposition reaction 0.5h, close afterwards methyl-borate steam and methane and adjust nitrogen flow, make above-mentioned tube furnace till cool to room temperature under the nitrogen atmosphere of 180ml/min flow velocity, make thus boron-carbon nanotube-sodium-chlor composite powder, wherein the quality percentage composition of boron-carbon nanotube is 5.1%;
Fig. 1 is the high resolution scanning electron microscope photo of the embodiment of the invention 1 prepared boron-carbon nanotube-sodium-chlor composite powder.By among this figure as seen, chemical vapour deposition reaction by mixed gas, synthetic a large amount of finely dispersed boron-carbon nanotubes in composite powder, its length-to-diameter ratio is larger, length reaches more than the 1 μ m, be subjected to the impact of the atom doped formation pentagon of B and N class graphite linings structure, the curvature of tube wall constantly changes, and causes formed boron-carbon nanotube to be bending and surface irregularity.
The 3rd step, the purification boron-carbon nanotube
The boron-carbon nanotube that second step is made by the concentration of 2g/L-sodium-chlor composite powder is put into the deionized water solution that mass percent concentration is 0.3% Sodium dodecylbenzene sulfonate, place the ultra-sonic dispersion instrument to disperse 10min that sodium-chlor is dissolved fully with the ultrasonic wave of 30kHz in the beaker that mentioned solution is housed, throw out in the solution is filtered, with washed with de-ionized water 3 times, then use Constant Temp. Oven in 80 ℃ of dry 2h, namely make the boron-carbon nanotube after the purification.
Fig. 2 is the transmission electron microscope photo of the boron-carbon nanotube after the embodiment of the invention 1 prepared purification.As seen, the boron-carbon nanotube after the purification is not reunited in transmission electron microscope powdered sample preparation process, can realize the Uniform Dispersion of single boron-carbon nanotube from this figure; The boron-carbon nanotube diameter 30nm that is synthesized, body has bamboo knot shaped structure, and outside surface is more coarse, has a large amount of projections and depression.
Fig. 3 is the high resolution transmission electron microscopy photo of the boron-carbon nanotube after the embodiment of the invention 1 prepared purification.As seen, the boron-carbon nanotube tube wall that is synthesized is multi-walled pipes shape structure from this figure, has good crystallization degree, does not find that decolorizing carbon class impurity substances occurs; Outer surface of tube body is coarse, and external diameter is between 25～35nm, and internal diameter of tube body is between 8～15nm; Having formed many connections between the boron-carbon nanotube inwall, is a kind bamboo joint structure, the about 20nm in the interval of every joint.
Embodiment 2
The first step, preparation nickel oxide-sodium-chlor catalyzer precursor
Be the ratio of nickelous nitrate: sodium-chlor=0.55:1 by weight, take by weighing Nickelous nitrate hexahydrate and the sodium-chlor of institute's expense, under the induction stirring state, the sodium-chlor that takes by weighing is dissolved in the deionized water by the concentration of 80g/L, then the Nickelous nitrate hexahydrate that takes by weighing is dissolved in the above-mentioned deionized water, continue induction stirring until sodium-chlor and Nickelous nitrate hexahydrate dissolve fully, place Constant Temp. Oven in 90 ℃ of dry 96h mentioned solution, evaporate fully to moisture, then nickelous nitrate and the sodium-chlor crystalline mixture that obtains after the drying placed ball grinder, adopt planetary ball mill with the speed ball milling 6h of 1000r/min, above-mentioned mixture after ball-milling processing is placed quartzy Noah's ark, should place the horizontal pipe furnace flat-temperature zone by the quartz Noah's ark, flow velocity with 240ml/min continues to pass into nitrogen and is warming up to 600 ℃ in this tube furnace, insulation 4h makes this tube furnace till cool to room temperature under the nitrogen atmosphere of 240ml/min flow velocity, makes nickel oxide-sodium-chlor catalyzer precursor;
Second step, preparation boron-carbon nanotube-sodium-chlor composite powder
The nickel oxide that the first step is made-sodium-chlor catalyzer precursor places quartzy Noah's ark, should place the horizontal pipe furnace flat-temperature zone by the quartz Noah's ark, flow velocity with 240ml/min passes into hydrogen and is warming up to 750 ℃ in this tube furnace, insulation 3.5h, then close hydrogen, be nitrogen with volume ratio again: the gas mixture of methyl-borate steam: methane=8:1:1 continues to pass in this tube furnace with the flow velocity of 600ml/min, under 750 ℃, carry out chemical vapour deposition reaction 1.5h, close afterwards methyl-borate steam and methane and adjust nitrogen flow, make above-mentioned tube furnace till cool to room temperature under the nitrogen atmosphere of 240ml/min flow velocity, make thus boron-carbon nanotube-sodium-chlor composite powder, wherein the quality percentage composition of boron-carbon nanotube is 17.6%;
The 3rd step, the purification boron-carbon nanotube
The boron-carbon nanotube that second step is made by the concentration of 5g/L-sodium-chlor composite powder is put into the deionized water solution that mass percent concentration is 1.0% Sodium dodecylbenzene sulfonate, place the ultra-sonic dispersion instrument to disperse 20min that sodium-chlor is dissolved fully with the ultrasonic wave of 40kHz in the beaker that mentioned solution is housed, throw out in the solution is filtered, with washed with de-ionized water 4 times, then use Constant Temp. Oven in 90 ℃ of dry 4h, namely make the boron-carbon nanotube after the purification.
