CN109052371A - A kind of graphene oxide dispersing Nano carbon tubes solution and preparation method thereof - Google Patents
A kind of graphene oxide dispersing Nano carbon tubes solution and preparation method thereof Download PDFInfo
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- CN109052371A CN109052371A CN201810783218.7A CN201810783218A CN109052371A CN 109052371 A CN109052371 A CN 109052371A CN 201810783218 A CN201810783218 A CN 201810783218A CN 109052371 A CN109052371 A CN 109052371A
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- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
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- C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
Abstract
The invention discloses a kind of graphene oxide dispersing Nano carbon tubes solution and preparation method thereof, which includes carbon nanotube, further include graphene oxide solution, and the ratio between graphene oxide and the mass concentration of carbon nanotube in the solution are (1 ~ 10): 1.The preparation method prepares graphene oxide solution by the amount of water in control oxidation link including step 1, using improved Hummers method；2, it weighs carbon nanotube to be put into container, suitable graphene oxide solution is added, and add alcohol dilution, obtain the suspension of graphene oxide and carbon nanotube；3, graphene oxide and the suspension of carbon nanotube are utilized into ultrasonic stirrer ultrasonic disperse, obtains the carbon nanotube dispersion solution comprising graphene oxide.The problem of it is poor that the present invention solves carbon nanotube dispersion effect, easy secondary agglomeration, in turn avoids the damage of carbon nano tube structure, improves the mechanical property of basis material.
Description
Technical field
The present invention relates to technical field of composite preparation, and in particular to a kind of graphene oxide dispersing Nano carbon tubes solution
And preparation method thereof.
Background technique
Since 1991 Japanese Scientists Sumio Iijima found on argon gas DC arc discharge cathode product carbon nanotube with
Come, has started the carbon nanotube research boom continued to this day.Carbon nanotube is graphite tubular structure, is graphite flake according to one
Determine seamless nanotube made of spiral film song.Carbon nanotube is divided into single wall and two kinds of multi wall, and diameter is in several nanometers to tens
Between nanometer, length can achieve several hundred nanometers to tens microns, and the longest is up to several millimeters of ranks.Carbon nanotube
Draw ratio is about 100-1000, can reach 1000-10000, therefore is considered as a kind of typical monodimension nanometer material.
In recent years carbon nanotube as the reinforcement material in composite material by wide coverage, and achieve it is certain at
Fruit.Research shows that carbon nanotube has apparent improvement to matrix mechanical property and physical property really, but also reports simultaneously
When continuing growing content of carbon nanotubes, the performance of material deteriorates instead.This is mainly due to carbon nanotube draw ratio is big,
And there are stronger Van der Waals force between carbon nanotube, so that it is easily reunited and cause material mechanical performance room for promotion small.According to text
Offer " Rapid and low temperature spark plasma sintering synthesis of novel
carbon nanotube reinforced titanium matrix composites” FC Wang, Carbon, 2015,
The titanium composite material of 95,396-407(fast low temperature discharge plasmas sintering synthesizing carbon nanotubes enhancing, FC Wang,
Carbon, volume 95,396-407,2015), evenly dispersed mass fraction is extremely limited in the base for carbon nanotube,
0.5 wt.% is not all generally exceeded, to increase substantially substrate performance, it is also necessary to improve the additive amount of carbon nanotube, but this
Contradiction is formd again with agglomeration traits itself.The agglomeration traits of carbon nanotube have become restriction Carbon Nanotubes Reinforced Composites
The critical bottleneck problem of technology development.
Summary of the invention
For the agglomeration traits of carbon nanotube, the technical problem to be solved by the invention is to provide a kind of graphene oxides
Dispersing Nano carbon tubes solution, it can improve the dispersibility of carbon nanotube in the base, promote basis material mechanical property.The present invention
A kind of preparation method of graphene oxide dispersing Nano carbon tubes is also provided.
