CN102442659B - Method for nondestructive dispersion of double-walled carbon nanotube by combination of N, N-dimethylformamide and ethylene glycol - Google Patents
Method for nondestructive dispersion of double-walled carbon nanotube by combination of N, N-dimethylformamide and ethylene glycol Download PDFInfo
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- CN102442659B CN102442659B CN201110309123XA CN201110309123A CN102442659B CN 102442659 B CN102442659 B CN 102442659B CN 201110309123X A CN201110309123X A CN 201110309123XA CN 201110309123 A CN201110309123 A CN 201110309123A CN 102442659 B CN102442659 B CN 102442659B
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 239000002079 double walled nanotube Substances 0.000 title claims abstract description 106
- 239000006185 dispersion Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 title abstract description 14
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 30
- 238000001237 Raman spectrum Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 238000005087 graphitization Methods 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract 2
- 230000003750 conditioning effect Effects 0.000 claims abstract 2
- 239000011159 matrix material Substances 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 27
- 230000002950 deficient Effects 0.000 claims description 19
- 238000004140 cleaning Methods 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 230000006378 damage Effects 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 19
- 239000002041 carbon nanotube Substances 0.000 description 17
- 229910021393 carbon nanotube Inorganic materials 0.000 description 17
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000013543 active substance Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002109 single walled nanotube Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
Relating to the technical field of nano-materials, the invention provides a method for nondestructive dispersion of a double-walled carbon nanotube by combination of N, N-dimethylformamide and ethylene glycol. Before dispersion, the double-walled carbon nanotube has a diameter of 2-10nm and a tube bundle diameter of 50-200nm. And the Raman spectrum ratio between a complete peak and a defect peak of the double-walled carbon nanotube is 5-6.3. The method comprises the steps of: taking ethylene glycol as a dispersion matrix, adding a dispersion conditioning agent N, N-dimethylformamide (in a volume ratio of 1:99-10:90), subjecting the mixture to ultrasonic dispersion for 8-24h, thus obtaining a double-walled carbon nanotube solution with a concentration up to 1.0mg mL<-1>. In the solution, the double-walled carbon nanotube has a diameter of 2-10nm, a tube bundle diameter of 10-100nm, and a Raman spectrum ratio between its complete peak and defect peak is 4.8-6.1. The dispersed double-walled carbon nanotube does not suffer obvious destruction in terms of its graphitization degree, but its length is cut short and the tube bundle is opened, thus bringing convenience for its application in various fields.
Description
Technical field
The present invention relates to the method that the carbon nanotube not damaged disperses in a kind of technical field of nano material, specifically a kind of method of disperseing double-walled carbon nano-tube by DMF and ethylene glycol combination not damaged.
Background technology
As a kind of novel nano material, carbon nanotube is since being found, because its unique geometry and electronic band structure have brought excellent mechanical property, electric property, thermal property and electromagnetic performance etc., these excellent performances make carbon nanotube exist great potential application advantage, it is cotton-shaped or Powdered that the carbon nanotube of general method preparation is group in macroscopic view, be with the prerequisite of its application it to be scattered in form uniform solution in the solvent.Involve the field such as chemisorption all has broad application prospects in aerospace, precision optical machinery and function weaving, solar energy power generating, an emission, electromagnetic shielding, suction such as carbon nano-tube solution.Carbon nanotube is the one dimension tubular structure in microtexture, its diameter is at 1-40 nm, length is up to several microns or centimetre-sized, so it generally is rambling winding state and occurs, make it be difficult to be dispersed, particularly for the more excellent L/D ratio of performance larger single wall or double-walled carbon nano-tube, its more difficult being scattered in the usual vehicle.So, when dispersing Nano carbon tubes, generally in solution, add tensio-active agent or carbon nano tube surface carried out grafting luminous energy group help it to be scattered in the solvent.Aforesaid method can effectively prepare carbon nano-tube solution, but the concentration of gained solution is very limited.The shortcoming of aforesaid method is that graft surface active agent molecule or luminous energy group are difficult to remove after carbon nano tube surface, affect the proper property of carbon nanotube, particularly because the adding of tensio-active agent or luminous energy group, the performances such as its electroconductibility, heat conduction decline to a great extent, and have lost the essence of carbon nanotube conducting, heat conduction and make it lose using value.
