CN106395790A - Preparation method and use of high purity carbon nanotube - Google Patents
Preparation method and use of high purity carbon nanotube Download PDFInfo
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- CN106395790A CN106395790A CN201610722710.4A CN201610722710A CN106395790A CN 106395790 A CN106395790 A CN 106395790A CN 201610722710 A CN201610722710 A CN 201610722710A CN 106395790 A CN106395790 A CN 106395790A
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- H01M4/00—Electrodes
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A preparation method of a high purity carbon nanotube comprises the following steps: A, in a reactor, adding 0.2 to 2 grams of a metal catalyst, and heating to 600 to 900 DEG C under the protection of nitrogen; B, according to the volume ratio of hydrogen to nitrogen of 1:2-9:8, adding hydrogen into the reactor, activating the catalyst for 40 to 80 minutes; C, according to the volume ratio of carbon source: nitrogen: etchant of 3-5:4-6:0.5-2, respectively adding a carbon source, the nitrogen and an etchant into the reactor for reaction for 40 to 80 minutes, improving the activity of the catalyst and removing amorphous carbon impurities covering the surface of the carbon nanotube through the decomposition of the etchant, and cooling to room temperature under the protection of the nitrogen for preparation of high purity granular carbon nanotube powder, wherein the etchant is one of alcohols or deionized water or a combination of a plurality of the alcohols or deionized water.The invention also provides use of the high purity carbon nanotube as a conductive agent of a lithium ion battery. The hydrogen is used as a catalyst active agent, the deionized water or the alcohols is /are used the etchant, the prepared carbon nanotube has high purity, and the activity of the catalyst is high.
Description
【Technical field】
The present invention relates to the Preparation method and use of CNT, more particularly to a kind of catalyst activity is high, impurity is low
High-purity carbon nano tube Preparation method and use.
【Background technology】
Since 1991 end of the year Japanese scholars Lijimat are found that the CNT being made up of carbon atom, CNT because
The particularity of its structure and show many with the diverse property of other carbonaceous materials so that CNT becomes
One of material of tool potentiality, it is widely used in the neck such as feds, capacitor, transistor, hydrogen storage material, composite
Domain.The preparation method of existing CNT mainly has arc discharge method, laser evaporization method and catalyst Assisted Chemical Vapor to sink
Area method etc..Wherein, arc discharge method prepares CNT quick, the feature that technological parameter is relatively easy to control that has a growth, but it is deposited
Growth temperature high, equipment is complicated, impurity in products is many, low yield and difficult purification and the defect being not suitable for batch production.Laser steams
The product quality of the method for sending out preparation is high, but it yields poorly.Catalysts Assistant Chemical Vapor Deposition is using Hydrocarbon cracking
The free carbon ion producing, separates out, in catalyst one end, a kind of method generating CNT, it is easy that the method has course of reaction
In control, strong applicability, preparation method is simple and the advantages of be produced on a large scale, it is widely used in preparing CNT.So
And, because the existing CNT prepared by Catalysts Assistant Chemical Vapor Deposition generally remains catalyst granules and nothing
Sizing carbon impurity, makes the performance of CNT cannot play to optimum state, leads to its application to be subject to large effect.Therefore,
How effectively to remove the impurity such as residual catalyst granule and amorphous carbon in CNT, with prepare disposable degree of crystallinity high,
The low CNT of impurity just becomes a kind of objective demand.
【Content of the invention】
Present invention seek to address that the problems referred to above, and provide one kind can improve catalyst activity, and remove carbon nano tube surface
Metal impurities and amorphous carbon impurity, to improve the preparation method of the high-purity carbon nano tube of carbon nano pipe purity.