Insight of the invention is that graphene oxide (GO) is a kind of important graphene generated during preparing graphene
Derivative contains a large amount of functional group in structure, and causing graphene oxide in aqueous solution has extraordinary dispersibility.This
The dispersibility for increasing carbon nanotube by the effect of surface of graphene oxide functional group is proposed in invention, is solved carbon nanotube and is reunited
Problem, while the mechanical property of basis material can be greatly improved using the synergistic effect of graphene oxide and carbon nanotube.
A kind of graphene oxide dispersing Nano carbon tubes solution provided by the invention, including carbon nanotube further include oxidation stone
Black alkene solution, the ratio between graphene oxide and the mass concentration of carbon nanotube in the solution are (1 ~ 10): 1.
The present invention also provides a kind of preparation methods of graphene oxide dispersing Nano carbon tubes solution, comprising the following steps:
Step 1, using the improved Hummers method (document that sees reference " Improved Synthesis of Graphene
Oxide, DC Marcano, Acs Nano, 4 (8): 4806-4814,2010, (" synthesis of graphene oxide ", DC
Marcano, Acs nanometers, the 4th phase volume 8, the 4806-4814 pages, 2010)), pass through in control oxidation link plus water
Amount preparation graphene oxide solution；
Step 2 weighs carbon nanotube and is put into container, and suitable graphene oxide solution is added, and adds alcohol dilution, obtains
The suspension of graphene oxide and carbon nanotube；
Graphene oxide and the suspension of carbon nanotube are utilized ultrasonic stirrer ultrasonic disperse by step 3, are obtained comprising oxidation stone
The carbon nanotube of black alkene disperses solution.
Preferably, being aoxidized in link in the step 1 and amount of deionized water is added is 0ml, X-ray photoelectron spectroscopic analysis
(XPS test) C/O(carbon oxygen atom percentage) than being 1.87.
Preferably, being aoxidized in link in the step 1 and amount of deionized water is added is 10ml, and XPS test C/O ratio is
2.09。
Preferably, the ultrasonic disperse time is 10min or more in the step 3.
The solution have the advantages that:
1, the present invention improves the dispersibility of carbon nanotube by the surface functional group of graphene oxide, with existing physics/change
The problem of method is compared, and it is poor to not only solve carbon nanotube dispersion effect, easy secondary agglomeration, while also avoiding carbon nanotube
The damage of structure, to cause the serious destruction of performance.
2, the graphene oxide preparation process that the present invention uses is simple, at low cost, with single carbon nanotube reinforcement phase
Than graphene oxide dispersing Nano carbon tubes solution improves the mechanical property of basis material.
Detailed description of the invention
Detailed description of the invention of the invention is as follows:
Fig. 1 is the both macro and micro organizational topography of embodiment 1；
Fig. 2 is the both macro and micro organizational topography of embodiment 2；
Fig. 3 is the both macro and micro organizational topography of embodiment 3；
Fig. 4 is the both macro and micro organizational topography of embodiment 4；
Fig. 5 is the metallographic microscope pattern comparison diagram of embodiment 1, embodiment 4 and embodiment 5；
Fig. 6 is gained titanium composite material compression stress-compression ratio curve comparison figure in supplement embodiment.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples:
Embodiment 1
Pure nano-carbon tube alcoholic solution is prepared, steps are as follows:
1) 20mg carbon nanotube is weighed in beaker, and adding alcohol to total volume is 100ml, obtains the suspended of carbon nanotube
Liquid；
2) suspension of carbon nanotube is utilized into ultrasonic stirrer ultrasonic disperse 10min, obtains the ultrasound of reunion shape carbon nanotube
Suspension afterwards.
The pure nano-carbon tube alcoholic solution drop of the present embodiment macro morphology such as Fig. 1 (a) after silicon wafer stands 3min is shown, dilute
Release shown in rear SEM microscopic appearance such as Fig. 1 (b): apparent clustering phenomena is presented in carbon nanotube in alcoholic solution, and microstructure is aobvious
Show that carbon nanotube is reunited together, at cotton-shaped distribution, the pattern of single-root carbon nano-tube cannot be distinguished.