Through the literature search of prior art is found, the research that the not damaged of carbon nanotube is disperseed also is in the exploratory stage at present.The Jie Ma of Shanghai Communications University and Zi Ping Wu etc. have delivered " Purification of single-walled carbon nNanotubes by a highly efficient and nondestructive approach " (non-invasive efficient purification of single-wall carbon nano tube) and " Journal of Power Scources " (power technology) the 195th phase in 2010 2143 pages " Preparation of dispersible double-walled carobn nanotubes and application as catalyst support in fuel cells " (double-walled carbon nano-tube of preparation high dispersive is used for the support of the catalyst of fuel cell) two literary compositions 2895 pages of " Chemistry of Materials " (chemical material) the 20th phases in 2008, in these two pieces of documents, not damaged purifying and the dispersion of carbon nanotube are suggested, they are by the method for solid state reaction and ultra-sonic dispersion, obtained the list of not damaged purifying and dispersion, double-walled carbon nano-tube solution has shown preferably performance.Yet because the method restriction, the maximum concentration of gained solution only has 0.15 mg mL
-1, thereby production cost is higher.
Summary of the invention
The present invention has developed the method that the double-walled carbon nano-tube not damaged disperses, dispersion medium by double-walled carbon nano-tube that not damaged is disperseed is optimized, then carry out ultrasonic for a long time, obtained being uniformly dispersed, considerable change do not occur in carbon nano tube surface structure and degree of graphitization, maximum concentration can reach 1.0 mg mL
-1Double-walled carbon nano-tube solution.Thereby bring great convenience for the subsequent applications of carbon nanotube; Raw material of the present invention is simple and easy to, and is with low cost, environmentally safe; In the production process without inflammable dangerous raw material; Product is easy to process, and yield is high, and equipment is simple, can semicontinuously operate, and is suitable for a large amount of productions.
The present invention relates to a kind of double-walled carbon nano-tube solution of high density, in the solution without obvious sediment and particle suspensions, solvent in the solution is by ethylene glycol and N, dinethylformamide forms, solute is comprised of less than the double-walled carbon nano-tube of 50 nm at 1-2 um, tube bank diameter in 2-10 nm, length diameter, and the complete peak of solute and the Raman spectrum ratio at defective peak are not less than 5.
The present invention is achieved by the following technical solutions, and the method by DMF and ethylene glycol combination not damaged dispersion double-walled carbon nano-tube that the present invention relates to comprises the steps:
Step 1, be analytical pure ethylene glycol and the N of 90:10-99:1 with volume ratio, dinethylformamide liquid is packed in the beaker of 50-500 mL and is put into Ultrasonic Cleaners and carry out ultra-sonic dispersion 5-30 min, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.
Step 2 is 0.15-1.0 mg mL with calculating concentration
-1Double-walled carbon nano-tube put into the solution that step 1 configuration mixes, the diameter of putting into double-walled carbon nano-tube is that 2-10 nm, length are that 5-20um, tube bank diameter are 50-200 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5-6.3.
Step 3, double-walled carbon nano-tube, ethylene glycol and N with gained in the step 2, the mixture of dinethylformamide is again put into the ultrasonic cleaning acc power and is carried out ultra-sonic dispersion 8-24 h, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.After ultra-sonic dispersion finishes, can obtain the double-walled carbon nano-tube dispersion liquid of different concns.The diameter of the double-walled carbon nano-tube double-walled carbon nano-tube after the dispersion is that 2-10 nm, length are that 1-4 um, tube bank diameter are 10-100 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 4.8-6.1.