For realizing the purpose of the present invention, the invention provides a kind of preparation method of high-purity carbon nano tube, the method bag
Include following steps：
A, in reactor add 0.2～2 gram of metallic catalyst, be warming up to 600～900 DEG C under nitrogen protection；
B, press hydrogen：The volume ratio of nitrogen is 1:2～9:8 add hydrogen in reactor, and catalyst is carried out activating 40
～80 minutes；
C, press carbon source：Nitrogen：The volume ratio of etching agent is 3～5:4～6：0.5～2 be separately added into in reactor carbon source,
Nitrogen and etching agent, react 40-80 minute, improve catalyst activity by the decomposition of etching agent and remove and be wrapped in CNT
The agraphitic carbon impurity on surface, is then cooled to room temperature under nitrogen protection, prepared graininess high-purity carbon nano tube powder body, institute
State the combination of one or more that etching agent is alcohols or deionized water.
Preferably, the preparation method preparing high-purity carbon nano tube of the present invention comprises the steps：
A, in reactor add 1 gram of metallic catalyst, be warming up to 800 DEG C under nitrogen protection；
B, press hydrogen：The volume ratio of nitrogen is 2:8 add hydrogen in reactor, and catalyst is carried out activating 60 minutes；
C, press carbon source：Nitrogen：The volume ratio of etching agent is 3～5:4～6：0.5～2 is separately added into carbon source in reactor,
Nitrogen and etching agent, react 60 minutes, improve catalyst activity by the decomposition of etching agent and remove and be wrapped in CNT table
The agraphitic carbon impurity in face, is then cooled to room temperature under nitrogen protection, prepared graininess high-purity carbon nano tube powder body, described
Etching agent is the combination of one or more of alcohols or deionized water.
In step a, described reactor is fixed bed reactors or fluidized-bed reactor.
In step a, described metallic catalyst be platinum based catalyst, nickel-base catalyst, cobalt-base catalyst, palladium-based catalyst,
One of ferrum-based catalyst, ruthenium-based catalyst, rhodium base catalyst.
In step c, described carbon source is one of methane, ethylene, propylene, methanol, ethanol.
In step c, described etching agent is the combination of one or more of methanol, ethanol, deionized water.
Described etching agent is deionized water.
In step c, the average caliber of described prepared carbon nanotube dust is 20～50 nanometers, average tube a length of 20～30
Micron, the G/D of Raman spectrum is more than 1, and metals content impurity is less than 0.2%.
Present invention also offers a kind of high-purity carbon nano tube is as the application of lithium ion battery conductive agent.
The contribution of the present invention is, its efficiently solve existing method preparation carbon nano pipe purity low, catalyst activity
Not high problem.The present invention under metallic catalyst effect, after cracking through carbon source, the decomposition of etching agent and catalytic reaction, system
The graininess high-purity carbon nano tube powder body obtaining.The hydrogen of the present invention can activate to catalyst；Additionally, the decomposition of etching agent
Not only increase activity and the life-span of catalyst, and can effectively remove metal impurities and wrap up the unformed of carbon nano tube surface
Carbon (the non-hexatomic ring such as five-membered ring, heptatomic ring) impurity, thus improve the purity of CNT.
【Brief description】
Fig. 1 is the SEM figure of the high-purity carbon nano tube powder body of the present invention.
Fig. 2 is the Raman figure of the high-purity carbon nano tube powder body of the present invention.
Fig. 3 is the TG figure of the high-purity carbon nano tube of the present invention.
Fig. 4 is high-purity carbon nano tube and the application of conventional carbon nanotube electrocondution slurry and the lithium ion battery circulation of the present invention
Figure.
Fig. 5 is high-purity carbon nano tube and the application of conventional carbon nanotube electrocondution slurry and the lithium-ion electric tank discharge of the present invention
Multiplying power figure.
【Specific embodiment】
The following example is being explained further and supplementing to the present invention, and the present invention is not limited in any way.
