CN107055512A - The method that the high dielectric filler of hud typed CNT is prepared using sol-gal process - Google Patents
The method that the high dielectric filler of hud typed CNT is prepared using sol-gal process Download PDFInfo
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- CN107055512A CN107055512A CN201710045087.8A CN201710045087A CN107055512A CN 107055512 A CN107055512 A CN 107055512A CN 201710045087 A CN201710045087 A CN 201710045087A CN 107055512 A CN107055512 A CN 107055512A
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Abstract
The method for preparing the high dielectric filler of hud typed CNT using sol-gal process belongs to field of composite material preparation.This filler is prepared by the method for sol gel sintered, it is main that sol-gel system solution is formed in absolute ethyl alcohol system using strontium nitrate and butyl titanate, add surfactant sodium dodecyl base benzene sulfonic acid sodium salt and acidifying CNT, make colloidal particle in multi-wall carbon nano-tube pipe surface formation sol gel layer, surfactant reduces carbon nano tube surface energy with carbon nano tube surface formation conjugation, so as to increase absorption of the ion in multi-walled carbon nanotube.High-temperature calcination processing is carried out after being dried through suction filtration in a nitrogen atmosphere and obtains final product.The consumption that this method passes through control surface activating agent, a series of high dielectric filler of hud typed multi-walled carbon nanotube of different-shapes is finally given, process conditions are simple, and experimental period is short, it is the effective way for preparing the high dielectric filler of hud typed CNT, with very excellent exploitation and application prospect.
Description
Technical field
The present invention is on preparing the strontium titanates cladding hud typed high dielectric filler of multi-walled carbon nanotube using sol-gel process
Preparation method, belong to composite preparation technical field.
Background technology
CNT has the hollow structure and high specific surface area of uniqueness as a kind of new carbonaceous Nano-Materials,
This special structure imparts its a variety of excellent performance.Such as excellent mechanical property, electric property, thermodynamic property,
Other good performances such as magnetic behavior and optical property.In being found in widely studied more than 20 years for CNT,
CNT in capacitor, hydrogen storage material, catalyst carrier, enhancing composite, the every field such as probe microscope tip all
It is widely used.And in recent years for the surface modified also always as the focus studied both at home and abroad of CNT
Receive the extensive concern of people.In related research, worker generally coats one layer of polymeric, metal, nothing in carbon pipe surface
Machine ceramic material etc., to form a kind of nano-core-shell structure material.Polymer overmold CNT, can make material formation with poly-
Compound is the nanowires material that insulating barrier CNT is electrically conductive core, is likely to become the wire of nano-device from now on, secondly
Polymer covering layer can also cause CNT to disperse in the composite evenly；Metallic cover CNT is main
Using its one-dimensional, there is supported catalyst very high specific surface area can greatly improve catalytic efficiency on the carbon nanotubes,
It may also be used simultaneously as ripple shielding material is inhaled；Inorganic ceramic material enveloped carbon nanometer tube can also assign its new characteristic,
Such as high dielectric ceramic barium titanate enveloped carbon nanometer tube can make its dielectric properties increase, and high heat conduction boron nitride can make carbon receive
The heat conductivility of mitron increases.
Strontium titanates is a kind of emerging multifunction electronic ceramic material.Many studies have shown that, cubic perovskite type strontium titanates
After reduction or doping, its dielectric properties is excellent, dielectric loss is low, dispersion frequency is high, heat endurance is good, and also excellent
Semiconducting behavior, may be utilized in fabricating mesohigh Large Copacity ceramic capacitor, grain-boundary layer capacitor, piezo-resistance, thermistor
And Multifunction Sensor.Recently as developing rapidly for science and technology, high accuracy, Gao Ke are proposed to electrode component
Preparation and research by property, multi-functional, miniaturization requirement, therefore high-purity, ultra-fine, uniform strontium titanates are always an active neck
Domain.Nanometer SrTiO is prepared at present3Powder method can be divided into solid phase method, liquid phase method and vapor phase method.Wherein vapor phase method primarily directed to
Material film in the form of sheets is prepared, equipment cost is higher, is unfavorable for market-oriented popularization.Comparative maturity is applied in solid phase method and wide
General is high-temperature solid-phase sintering method, and it is simple by process equipment, easy to operate, available for industrial large-scale production metatitanic acid
Strontium, but due to substantial amounts of chemical bond rupture and restructuring must be made during synthetic material, and atom will also make certain distance
Migration so that the process must be carried out at a higher temperature, and the temperature of solid sintering technology synthesis strontium titanates is general 1000
More than DEG C, therefore material synthesized by the method is difficult to meet photochemical catalyst small size, bigger serface and there are as far as possible
The requirement of beneficial defective bit.Wet chemistry method due in course of reaction each raw material reacted to each other with liquid form, reach atomic level
Contact, improves the uniformity and adequacy of reaction system, has effectively facilitated the formation of crystalline phase, preparing photocatalyst material side
Face shows many superior conditions.Wet chemical method mainly includes coprecipitation, water-bath synthetic method and sol-gal process,
This be also synthesis photochemical catalyst experimental study in pass through frequently with material preparation method.