Pure nano-carbon tube alcoholic solution manufactured in the present embodiment is for dispersing carbon nanometer with graphene oxide of the invention
Pipe solution compares.
Embodiment 2
The step of preparing the first graphene oxide dispersing Nano carbon tubes solution is as follows:
1) 1g graphite powder (> 325 mesh) and 12.75g CrO3It is added in beaker, is slowly added to 10.5ml HCl (37.5wt.%),
2h is stirred at room temperature in draught cupboard, product is washed with deionized water to after colourless and dries 12h in 60 DEG C of vacuum drying ovens, obtains graphite and inserts
Layer compound；
2) graphite intercalation compound is immersed into 30%H in large beaker2O23 times are washed again after 20h in solution 60ml to be changed
Learn expanded graphite；
3) by chemically expansible graphite impregnation to 98% H of 200ml2SO4 10min removes the water of intercalation, and filters removal excess of sulfur
Acid obtains dehydration expanded graphite；
4) by 120ml H in ice-water bath2SO4、13.3ml H3PO4It is mixed with dehydration expanded graphite, and adds in 30min
Enter 6g KMnO4, ice-water bath is removed, stable system is stirred to react 4h at 50 DEG C, obtains the graphene oxide containing insoluble chromic salts
Solution；
5) system is cooled to room temperature, 200ml ice water and 15ml H is slowly added in 30min2O2, insoluble chromic salts is decomposed,
Obtain glassy yellow graphene oxide solution；
6) 30ml HCl is added in glassy yellow graphene oxide solution, makes overnight precipitation, then graphene oxide is precipitated and is centrifuged
Other ions removed in solution are washed to PH > 5, graphene oxide concentrated solution is obtained；
7) it weighs 20mg carbon nanotube and the graphene oxide concentrated solution containing graphene oxide 20mg is added in beaker, and add
Adding alcohol to total volume is that 100ml is obtained so that graphene oxide concentration is 0.2mg/ml, carbon nanotube concentration 0.2mg/ml
To the suspension of graphene oxide and carbon nanotube；
8) graphene oxide alkene and the suspension of carbon nanotube are utilized into ultrasonic stirrer ultrasonic disperse, obtain graphene oxide and
The mixed solution of carbon nanotube.
The graphene oxide concentration of the present embodiment is that 0.2mg/ml mixing liquid drips the macro morphology after silicon wafer stands 3min
As shown in Fig. 2 (a), after dilution shown in SEM microscopic appearance such as Fig. 2 (b), the alcoholic solution phase with the pure nano-carbon tube of embodiment 1
Than after adding graphene oxide solution, the dispersibility of carbon nanotube has apparent improvement, but also has the group of a certain amount of small size
Tufted substance exists.It sees that large stretch of cotton-shaped carbon nanotube is broken up in microstructure, the carbon nanotube region of fritter is presented,
And it links together each other, local cell domain carbon nanotube is still the phenomenon that presentation is reunited.