Embodiment 1
Add 1g platinum based catalyst in fixed bed reactors, be warming up to 800 DEG C under nitrogen protection, add in reactor
Entering volume ratio is hydrogen：Nitrogen=1:9 hydrogen carries out activating to catalyst 60 minutes, then adds volume ratio in reactor
For methane：Nitrogen：Deionized water=5:4:1 methane and deionized water react 1 hour, after reaction terminates, under nitrogen protection
It is cooled to room temperature, obtain graininess high-purity carbon nano tube powder body 70g.To product respectively in scanning electron microscope, Raman spectrometer, heat
Weight analysis instrument and plasma mass spectrograph are characterized, characterization result as shown in Fig. 1-3 and table 1, in terms of the SEM figure shown in from Fig. 1
Go out, carbon nanotube dust degree of crystallinity is high, average caliber is 20～50 nanometers, a length of 30 microns of average tube；Raman shown in from Fig. 2
Collection of illustrative plates is found out, G/D is more than 1；TG figure shown in from Fig. 3 is found out, up to 626 DEG C of the thermal weight loss decomposition temperature of product, from shown in table 1
Plasma Mass Spectrometry analysis result can be seen that, metal impurities be less than 0.2%.This explanation, the product high purity carbon of the present embodiment
Nanotube dust degree of crystallinity is high, and the impurity content such as metal impurities and amorphous carbon is low.
Prepared carbon nanotube dust is further prepared into carbon nanotube conducting slurry, is applied to lithium ion battery material
In, and test battery performance.CNT ratio using same amount carries out data analysiss, and analysis result is as illustrated in figures 4-5.
Can analyze from Fig. 4-5, in discharge-rate, cycle performance aspect has for high-purity carbon nano tube electrocondution slurry and conventional electrocondution slurry
Clear superiority, and heavy-current discharge is with the obvious advantage.This explanation, the high-purity carbon nano tube good conductivity of the present embodiment, unformed
The impurity such as carbon are few.
Table 1 high-purity carbon pipe powder body ICP test result
| Project | Fe | Co | Ni | Cu | Zn | Cr |
| Content (ppm) | <1500 | <20 | <20 | <20 | <20 | <20 |
Embodiment 2
Add 1g ruthenium-based catalyst in fixed bed reactors, be warming up to 800 DEG C under nitrogen protection, add in reactor
Entering volume ratio is hydrogen：Nitrogen=2:8 hydrogen, carries out activating to catalyst 60 minutes, then adds volume in reactor
Than for methanol：Nitrogen：Deionized water=5:4.5:0.5 methanol and deionized water react 1 hour, after reaction terminates, in nitrogen
Protection decline warms to room temperature, and obtains graininess high-purity carbon nano tube powder body 75g.Scanned Electronic Speculum, Raman spectrometer, thermogravimetric are divided
Analyzer and plasma mass spectrograph characterize, and result shows that prepared carbon nanotube dust degree of crystallinity is high, and average caliber is 30～50
Nanometer, a length of 25 microns of average tube, G/D is more than 1, and metal impurities are less than 0.2%.
Prepared carbon nanotube dust is further prepared into carbon nanotube conducting slurry, is applied to lithium ion battery material
In, and test battery performance.Test result shows, the high-purity carbon nano tube electrocondution slurry of the present embodiment and conventional electrocondution slurry
In discharge-rate, cycle performance aspect has a clear superiority, and heavy-current discharge is with the obvious advantage.
Embodiment 3
Add 1g cobalt-base catalyst in fixed bed reactors, be warming up to 800 DEG C under nitrogen protection, add in reactor
Entering volume ratio is hydrogen：Nitrogen=2:8 hydrogen, carries out activating to catalyst 60 minutes, then adds volume in reactor
Than for ethanol：Nitrogen：Deionized water=3:6:1 ethanol and deionized water react 1 hour, after reaction terminates, in nitrogen protection
Decline warms to room temperature, and obtains graininess high-purity carbon nano tube powder body 78g.Scanned Electronic Speculum, Raman spectrometer, thermogravimetric analyzer
And plasma mass spectrograph characterizes, result shows that prepared carbon nanotube dust degree of crystallinity is high, and average caliber is 25～40 nanometers,
A length of 20 microns of average tube, G/D is more than 1, and metal impurities are less than 0.2%.