In many researchs in recent years, the research for strontium titanates enveloped carbon nanometer tube is very rare, but has very
Many workers have attempted to make barium titanate be coated on multi-walled carbon nanotube using Chemical Physics method.Wherein have and use hydro-thermal legal system
Standby barium titanate cladding multi-walled carbon nanotube, pulse ion sputtering prepare the methods such as barium titanate cladding multi-walled carbon nanotube.Use for reference all
The method of many barium titanate enveloped carbon nanometer tubes, we devise adds in strontium nitrate and butyl titanate sol-gel solution
Multi-walled carbon nanotube and neopelex are acidified, by filtering, drying and calcination processing, strontium titanates bag has been obtained
The hud typed high dielectric filler of acidifying multi-walled carbon nanotube covered.Research discovery, surfactant sodium dodecyl base benzene sulfonic acid sodium salt structure
Phenyl ring in formula can form conjugation with the hexatomic ring of carbon nano tube surface and adsorb on tube wall, so as to drop low-carbon nano
The surface energy of pipe, adds absorption of the nano-particle in carbon nano tube surface；The colloidal particle in system is inhaled by electrostatic simultaneously
Attached effect absorption considerably increases adhesion amount of the particle in carbon nano tube surface, so as to solve metatitanic acid in carbon nano tube surface
The problem of strontium cladding is uneven.And can be realized to carbon nano tube surface cladding thickness by the consumption of control surface activating agent
The controllable adjustment of degree.
The content of the invention
The high dielectric filler of hud typed CNT is prepared it is an object of the invention to provide a kind of utilization sol-gel process
Preparation method.In preparation process, strontium nitrate and butyl titanate collosol-gelatum system solution are configured first, then many wall carbon are received
Mitron is added in sol-gel system with neopelex, the stirring ageing 3h under 40 DEG C of water bath conditions.Through suction filtration,
High-temperature calcination is handled after drying, obtains the final strontium titanates cladding hud typed high dielectric filler of multi-walled carbon nanotube.This filler
It can be widely applied to the preparation and research of dielectric material.
The strontium titanates cladding multi-walled carbon nanotube that the present invention is provided prepares the preparation process of hud typed high dielectric filler,
Comprise the concrete steps that：
(1) configuration strontium nitrate and butyl titanate collosol-gelatum system solution；
(2) that a certain proportion of multi-walled carbon nanotube and neopelex are added into (1) collosol-gelatum system is molten
In liquid, ultrasonic disperse 1h；
(3) (2) system is stirred to vacuum drying after ageing 3h, suction filtration under 40 DEG C of water bath conditions；
(4) product for drying (3) carries out high-temperature calcination processing under 800 DEG C of nitrogen atmospheres and obtains target product.