Embodiment 3
The step of preparing second of graphene oxide dispersing Nano carbon tubes solution is as follows:
1) 1g graphite powder (> 325 mesh) and 12.75g CrO3It is added in beaker, is slowly added to 10.5ml HCl (37.5wt.%),
2h is stirred at room temperature in draught cupboard, and product is washed with deionized water to after colourless and dries 12h in 60 DEG C of vacuum drying ovens, obtains graphite intercalation
Compound；
2) graphite intercalation compound is immersed into 30%H in large beaker2O23 times are washed again after 20h in solution 60ml to be changed
Learn expanded graphite；
3) by chemically expansible graphite impregnation to 200ml 98%H2SO410min removes the water of intercalation, and filters removal excess of sulfur
Acid obtains dehydration expanded graphite；
4) by 120ml H in ice-water bath2SO4、13.3ml H3PO4It is mixed with dehydration expanded graphite, and adds in 30min
Enter 6g KMnO4, ice-water bath is removed, stable system is stirred to react 4h at 50 DEG C, obtains the graphene oxide containing insoluble chromic salts
Solution；
5) system is cooled to room temperature, 200ml ice water and 15ml H is slowly added in 30min2O2, insoluble chromic salts is decomposed,
Obtain glassy yellow graphene oxide solution；
6) 30ml HCl is added in glassy yellow graphene oxide solution, makes overnight precipitation, then graphene oxide is precipitated and is centrifuged
Other ions removed in solution are washed to PH > 5, graphene oxide concentrated solution is obtained；
7) it weighs 20mg carbon nanotube and the graphene oxide concentrated solution containing graphene oxide 100mg is added in beaker, and add
Adding alcohol to total volume is that 100ml is obtained so that graphene oxide concentration is 1mg/ml, carbon nanotube concentration 0.2mg/ml
The suspension of graphene oxide and carbon nanotube；
8) graphene oxide alkene and the suspension of carbon nanotube are utilized into ultrasonic stirrer ultrasonic disperse, obtain graphene oxide and
The mixed solution of carbon nanotube.
The graphene oxide concentration of the present embodiment be 1mg/ml mixing liquid drip in silicon wafer stand 3min after macro morphology such as
Shown in Fig. 3 (a), SEM microscopic appearance is such as shown in Fig. 3 (b) after dilution: no matter from increase oxygen in macrostructure or microstructure
The content of graphite alkene is all conducive to the dispersibility of carbon nanotube, and the opposite embodiment 2 of dispersibility has further improvement, from micro-
It sees result and sees that carbon nanotube is integrally presented and is uniformly dispersed, fritter carbon nanotube region no longer links together, but part is still deposited
In cotton-shaped distribution.
Embodiment 4
The step of preparing the third graphene oxide dispersing Nano carbon tubes solution is as follows:
1) 1g graphite powder (> 325 mesh) and 12.75g CrO3 are added in beaker, are slowly added to 10.5ml HCl (37.5wt.%),
2h is stirred at room temperature in draught cupboard, product is washed with deionized water to after colourless and dries 12h in 60 DEG C of vacuum drying ovens, obtains graphite and inserts
Layer compound；
2) graphite intercalation compound is immersed into 30% H in large beaker2O23 times are washed again after 20h in solution 60ml to be changed
Learn expanded graphite；
3) by chemically expansible graphite impregnation to 98% H2 of 200mlSO410min removes the water of intercalation, and filters removal excess of sulfur
Acid obtains dehydration expanded graphite；
4) by 120ml H in ice-water bath2SO4, 13.3ml H3PO4 and dehydration expanded graphite be mixed, and in 30min
6g KMnO4 is added, removes ice-water bath, stable system is stirred to react 4h at 50 DEG C, obtains the graphite oxide containing insoluble chromic salts
Alkene solution；
5) system is cooled to room temperature, 200ml ice water and 15mlH is slowly added in 30min2O2, insoluble chromic salts is decomposed, is obtained
To glassy yellow graphene oxide solution；
6) 30ml HCl is added in glassy yellow graphene oxide solution, makes overnight precipitation, then graphene oxide is precipitated and is centrifuged
Other ions removed in solution are washed to PH > 5, graphene oxide concentrated solution is obtained；
7) it weighs 20mg carbon nanotube and the graphene oxide concentrated solution containing graphene oxide 200mg is added in beaker, and add
Adding alcohol to total volume is that 100ml is obtained so that graphene oxide concentration is 2mg/ml, carbon nanotube concentration 0.2mg/ml
The suspension of graphene oxide and carbon nanotube；
8) graphene oxide alkene and the suspension of carbon nanotube are utilized into ultrasonic stirrer ultrasonic disperse, obtain graphene oxide and
The mixed solution of carbon nanotube.