Prepared carbon nanotube dust is further prepared into carbon nanotube conducting slurry, is applied to lithium ion battery material
In, and test battery performance.Test result shows, the high-purity carbon nano tube electrocondution slurry of the present embodiment and conventional electrocondution slurry
In discharge-rate, cycle performance aspect has a clear superiority, and heavy-current discharge is with the obvious advantage.
Embodiment 4
Add 1g palladium-based catalyst in fixed bed reactors, be warming up to 800 DEG C under nitrogen protection, add in reactor
Entering volume ratio is hydrogen：Nitrogen=2:8 hydrogen, carries out activating to catalyst 60 minutes, then adds volume in reactor
Than for ethylene：Nitrogen：Deionized water=3:6:1 ethylene and deionized water react 1 hour, after reaction terminates, in nitrogen protection
Decline warms to room temperature, and obtains graininess high-purity carbon nano tube powder body 70g.Scanned Electronic Speculum, Raman spectrometer, thermogravimetric analyzer
And plasma mass spectrograph characterizes, result shows that prepared carbon nanotube dust degree of crystallinity is high, and average caliber is 30～50 nanometers,
A length of 28 microns of average tube, G/D is more than 1, and metal impurities are less than 0.2%.
Prepared carbon nanotube dust is further prepared into carbon nanotube conducting slurry, is applied to lithium ion battery material
In, and test battery performance.Test result shows, the high-purity carbon nano tube electrocondution slurry of the present embodiment and conventional electrocondution slurry
In discharge-rate, cycle performance aspect has a clear superiority, and heavy-current discharge is with the obvious advantage.
Embodiment 5
Add 1g ferrum-based catalyst in fixed bed reactors, be warming up to 800 DEG C under nitrogen protection, add in reactor
Entering volume ratio is hydrogen：Nitrogen=2:8 hydrogen, carries out activating to catalyst 60 minutes, then adds volume in reactor
Than for propylene：Nitrogen：Deionized water=4:4:2 propylene and deionized water react 1 hour, after reaction terminates, in nitrogen protection
Decline warms to room temperature, and obtains graininess high-purity carbon nano tube powder body 73g.Scanned Electronic Speculum, Raman spectrometer, thermogravimetric analyzer
And plasma mass spectrograph characterizes, result shows that prepared carbon nanotube dust degree of crystallinity is high, and average caliber is 25～45 nanometers,
A length of 30 microns of average tube, G/D is more than 1, and metal impurities are less than 0.2%.
Prepared carbon nanotube dust is further prepared into carbon nanotube conducting slurry, is applied to lithium ion battery material
In, and test battery performance.Test result shows, the high-purity carbon nano tube electrocondution slurry of the present embodiment and conventional electrocondution slurry
In discharge-rate, cycle performance aspect has a clear superiority, and heavy-current discharge is with the obvious advantage.
Embodiment 6
Add 1g rhodium base catalyst in fixed bed reactors, be warming up to 800 DEG C under nitrogen protection, add in reactor
Entering volume ratio is hydrogen：Nitrogen=2:8 hydrogen, carries out activating to catalyst 60 minutes, then adds volume in reactor
Than for ethanol：Nitrogen：Methane=2:4:4 ethanol and methane reaction 1 hour, after reaction terminates, are cooled under nitrogen protection
Room temperature, obtains graininess high-purity carbon nano tube powder body 75g.Scanned Electronic Speculum, Raman spectrometer, thermogravimetric analyzer and plasma
Body mass-spectroscopic characterization, result shows that prepared carbon nanotube dust degree of crystallinity is high, and average caliber is 30～50 nanometers, average pipe range
For 20 microns, G/D is more than 1, and metal impurities are less than 0.2%.
Prepared carbon nanotube dust is further prepared into carbon nanotube conducting slurry, is applied to lithium ion battery material
In, and test battery performance.Test result shows, the high-purity carbon nano tube electrocondution slurry of the present embodiment and conventional electrocondution slurry
In discharge-rate, cycle performance aspect has a clear superiority, and heavy-current discharge is with the obvious advantage.