The method that the high dielectric filler of hud typed CNT is prepared using sol-gel process, it is characterised in that specific steps
It is：
1) 2.815g strontium nitrates are dissolved in 25 milliliters of deionized water, 10min is stirred at 40 DEG C makes it fully dissolve,
It is denoted as solution A；
2) 4.526g butyl titanate is added in 40 milliliters of absolute ethyl alcohol, 15min is stirred at 40 DEG C makes it
Fully dissolving, is denoted as solution B；
3) by step 1) in solution A be added drop-wise to step 2 dropwise) in solution B in, it is to be mixed it is uniform after use glacial acetic acid
PH value is adjusted, pH=4-6 is obtained mixed solution；
4) by step 3) in obtained mixed solution at 40 DEG C plus stirring fully reaction 1h, then 0.1g is acidified into many wall carbon
Nanotube and surfactant sodium dodecyl base benzene sulfonic acid sodium salt are added in above-mentioned mixed solution, wherein neopelex matter
Amount is be acidified multi-walled carbon nanotube quality 0.5-10 times；；By mixed solution ultrasonic disperse 1h, continue under 40 DEG C of water bath conditions
Stirring 3h makes the abundant solation of mixed solution；；
5) after reaction stops, suction filtration obtains the multi-wall carbon nano-tube pipe powder with strontium titanates precursor sol layer, and vacuum is done
Dry removal solvent；
6) dried powder is subjected to calcination processing in a nitrogen atmosphere, obtains final product, be denoted as STO-MWCNTs.
Further, the step 6) in calcination processing thermograde be 500 DEG C of constant temperature 1h, then in 800 DEG C of constant temperature 2h.
Further, carboxyl-content is in acidifying multi-walled carbon nanotube：1.23-2.00wt%.
The sol-gel process that the present invention is provided prepares the side that strontium titanates coats the hud typed high dielectric filler of multi-walled carbon nanotube
The characteristics of method is：
1. using the colloidal particle in strontium nitrate and butyl titanate collosol-gelatum system in multi-wall carbon nano-tube pipe surface
The conjugation of electrostatic adsorption and neopelex and multi-wall carbon nano-tube tube wall interacts, to realize that strontium titanates exists
The cladding of multi-wall carbon nano-tube pipe surface；
2. compared to traditional preparation methods, this programme calcining heat is low, the constant temperature 2h only at 800 DEG C, you can make strontium titanates brilliant
Body is firmly attached on multi-wall carbon nano-tube tube wall, and difficult for drop-off；
3. the controllable of multi-walled carbon nanotube surface coating layer thickness can be realized by control surface activating agent consumption；
4. the program is short experimental period, simple to operate, low toxicity and yield height.
Brief description of the drawings
Fig. 1：The sol-gel process that the present invention is provided prepares the process chart of the high dielectric filler of hud typed CNT.
Fig. 2：The sol-gel process that the present invention is provided prepares the sintering heating curve of the high dielectric filler of hud typed CNT
Figure.
Fig. 3：Sol-gel process prepares the transmission electron microscope photo of the high dielectric filler of hud typed CNT.
A) surfactant SDBS and multi-walled carbon nanotube mass ratio are 1:2
B) surfactant SDBS and multi-walled carbon nanotube mass ratio are 1:1
C) surfactant SDBS and multi-walled carbon nanotube mass ratio are 5:1
D) surfactant SDBS and multi-walled carbon nanotube mass ratio are 10:1
Fig. 4：The XRD of the high dielectric filler of hud typed CNT (STO-MWCNTs) is prepared using sol-gel process.
Fig. 5：Sol-gel process prepares the reaction mechanism figure of the high dielectric filler of hud typed CNT.
Embodiment
Embodiment 1
25ml deionized waters are poured into 50 milliliters of beakers, is put into water-bath and is heated to 40 DEG C, in the work of magnetic agitation
Addition 2.815g strontium nitrates under, are completely dissolved it and are denoted as solution A；40 milliliters of absolute ethyl alcohols are added to 250 milliliters of burnings
In cup, it is put into water-bath and is heated to 40 DEG C, the addition 4.526g butyl titanates in the presence of magnetic agitation make its complete
Dissolving is denoted as solution B；In the beaker for solution B solution A being added drop-wise under magnetic agitation, after reacting 1h after completion of dropping.Upwards
State and 0.1g acidifyings multi-walled carbon nanotube is added in mixed solution (carboxyl-content is：1.23-2.00wt%) with 0.05g dodecyls
Benzene sulfonic acid sodium salt ultrasonic disperse 1h.Afterwards mixed solution is stopped reacting in 40 DEG C of water-bath plus after stirring continuation reaction 3h,
Sintered in a nitrogen atmosphere after suction filtration vacuum drying again, its heating curve is as shown in Figure 2.Final product is obtained after sintered.