Embodiment 3
The first step, preparation nickel oxide-sodium-chlor catalyzer precursor
Be the ratio of nickelous nitrate: sodium-chlor=0.26:1 by weight, take by weighing Nickelous nitrate hexahydrate and the sodium-chlor of institute's expense, under the induction stirring state, the sodium-chlor that takes by weighing is dissolved in the deionized water by the concentration of 65g/L, then the Nickelous nitrate hexahydrate that takes by weighing is dissolved in the above-mentioned deionized water, continue induction stirring until sodium-chlor and Nickelous nitrate hexahydrate dissolve fully, place Constant Temp. Oven in 75 ℃ of dry 72h mentioned solution, evaporate fully to moisture, then nickelous nitrate and the sodium-chlor crystalline mixture that obtains after the drying placed ball grinder, adopt planetary ball mill with the speed ball milling 4h of 800r/min, above-mentioned mixture after ball-milling processing is placed quartzy Noah's ark, should place the horizontal pipe furnace flat-temperature zone by the quartz Noah's ark, flow velocity with 210ml/min continues to pass into nitrogen and is warming up to 470 ℃ in this tube furnace, insulation 3h makes this tube furnace till cool to room temperature under the nitrogen atmosphere of 210ml/min flow velocity, makes nickel oxide-sodium-chlor catalyzer precursor;
Second step, preparation boron-carbon nanotube-sodium-chlor composite powder
The nickel oxide that the first step is made-sodium-chlor catalyzer precursor places quartzy Noah's ark, should place the horizontal pipe furnace flat-temperature zone by the quartz Noah's ark, flow velocity with 210ml/min passes into hydrogen and is warming up to 650 ℃ in this tube furnace, insulation 2.5h, then close hydrogen, be nitrogen with volume ratio again: the gas mixture of methyl-borate steam: methane=6:0.8:1 continues to pass in this tube furnace with the flow velocity of 470ml/min, under 650 ℃, carry out chemical vapour deposition reaction 1h, close afterwards methyl-borate steam and methane and adjust nitrogen flow, make above-mentioned tube furnace till cool to room temperature under the nitrogen atmosphere of 210ml/min flow velocity, make thus boron-carbon nanotube-sodium-chlor composite powder, wherein the quality percentage composition of boron-carbon nanotube is 8.3%;
The 3rd step, the purification boron-carbon nanotube
The boron-carbon nanotube that second step is made by the concentration of 4g/L-sodium-chlor composite powder is put into the deionized water solution that mass percent concentration is 0.65% Sodium dodecylbenzene sulfonate, place the ultra-sonic dispersion instrument to disperse 15min that sodium-chlor is dissolved fully with the ultrasonic wave of 35kHz in the beaker that mentioned solution is housed, throw out in the solution is filtered, with washed with de-ionized water 3 times, then use Constant Temp. Oven in 85 ℃ of dry 3h, namely make the boron-carbon nanotube after the purification.
Starting material related among above-mentioned all embodiment are all by commercially available, and used equipment and process all is that those skilled in the art are known.