Embodiment 7
Add 0.2g nickel-base catalyst in fixed bed reactors, be warming up to 600 DEG C under nitrogen protection, in reactor
Addition volume ratio is hydrogen：Nitrogen=1:9 hydrogen, carries out activating to catalyst 40 minutes, then adds body in reactor
Long-pending ratio is ethanol：Nitrogen：Deionized water=5:4:1 ethanol and deionized water react 40 minutes, after reaction terminates, protect in nitrogen
Shield decline warms to room temperature, and obtains graininess high-purity carbon nano tube powder body 70g.Scanned Electronic Speculum, Raman spectrometer, thermogravimetric analysiss
Instrument and plasma mass spectrograph characterize, and result shows that prepared carbon nanotube dust degree of crystallinity is high, and average caliber is received for 35～50
Rice, a length of 25 microns of average tube, G/D is more than 1, and metal impurities are less than 0.2%.
Prepared carbon nanotube dust is further prepared into carbon nanotube conducting slurry, is applied to lithium ion battery material
In, and test battery performance.Test result shows, the high-purity carbon nano tube electrocondution slurry of the present embodiment and conventional electrocondution slurry
In discharge-rate, cycle performance aspect has a clear superiority, and heavy-current discharge is with the obvious advantage.
Embodiment 8
Add 2g nickel based metal catalyst in a fluidized bed reactor, be warming up to 900 DEG C under nitrogen protection, to reactor
Middle addition volume ratio is hydrogen：Nitrogen=2:8 hydrogen, carries out activating to catalyst 40 minutes, then adds in reactor
Volume ratio is ethanol：Nitrogen：Deionized water=5:4:1 ethanol and deionized water react 80 minutes, after reaction terminates, in nitrogen
Protection decline warms to room temperature, and obtains graininess high-purity carbon nano tube powder body 75g.Scanned Electronic Speculum, Raman spectrometer, thermogravimetric are divided
Analyzer and plasma mass spectrograph characterize, and result shows that prepared carbon nanotube dust degree of crystallinity is high, and average caliber is 40～50
Nanometer, a length of 27 microns of average tube, G/D is more than 1, and metal impurities are less than 0.2%.
Prepared carbon nanotube dust is further prepared into carbon nanotube conducting slurry, is applied to lithium ion battery material
In, and test battery performance.Test result shows, the high-purity carbon nano tube electrocondution slurry of the present embodiment and conventional electrocondution slurry
In discharge-rate, cycle performance aspect has a clear superiority, and heavy-current discharge is with the obvious advantage.
Take this, the present invention, under metallic catalyst effect, with methane, ethylene, propylene, methanol or ethanol as carbon source, passes through
Add hydrogen and etching agent, after cracking through carbon source, the decomposition of etching agent and catalytic reaction, prepared graininess high purity carbon is received
Mitron powder body.The hydrogen of the present invention can activate to catalyst；Additionally, the decomposition of etching agent not only increases the work of catalyst
Property and the life-span, and can effectively remove metal impurities and parcel carbon nano tube surface agraphitic carbon (five-membered ring, heptatomic ring etc. are non-
Hexatomic ring) impurity, thus improve the purity of CNT.
Although being disclosed to the present invention by above example, protection scope of the present invention is not limited thereto,
Under conditions of without departing from present inventive concept, the right of the present invention all will be fallen into the deformation that each component is done above, replacement etc.
In claimed range.