The present invention has following beneficial effect:Ethylene glycol has low surface energy (47.9 mN m
-1), along with the increase of ultrasonic time, increasing ethylene glycol liquid can be infiltrated on the double-walled carbon nano-tube interfascicular, thereby tube bank is expanded and soft, and under the effect of ultrasonic mechanical force, tube bank is stripped from or cuts short.Increase along with double-walled carbon nano-tube concentration in the solution, the double-walled carbon nano-tube interfascicular becomes finer and close, so that ethylene glycol is difficult to be infiltrated on the double-walled carbon nano-tube interfascicular again, high boiling wetting ability non-protonic solvent DMF has lower surface energy (35.2 mN m
-1), can make the hydrophilic C-H of generation in the mixing solutions and H-C-H strong, thereby so that ethylene glycol to enter to enter once again fine and close double-walled carbon nano-tube intrafascicular and further disperse this carbon nanotube.On the other hand because the high viscosity (21 mPas) of ethylene glycol but the sedimentation of the double-walled carbon nano-tube that establishment disperses, thereby can make this double-walled carbon nano-tube solution be able to Uniform Dispersion, but along with N, further adding (ethylene glycol and the N of dinethylformamide, the volume ratio of dinethylformamide is rear greater than 9), the C-N on double-walled carbon nano-tube surface is strong can be increased (this strong degree of graphitization that can greatly reduce carbon nanotube), and the surperficial degree of graphitization of double-walled carbon nano-tube begins to descend.
The present invention is simple for process, and the double-walled carbon nano-tube homogeneous solution that obtains can semi-continuously prepare.And can automatically regulate by the add-on of DMF the maximum concentration of preparation double-walled carbon nano-tube solution.Because the double-walled carbon nano-tube degree of graphitization is not suffered obvious destruction in the homodisperse solution, make the double-walled carbon nano-tube of gained keep the performances such as its intrinsic high conduction, heat conduction, and its length is cut short, and tube bank is opened, for its application in each field brings great convenience.Raw material of the present invention is simple and easy to, and is with low cost, environmentally safe; Without inflammable dangerous raw material; Product is easy to process, and yield is high, and equipment is simple, can realize semicontinuous operation, is suitable for a large amount of productions.
Embodiment
The below elaborates to embodiments of the invention: the present embodiment is implemented under take technical solution of the present invention as prerequisite, has provided detailed embodiment and process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Be analytical pure ethylene glycol and the N of 99:1 with volume ratio, dinethylformamide liquid is packed in the beaker of 50 mL and is put into Ultrasonic Cleaners and carry out ultra-sonic dispersion 5 min, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.Be 0.15 mg mL with calculating concentration
-1Double-walled carbon nano-tube put into finely dispersed ethylene glycol and N, in the mixing solutions of dinethylformamide, the diameter of putting into double-walled carbon nano-tube is that 2-10 nm, length are that 5-20 um, tube bank diameter are 50-200 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5.Double-walled carbon nano-tube, ethylene glycol and N with above-mentioned configuration, the mixture of dinethylformamide is again put into the ultrasonic cleaning acc power and is carried out ultra-sonic dispersion 8 h, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.After ultra-sonic dispersion finishes, can obtain the dispersion soln of double-walled carbon nano-tube.The diameter of the double-walled carbon nano-tube double-walled carbon nano-tube after the dispersion is that 2-10 nm, length are that 1-2 um, tube bank diameter are 10-100 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 4.8.
Embodiment 2
Be analytical pure ethylene glycol and the N of 98:2 with volume ratio, dinethylformamide liquid is packed in the beaker of 100 mL and is put into Ultrasonic Cleaners and carry out ultra-sonic dispersion 15 min, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.Be 0.25 mg mL with calculating concentration
-1Double-walled carbon nano-tube put into finely dispersed ethylene glycol and N, in the mixing solutions of dinethylformamide, the diameter of putting into double-walled carbon nano-tube is that 2-10 nm, length are that 5-20 um, tube bank diameter are 50-200 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5.3.Double-walled carbon nano-tube, ethylene glycol and N with above-mentioned configuration, the mixture of dinethylformamide is again put into the ultrasonic cleaning acc power and is carried out ultra-sonic dispersion 12 h, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.After ultra-sonic dispersion finishes, can obtain the dispersion soln of double-walled carbon nano-tube.The diameter of the double-walled carbon nano-tube double-walled carbon nano-tube after the dispersion is that 2-10 nm, length are that 1-3 um, tube bank diameter are 10-100 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5.1.