Fig. 3 (a) is hud typed high dielectric filler (particular flow sheet such as figure of strontium titanates cladding multi-walled carbon nanotube manufactured in the present embodiment
Shown in 1) transmission electron microscope photo.It can be seen that there is a small amount of strontium titanates particle to adhere in multi-wall carbon nano-tube pipe outer wall,
Surfactant SDBS and multi-walled carbon nanotube mass ratio are 1:Under conditions of 2, reach strontium titanates nano-particle in carbon
The Expected Results of nanotube surface part attachment.
Embodiment 2
25 ml deionized waters are poured into 50 milliliters of beakers, is put into water-bath and is heated to 40 DEG C, in magnetic agitation
Addition 2.815g strontium nitrates under effect, are completely dissolved it and are denoted as solution A；40 milliliters of absolute ethyl alcohols are added to 250 milliliters
In beaker, it is put into water-bath and is heated to 40 DEG C, the addition 4.526g butyl titanates in the presence of magnetic agitation makes its complete
Fully dissolved is denoted as solution B；In the beaker for solution B solution A being added drop-wise under magnetic agitation, after reacting 1h after completion of dropping.To
0.1g acidifyings multi-walled carbon nanotube is added in above-mentioned mixed solution, and (carboxyl-content is：1.23-2.00wt%) with 0.1g dodecanes
Base benzene sulfonic acid sodium salt ultrasonic disperse 1h.Mixed solution is stopped in 40 DEG C of water-bath plus after stirring continuation reaction 3h afterwards anti-
Should, then sintered in a nitrogen atmosphere after suction filtration vacuum drying, its heating curve is as shown in Figure 2.Finally produced after sintered
Thing.Fig. 3 (b) is that the transmission electron microscope of the hud typed high dielectric filler of strontium titanates cladding multi-walled carbon nanotube manufactured in the present embodiment shines
Piece.As can be seen from the figure after dosage of surfactant reaches 0.1g, there is strontium titanates particle accumulation layer segment to be attached to carbon and receive
On mitron outer wall, there are more strontium titanates nano-particles to coat compared to embodiment 1.Demonstrate surfactant SDBS and many
Wall carbon nano tube mass ratio is 1:When 1, strontium titanates can have been reached in the most cladding of multi-wall carbon nano-tube pipe surface, but wrap
Cover complete not enough.
Embodiment 3
25 ml deionized waters are poured into 50 milliliters of beakers, is put into water-bath and is heated to 40 DEG C, in magnetic agitation
Addition 2.815g strontium nitrates under effect, are completely dissolved it and are denoted as solution A；40 milliliters of absolute ethyl alcohols are added to 250 milliliters
In beaker, it is put into water-bath and is heated to 40 DEG C, the addition 4.526g butyl titanates in the presence of magnetic agitation makes its complete
Fully dissolved is denoted as solution B；In the beaker for solution B solution A being added drop-wise under magnetic agitation, after reacting 1h after completion of dropping.To
0.1g acidifyings multi-walled carbon nanotube is added in above-mentioned mixed solution, and (carboxyl-content is：1.23-2.00wt%) with 0.5g dodecanes
Base benzene sulfonic acid sodium salt ultrasonic disperse 1h.Mixed solution is stopped in 40 DEG C of water-bath plus after stirring continuation reaction 3h afterwards anti-
Should, then sintered in a nitrogen atmosphere after suction filtration vacuum drying, its heating curve is as shown in Figure 2.Finally produced after sintered
Thing.Fig. 3 (c) is that the transmission electron microscope of the hud typed high dielectric filler of strontium titanates cladding multi-walled carbon nanotube manufactured in the present embodiment shines
Piece.From unlike embodiment 1, embodiment 2, passing through enlarged surface activating agent SDBS usage amount so that surfactant
SDBS and multi-walled carbon nanotube mass ratio are 5:When 1, the multi-wall carbon nano-tube pipe surface finally given has complete strontium titanates to receive
Rice grain clad, shows that introduce more surfactant sodium dodecyl base benzene sulfonic acid sodium salts reduces multi-walled carbon nanotube really
Surface can so that more ions can be attached to its surface, and forming obvious strontium titanates on its surface after oversintering receives
Rice grain clad.