Claims (1)
1. the preparation method of boron-carbon nanotube is characterized in that: be a kind of preparation method by the synthetic boron-carbon nanotube of chemical Vapor deposition process, concrete steps are as follows:
The first step, preparation nickel oxide-sodium-chlor catalyzer precursor
It is nickelous nitrate by weight: the ratio of sodium-chlor=0.02～0.55:1, take by weighing Nickelous nitrate hexahydrate and the sodium-chlor of institute's expense, under the induction stirring state, the sodium-chlor that takes by weighing is dissolved in the deionized water by the concentration of 50～80g/L, then the Nickelous nitrate hexahydrate that takes by weighing is dissolved in the above-mentioned deionized water, continue induction stirring until sodium-chlor and Nickelous nitrate hexahydrate dissolve fully, place Constant Temp. Oven in 60～90 ℃ of drying 48～96h mentioned solution, evaporate fully to moisture, then nickelous nitrate and the sodium-chlor crystalline mixture that obtains after the drying placed ball grinder, adopt planetary ball mill with speed ball milling 3～6h of 500～1000r/min, above-mentioned mixture after ball-milling processing is placed quartzy Noah's ark, should place the horizontal pipe furnace flat-temperature zone by the quartz Noah's ark, flow velocity with 180～240ml/min continues to pass into nitrogen and is warming up to 350～600 ℃ in this tube furnace, insulation 2～4h, make this tube furnace till cool to room temperature under the nitrogen atmosphere of 180～240ml/min flow velocity, make nickel oxide-sodium-chlor catalyzer precursor;
Second step, preparation boron-carbon nanotube-sodium-chlor composite powder
The nickel oxide that the first step is made-sodium-chlor catalyzer precursor places quartzy Noah's ark, should place the horizontal pipe furnace flat-temperature zone by the quartz Noah's ark, flow velocity with 180～240ml/min passes into hydrogen and is warming up to 550～750 ℃ in this tube furnace, insulation 1.5～3.5h, then close hydrogen, be nitrogen with volume ratio again: methyl-borate steam: the gas mixture of methane=4～8:0.5～1:1 continues to pass in this tube furnace with the flow velocity of 330～600ml/min, under 550～750 ℃, carry out chemical vapour deposition reaction 0.5～1.5h, close afterwards methyl-borate steam and methane and adjust nitrogen flow, make above-mentioned tube furnace till cool to room temperature under the nitrogen atmosphere of 180～240ml/min flow velocity, make thus boron-carbon nanotube-sodium-chlor composite powder, wherein the quality percentage composition of boron-carbon nanotube is 5.1～17.6%;
The 3rd step, the purification boron-carbon nanotube
The boron-carbon nanotube that second step is made by the concentration of 2～5g/L-sodium-chlor composite powder is put into the deionized water solution that mass percent concentration is 0.3～1.0% Sodium dodecylbenzene sulfonate, place the ultra-sonic dispersion instrument to disperse 10～20min that sodium-chlor is dissolved fully with the ultrasonic wave of 30kHz～40kHz in the beaker that mentioned solution is housed, throw out in the solution is filtered, with washed with de-ionized water 3～4 times, then use Constant Temp. Oven in 80～90 ℃ of drying 2～4h, namely make the boron-carbon nanotube after the purification.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103496689A (en) * | 2013-09-23 | 2014-01-08 | 同济大学 | Preparation method of boron-doped p type carbon nanotube with high seebeck coefficient |
| CN111517356A (en) * | 2020-04-30 | 2020-08-11 | 浙江理工大学 | Cu2O nanotube and method for producing the same |
| US11254055B2 (en) | 2017-04-21 | 2022-02-22 | Hewlett-Packard Development Company, L.P. | Additive manufacturing machine heat flux |
| CN115124007A (en) * | 2022-06-20 | 2022-09-30 | 北京化工大学 | Preparation method of multi-stage regulation and control hydrophilic-hydrophobic boron carbon nitrogen nano material |
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| CN1830781A (en) * | 2006-03-17 | 2006-09-13 | 燕山大学 | Method of preparing boron carbon nitrogen nanometer pipe under low temperature |
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| CN1830781A (en) * | 2006-03-17 | 2006-09-13 | 燕山大学 | Method of preparing boron carbon nitrogen nanometer pipe under low temperature |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496689A (en) * | 2013-09-23 | 2014-01-08 | 同济大学 | Preparation method of boron-doped p type carbon nanotube with high seebeck coefficient |
| CN103496689B (en) * | 2013-09-23 | 2015-04-15 | 同济大学 | Preparation method of boron-doped p type carbon nanotube with high seebeck coefficient |
| US11254055B2 (en) | 2017-04-21 | 2022-02-22 | Hewlett-Packard Development Company, L.P. | Additive manufacturing machine heat flux |
| CN111517356A (en) * | 2020-04-30 | 2020-08-11 | 浙江理工大学 | Cu2O nanotube and method for producing the same |
| CN111517356B (en) * | 2020-04-30 | 2022-03-29 | 浙江理工大学 | Cu2O nanotube and method for producing the same |
| CN115124007A (en) * | 2022-06-20 | 2022-09-30 | 北京化工大学 | Preparation method of multi-stage regulation and control hydrophilic-hydrophobic boron carbon nitrogen nano material |
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| CN103030120B (en) | 2014-07-16 |
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