Embodiment 3
Be analytical pure ethylene glycol and the N of 97:3 with volume ratio, dinethylformamide liquid is packed in the beaker of 200 mL and is put into Ultrasonic Cleaners and carry out ultra-sonic dispersion 30 min, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.Be 0.35 mg mL with calculating concentration
-1Double-walled carbon nano-tube put into finely dispersed ethylene glycol and N, in the mixing solutions of dinethylformamide, the diameter of putting into double-walled carbon nano-tube is that 2-10 nm, length are that 5-20 um, tube bank diameter are 50-200 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 6.3.Double-walled carbon nano-tube, ethylene glycol and N with above-mentioned configuration, the mixture of dinethylformamide is again put into the ultrasonic cleaning acc power and is carried out ultra-sonic dispersion 24 h, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.After ultra-sonic dispersion finishes, can obtain the dispersion soln of double-walled carbon nano-tube.The diameter of the double-walled carbon nano-tube double-walled carbon nano-tube after the dispersion is that 2-10 nm, length are that 1-2 um, tube bank diameter are 10-100 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 6.1.
Embodiment 4
Be analytical pure ethylene glycol and the N of 96:4 with volume ratio, dinethylformamide liquid is packed in the beaker of 500 mL and is put into Ultrasonic Cleaners and carry out ultra-sonic dispersion 30 min, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.Be 0.45 mg mL with calculating concentration
-1Double-walled carbon nano-tube put into finely dispersed ethylene glycol and N, in the mixing solutions of dinethylformamide, the diameter of putting into double-walled carbon nano-tube is that 2-10 nm, length are that 5-20 um, tube bank diameter are 50-200 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5.8.Double-walled carbon nano-tube, ethylene glycol and N with above-mentioned configuration, the mixture of dinethylformamide is again put into the ultrasonic cleaning acc power and is carried out ultra-sonic dispersion 24 h, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.After ultra-sonic dispersion finishes, can obtain the dispersion soln of double-walled carbon nano-tube.The diameter of the double-walled carbon nano-tube double-walled carbon nano-tube after the dispersion is that 2-10 nm, length are that 1-3 um, tube bank diameter are 10-100 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5.6.
Embodiment 5
Be analytical pure ethylene glycol and the N of 95:5 with volume ratio, dinethylformamide liquid is packed in the beaker of 300 mL and is put into Ultrasonic Cleaners and carry out ultra-sonic dispersion 20 min, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.Be 0.60 mg mL with calculating concentration
-1Double-walled carbon nano-tube put into finely dispersed ethylene glycol and N, in the mixing solutions of dinethylformamide, the diameter of putting into double-walled carbon nano-tube is that 2-10 nm, length are that 5-20 um, tube bank diameter are 50-200 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5.5.Double-walled carbon nano-tube, ethylene glycol and N with above-mentioned configuration, the mixture of dinethylformamide is again put into the ultrasonic cleaning acc power and is carried out ultra-sonic dispersion 20 h, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.After ultra-sonic dispersion finishes, can obtain the dispersion soln of double-walled carbon nano-tube.The diameter of the double-walled carbon nano-tube double-walled carbon nano-tube after the dispersion is that 2-10 nm, length are that 1-2 um, tube bank diameter are 10-100 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5.3.
Embodiment 6
Be analytical pure ethylene glycol and the N of 93:7 with volume ratio, dinethylformamide liquid is packed in the beaker of 500 mL and is put into Ultrasonic Cleaners and carry out ultra-sonic dispersion 10 min, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.Be 0.80 mg mL with calculating concentration
-1Double-walled carbon nano-tube put into finely dispersed ethylene glycol and N, in the mixing solutions of dinethylformamide, the diameter of putting into double-walled carbon nano-tube is that 2-10 nm, length are that 5-20 um, tube bank diameter are 50-200 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 6.3.Double-walled carbon nano-tube, ethylene glycol and N with above-mentioned configuration, the mixture of dinethylformamide is again put into the ultrasonic cleaning acc power and is carried out ultra-sonic dispersion 20 h, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.After ultra-sonic dispersion finishes, can obtain the dispersion soln of double-walled carbon nano-tube.The diameter of the double-walled carbon nano-tube double-walled carbon nano-tube after the dispersion is that 2-10 nm, length are that 1-2 um, tube bank diameter are 10-100 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5.8.