Embodiment 4
25 ml deionized waters are poured into 50 milliliters of beakers, is put into water-bath and is heated to 40 DEG C, in magnetic agitation
Addition 2.815g strontium nitrates under effect, are completely dissolved it and are denoted as solution A；40 milliliters of absolute ethyl alcohols are added to 250 milliliters
In beaker, it is put into water-bath and is heated to 40 DEG C, the addition 4.526g butyl titanates in the presence of magnetic agitation makes its complete
Fully dissolved is denoted as solution B；In the beaker for solution B solution A being added drop-wise under magnetic agitation, after reacting 1h after completion of dropping.To
0.1g acidifyings multi-walled carbon nanotube is added in above-mentioned mixed solution, and (carboxyl-content is：1.23-2.00wt%) with 1g dodecyls
Benzene sulfonic acid sodium salt ultrasonic disperse 1h.Afterwards mixed solution is stopped reacting in 40 DEG C of water-bath plus after stirring continuation reaction 3h,
Sintered in a nitrogen atmosphere after suction filtration vacuum drying again, its heating curve is as shown in Figure 2.Final product is obtained after sintered.
Fig. 3 (d) is the transmission electron microscope photo of the hud typed high dielectric filler of strontium titanates cladding multi-walled carbon nanotube manufactured in the present embodiment.
It can be seen that being 10 in surfactant SDBS and multi-walled carbon nanotube mass ratio:Under conditions of 1, strontium titanates cladding
Thickness degree substantially increases, and this is also demonstrated again that can be effective by changing the consumption of surfactant sodium dodecyl base benzene sulfonic acid sodium salt
Regulate and control the thickness of carbon nano tube surface clad.
Claims (3)
1. the method for preparing the high dielectric filler of hud typed CNT using sol-gel process, it is characterised in that comprise the concrete steps that：
1) 2.815g strontium nitrates are dissolved in 25 milliliters of deionized water, 10min is stirred at 40 DEG C makes it fully dissolve, and is denoted as
Solution A；
2) 4.526g butyl titanate is added in 40 milliliters of absolute ethyl alcohol, 15min is stirred at 40 DEG C makes its abundant
Dissolving, is denoted as solution B；
3) by step 1) in solution A be added drop-wise to step 2 dropwise) in solution B in, it is to be mixed it is uniform after adjusted using glacial acetic acid
PH value, makes pH=4-6 obtain mixed solution；
4) by step 3) in obtained mixed solution at 40 DEG C plus stirring fully reaction 1h, then 0.1g is acidified into multi-wall carbon nano-tube
Pipe and surfactant sodium dodecyl base benzene sulfonic acid sodium salt are added in above-mentioned mixed solution, and wherein neopelex quality is
It is acidified 0.5-10 times of multi-walled carbon nanotube quality；；By mixed solution ultrasonic disperse 1h, continue to stir under 40 DEG C of water bath conditions
3h makes the abundant solation of mixed solution；；
5) after reaction stops, suction filtration obtains the multi-wall carbon nano-tube pipe powder with strontium titanates precursor sol layer, and vacuum drying is gone
Except solvent；
6) dried powder is subjected to calcination processing in a nitrogen atmosphere, obtains final product, be denoted as STO-MWCNTs.
2. the method as described in claim 1, it is characterised in that the step 6) in calcination processing thermograde be 500 DEG C of perseverances
Warm 1h, then in 800 DEG C of constant temperature 2h.
3. the method as described in claim 1, it is characterised in that：Carboxyl-content is in acidifying multi-walled carbon nanotube：1.23-
2.00wt%.
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Citations (1)
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|---|---|---|---|---|
| CN104609456A (en) * | 2014-12-31 | 2015-05-13 | 浙江理工大学 | Preparation method for C/N co-doped porous cuprous oxide nanospheres based on sericin protein |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609456A (en) * | 2014-12-31 | 2015-05-13 | 浙江理工大学 | Preparation method for C/N co-doped porous cuprous oxide nanospheres based on sericin protein |
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| ARCHANA PANDEY ET AL: "Very Stable Electron Field Emission", 《ACS NANO》 * |
| HIROSHI TABATA ET AL: "Metal-oxide-layer-coated single-walled carbon nanotubes as a sensor for trace amounts of oxygen", 《APPLIED PHYSICS EXPRESS》 * |
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