The graphene oxide concentration of the present embodiment be 2mg/ml mixing liquid drip in silicon wafer stand 3min after macro morphology such as
Shown in Fig. 4 (a), after dilution shown in SEM microscopic appearance such as Fig. 4 (b): when the mass ratio of graphene oxide and carbon nanotube improve to
When 10:1, mixed solution is relatively uniform, and the nearly imperceptible Cluster Phenomenon of macroscopic view, microstructure is seen that carbon nanotube is available and filled
That divides is evenly dispersed, and agglomeration will not occur.
The XPS of the present embodiment graphene oxide dispersing Nano carbon tubes solution is tested, and C/O ratio is 1.87.
Embodiment 5
The step of preparing the 4th kind of graphene oxide dispersing Nano carbon tubes solution is not both with embodiment 4:
4) by 120ml H in ice-water bath2SO4、13.3ml H3PO4It mixes and stirs with dehydration expanded graphite with 10ml deionized water
It mixes.
The XPS of the present embodiment graphene oxide dispersing Nano carbon tubes solution is tested, and C/O ratio is 2.09.Embodiment 4 and implementation
Example 5 is compared, and oxygen content is greater than embodiment 5, the oxidation of embodiment 4 in the graphene oxide dispersing Nano carbon tubes solution of embodiment 4
Graphene dispersion carbon nano-tube solution degree of oxidation is high.
In Fig. 5, (a) is the pure nano-carbon tube alcoholic solution of embodiment 1 in metallographic microscope shape appearance figure；It (b) is embodiment 4
GO concentration be 2mg/ml, C/O ratio be 1.87 carbon nanotube mixing liquids in metallographic microscope shape appearance figure；It (c) is embodiment 5
Graphene oxide concentration is that 2mg/ml, C/O ratio are 2.09 carbon nanotube mixing liquids in metallographic microscope shape appearance figure.In terms of Fig. 5
Out, carbon nanotube dispersibility ratio Fig. 5 (c) of Fig. 5 (b) more preferably, so the graphene oxide of different degree of oxidation is to carbon nanotube
Dispersibility, which improves, to be had a certain impact, and with the raising of graphene oxide degree of oxidation, improves effect to the dispersibility of carbon nanotube
Fruit is better.
Supplement embodiment
1, institute's carbon nanotubes in 1 gained pure nano-carbon tube alcoholic solution of embodiment is mixed with titanium valve 0.005:1 in mass ratio,
It is uniformly distributed two-phase using 10 min of ultrasonic stirrer ultrasonic disperse, obtains the mixed solution of carbon nanotube and titanium valve；
Above-mentioned mixed solution is placed in water-bath and is stirred for 24 hours to substantially dry, is dried in vacuum drying oven drying time 12h,
Obtain the composite granule of carbon nanotube and titanium valve mixing；
Above-mentioned mixed composite granule is pressurizeed 200MPa in a mold, keeps 1min, obtains carbon nanotube and titanium valve mixing
Composite powder column；
The composite powder column is put into tube furnace and is sintered under argon gas protection environment, sintering heating rate is 10 DEG C/min,
Being sintered maximum temperature is 1050 DEG C, and the heat preservation sintering time is 3h, then furnace cooling, obtains the titanium-based material of carbon nanotube enhancing
Material.Learn that the yield strength of the material of preparation is 526.7MPa from test (using GB/T 7314-1987 testing standard) result,
Compressive strength is 1550.1MPa.
Titanium base material compression stress-compression ratio curve of carbon nanotube enhancing is as shown in the darker curve in Fig. 6.