Claims (9)
1. a kind of preparation method of high-purity carbon nano tube is it is characterised in that the method comprises the steps：
A, in reactor add 0.2～2 gram of metallic catalyst, be warming up to 600～900 DEG C under nitrogen protection；
B, press hydrogen：The volume ratio of nitrogen is 1:2～9:8 add hydrogen in reactor, and catalyst is carried out activating 40～80
Minute；
C, press carbon source：Nitrogen：The volume ratio of etching agent is 3～5:4～6：0.5～2 is separately added into carbon source, nitrogen in reactor
And etching agent, react 40-80 minute, catalyst activity is improved by the decomposition of etching agent and removes and be wrapped in carbon nano tube surface
Agraphitic carbon impurity, be then cooled to room temperature under nitrogen protection, prepared graininess high-purity carbon nano tube powder body, described quarter
Erosion agent is the combination of one or more of alcohols or deionized water.
2. the preparation method of high-purity carbon nano tube as claimed in claim 1 is it is characterised in that the method includes walking as follows
Suddenly：
A, in reactor add 1 gram of metallic catalyst, be warming up to 800 DEG C under nitrogen protection；
B, press hydrogen：The volume ratio of nitrogen is 2:8 add hydrogen in reactor, and catalyst is carried out activating 60 minutes；
C, press carbon source：Nitrogen：The volume ratio of etching agent is 3～5:4～6：0.5～2 is separately added into carbon source, nitrogen in reactor
And etching agent, react 60 minutes, catalyst activity is improved by the decomposition of etching agent and removes and be wrapped in carbon nano tube surface
Agraphitic carbon impurity, is then cooled to room temperature under nitrogen protection, prepared graininess high-purity carbon nano tube powder body, described etching
Agent is the combination of one or more of alcohols or deionized water.
3. the preparation method of high-purity carbon nano tube as claimed in claim 1 or 2 is it is characterised in that in step a, described anti-
Device is answered to be fixed bed reactors or fluidized-bed reactor.
4. the preparation method of high-purity carbon nano tube as claimed in claim 1 or 2 is it is characterised in that in step a, described gold
Metal catalyst be platinum based catalyst, nickel-base catalyst, cobalt-base catalyst, palladium-based catalyst, ferrum-based catalyst, ruthenium-based catalyst,
One of rhodium base catalyst.
5. the preparation method of high-purity carbon nano tube as claimed in claim 1 or 2 is it is characterised in that in step c, described carbon
Source is one of methane, ethylene, propylene, methanol, ethanol.
6. the preparation method of high-purity carbon nano tube as claimed in claim 1 or 2 is it is characterised in that in step c, described quarter
Erosion agent is the combination of one or more of methanol, ethanol, deionized water.
7. the preparation method of high-purity carbon nano tube as claimed in claim 6 is it is characterised in that described etching agent is deionization
Water.
8. the preparation method of high-purity carbon nano tube as claimed in claim 2 is it is characterised in that in step c, described prepared
The average caliber of carbon nanotube dust is 20～50 nanometers, a length of 20～30 microns of average tube, and the G/D of Raman spectrum is more than 1, gold
Belong to impurity content and be less than 0.2%.
9. high-purity carbon nano tube as claimed in claim 1 is as the application of lithium ion battery conductive agent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721046A (en) * | 2018-12-24 | 2019-05-07 | 淮安信息职业技术学院 | A kind of preparation method of conductive carbon nanotube |
| CN110894579A (en) * | 2019-12-10 | 2020-03-20 | 昆明理工大学 | Preparation method of hydrogen-etched carbon nanotube reinforced copper-based composite material |
-
2016
- 2016-08-25 CN CN201610722710.4A patent/CN106395790A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721046A (en) * | 2018-12-24 | 2019-05-07 | 淮安信息职业技术学院 | A kind of preparation method of conductive carbon nanotube |
| CN109721046B (en) * | 2018-12-24 | 2023-06-06 | 江苏电子信息职业学院 | Preparation method of conductive carbon nano tube |
| CN110894579A (en) * | 2019-12-10 | 2020-03-20 | 昆明理工大学 | Preparation method of hydrogen-etched carbon nanotube reinforced copper-based composite material |
| CN110894579B (en) * | 2019-12-10 | 2021-05-11 | 昆明理工大学 | Preparation method of hydrogen-etched carbon nanotube reinforced copper-based composite material |
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