Embodiment 7
Be analytical pure ethylene glycol and the N of 90:10 with volume ratio, dinethylformamide liquid is packed in the beaker of 500 mL and is put into Ultrasonic Cleaners and carry out ultra-sonic dispersion 18 min, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.Be 1.0 mg mL with calculating concentration
-1Double-walled carbon nano-tube put into finely dispersed ethylene glycol and N, in the mixing solutions of dinethylformamide, the diameter of putting into double-walled carbon nano-tube is that 2-10 nm, length are that 5-20 um, tube bank diameter are 50-200 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 6.3.Double-walled carbon nano-tube, ethylene glycol and N with above-mentioned configuration, the mixture of dinethylformamide is again put into the ultrasonic cleaning acc power and is carried out ultra-sonic dispersion 24 h, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners.After ultra-sonic dispersion finishes, can obtain the dispersion soln of double-walled carbon nano-tube.The diameter of the double-walled carbon nano-tube double-walled carbon nano-tube after the dispersion is that 2-10 nm, length are that 1-2 um, tube bank diameter are 10-80 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5.2.
Claims (2)
1. method of disperseing double-walled carbon nano-tube by DMF and ethylene glycol combination not damaged is characterized in that:
Dispersion soln is by ethylene glycol and N, dinethylformamide forms, ethylene glycol is as disperseing matrix, N, dinethylformamide is for disperseing conditioning agent, and behind long ultra-sonic dispersion, the length of double-walled carbon nano-tube has obtained significantly cutting short, tube bank is opened, and its degree of graphitization does not occur significantly to change; The volume ratio of described ethylene glycol and DMF is 90:10-99:1.
2. DMF according to claim 1 and ethylene glycol make up the method that not damaged disperses double-walled carbon nano-tube, it is characterized in that comprising following concrete steps:
Step 1, be analytical pure ethylene glycol and the N of 90:10-99:1 with volume ratio, dinethylformamide liquid is packed in the beaker of 50-500 mL and is put into Ultrasonic Cleaners and carry out ultra-sonic dispersion 5-30 min, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners; Step 2 is 0.15-1.0 mg mL with calculating concentration
-1Double-walled carbon nano-tube put into the solution that step 1 configuration mixes, the diameter of putting into double-walled carbon nano-tube is that 2-10 nm, length are that 5-20 um, tube bank diameter are 50-200 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 5-6.3; Step 3, double-walled carbon nano-tube, ethylene glycol and N with gained in the step 2, the mixture of dinethylformamide is again put into the ultrasonic cleaning acc power and is carried out ultra-sonic dispersion 8-24 h, ultrasonic cleaning acc power 600 W pass into recirculated water and guarantee that water temperature keeps 25 ° of C in the cleaning machine in the Ultrasonic Cleaners; After ultra-sonic dispersion finishes, can obtain the double-walled carbon nano-tube dispersion liquid of different concns; The diameter of the double-walled carbon nano-tube double-walled carbon nano-tube after the dispersion is that 2-10 nm, length are that 1-4 um, tube bank diameter are 10-100 nm, and the complete peak of double-walled carbon nano-tube and the Raman spectrum ratio at defective peak are 4.8-6.1.
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| CN1436721A (en) * | 2002-02-08 | 2003-08-20 | 中国科学院化学研究所 | Prepn of water soluble carbon nanotube |
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| CN1436721A (en) * | 2002-02-08 | 2003-08-20 | 中国科学院化学研究所 | Prepn of water soluble carbon nanotube |
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| Title |
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