2, the total amount and titanium valve of institute's carbon nanotubes and graphene oxide in 2 gained of embodiment solution of the invention are pressed into matter
Amount is mixed than 0.005:1, is uniformly distributed two-phase using 10 min of ultrasonic stirrer ultrasonic disperse, is obtained graphene oxide, carbon
The mixed solution of nanotube and titanium valve；
Above-mentioned mixed solution is placed in water-bath and is stirred for 24 hours to substantially dry, is dried in vacuum drying oven drying time 12h,
Obtain the composite granule of graphene oxide, carbon nanotube and titanium valve mixing；
Above-mentioned mixed composite granule is pressurizeed 200MPa in a mold, keeps 1min, obtain graphene oxide, carbon nanotube and
The composite powder column of titanium valve mixing；
The composite powder column is put into tube furnace and is sintered under argon gas protection environment, sintering heating rate is 10 DEG C/min,
Being sintered maximum temperature is 1050 DEG C, and the heat preservation sintering time is 3h, and then furnace cooling, obtains graphene oxide and carbon nanotube
Cooperate with the titanium base material of enhancing.Learn that the material of preparation is bent from test (using GB/T 7314-1987 testing standard) result
Taking intensity is 829.3MPa, compressive strength 2088.8MPa.
The graphene oxide is cooperateed with carbon nanotube in the titanium base material compression stress-compression ratio curve such as Fig. 6 of enhancing
Shown in lighter curve.As seen from Figure 6: the mechanical property of graphene oxide and the titanium base material of carbon nanotube collaboration enhancing is than pure
Carbon nanotube reinforcement titanium base material is superior.
Graphene oxide preparation process is simple, at low cost, as the reinforcement of composite material, is dispersed using graphene oxide
Carbon nano-tube solution can be effectively reduced the additive amount of pure nano-carbon tube, reduce the production cost of composite material.
Claims (5)
1. a kind of graphene oxide dispersing Nano carbon tubes solution, including carbon nanotube, it is characterized in that: further including that graphene oxide is molten
Liquid, the ratio between graphene oxide and the mass concentration of carbon nanotube in the solution are (1 ~ 10): 1.
2. the preparation method of graphene oxide dispersing Nano carbon tubes solution described in a kind of claim 1, characterized in that including following
Step:
Step 1 prepares graphene oxide solution by the amount of water in control oxidation link using improved Hummers method；
Step 2 weighs carbon nanotube and is put into container, and suitable graphene oxide solution is added, and adds alcohol dilution, obtains
The suspension of graphene oxide and carbon nanotube；
Graphene oxide and the suspension of carbon nanotube are utilized ultrasonic stirrer ultrasonic disperse by step 3, are obtained comprising oxidation stone
The carbon nanotube of black alkene disperses solution.
3. preparation method according to claim 2, characterized in that aoxidized in link in the step 1 and deionization is added
Water is 0ml, and it is 1.87 that XPS, which tests C/O ratio,.
4. preparation method according to claim 2, characterized in that aoxidized in link in the step 1 and deionization is added
Water is 10ml, and it is 2.09 that XPS, which tests C/O ratio,.
5. preparation method according to claim 1, characterized in that in the step 3 the ultrasonic disperse time be 10min with
On.
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| CN111154144A (en) * | 2020-02-14 | 2020-05-15 | 台州学院 | Preparation method of graphene oxide reinforced carbon fiber material |
| CN111440378A (en) * | 2020-05-09 | 2020-07-24 | 国网湖南省电力有限公司 | Semiconductive shielding composite material, preparation method thereof and application thereof in power cable |
| CN112441777A (en) * | 2019-08-30 | 2021-03-05 | 西安美刚达科技发展有限公司 | Nano fireproof material and preparation method thereof |
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| CN109666821A (en) * | 2019-02-14 | 2019-04-23 | 重庆大学 | A kind of titanium composite material and preparation method thereof |
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| CN112441777A (en) * | 2019-08-30 | 2021-03-05 | 西安美刚达科技发展有限公司 | Nano fireproof material and preparation method thereof |
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| CN111440378A (en) * | 2020-05-09 | 2020-07-24 | 国网湖南省电力有限公司 | Semiconductive shielding composite material, preparation method thereof and application thereof in power cable |
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