CN105948017A - Carbon nanofiber filled with metal oxide nanoparticles and preparation method thereof - Google Patents
Carbon nanofiber filled with metal oxide nanoparticles and preparation method thereof Download PDFInfo
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- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/10—Filled nanotubes
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
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- C01B2202/36—Diameter
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention relates to carbon nanofiber filled with metal oxide nanoparticles and a preparation method thereof. The carbon nanofiber filled with the metal oxide nanoparticles is prepared through the following steps: filling carbon nanofiber tubes with a metal salt solution under the action of milling, and carrying out drying and calcination, wherein the particle sizes of the metal oxide nanoparticles are in a range of 5 to 30 nm. The method provided by the invention has the characteristics of short filling time, capability of realizing high filling volume, simple process, greenness, environmental protection, low cost, easiness in industrialization, etc.; and the obtained carbon nanofiber has excellent mechanical and chemical stability, and has good application prospects in the fields of catalysis, sensors, electromagnetic shielding, new energy, biotechnology, high-performance composite materials, etc.
Description
Technical field
The invention belongs to carbon nanomaterial processing and applied technical field, be specifically related to a kind of metal-oxide and receive
Carbon nano-fiber that rice corpuscles is filled and preparation method thereof.
Background technology
Carbon nano-fiber or this kind of carbon nanomaterial of CNT have hollow structure and are nanoscale, permissible
Fill there is the nano material of functional characteristic, thus obtain and a kind of be totally different from packing material and be filled
The hybrid material of carbon nanomaterial.So filling technique becomes the focus of people's research to relevant applied research.
Carbon nano-fiber and CNT belong to nano-carbon material together, have a lot of similarity, the most all have and receive
Metrical scale, hollow structure, excellent electricity, magnetic, heat and mechanical performance and close preparation method.The two
Mainly there is difference at appearance structure, size, process technique and one-tenth present aspect.The common list of CNT
Wall carbon nano tube, double-walled carbon nano-tube and multi-walled carbon nano-tubes polytype, be seen as being rolled up by graphene layer
The tubular material with nanoscale of Qu Ercheng, and carbon nano-fiber common " folded cup " and " arranged in parallel "
Etc. type；The external diameter of CNT and internal diameter are general respectively 3～80nm and 1～15nm, outside carbon nano-fiber
Footpath and internal diameter are general respectively 100～200nm and 30～150nm；CNT the most easily tangles, be difficult to point
Dissipate, application need, through techniques such as complicated purification, surface modification and modifications, cause integrated cost higher,
And carbon nano-fiber is loosely organized, easily disperse, processes technique simple, thus there is lower integrated cost.
Take the lead in having obtained filling the multi-walled carbon nano-tubes of Pb from Ajayan in 1993 since, people are so far
Utilize various method that with simple substance or compound form (in the majority with oxide), tens kinds of elements are filled out inhomogeneity
In the CNT of type, current fill method mainly includes liquid phase wet chemical method, solid phase fusion method, electric arc
Electric discharge, catalytic pyrolysis method etc..CNT after filling, especially fills nano metal or metal
The nano container of oxide, magnetic storage, nano electron device, nanocatalyst, new energy materials,
The fields such as sensor, microelectrode, orientation reinforcing material show and highlight application potential widely.Liquid phase humidifying
Method is the method that carbon nano-tube filled metal-oxide is conventional, it is common that by molten for some soluble metallic salts
Liquid is filled in CNT pipe under capillarity, is then passed through thermal decomposition process and makes slaine be decomposed into
Oxide, the method has that technique simply and readily controls, preparation temperature is low, can filler kind select
The advantages such as many.From the existing document report (.SnO such as Zhang Ying2Filling carbon nano-pipe electrochemical lithium storage research [J].
Power technology 01 phase in 2005) and patented technology (CN 1704376, CN101962169A, CN 101456074)
From the point of view of, liquid phase wet chemical method is typically necessary, with strong acid, CNT is carried out oxidation processes, it is therefore an objective to beat
Opening the end cap of CNT and form unlimited filling channel, this process typically takes longer, a few hours extremely
Tens of hours, in soluble metal salt solution, soak tens of hours to tens of days time the most again,
Therefore there is the most for a long time, have carbon nano tube structure to a certain extent the weak point of destruction in the method,
Affected additionally, due to by solvent effect in filling process, the implant amount obtained in CNT is few, in
Discrete particle.In some application especially in the fields such as nano-catalytic, battery electrode material, sensor,
The metal oxide filled carbon nanotube that existing patented technology obtains still has bigger lifting empty on usefulness plays
Between.This mainly shows two aspects, and one is that CNT is easily reunited, and difficult dispersion, two is CNT
Internal diameter is less, and filler metal oxide surrounding space is restricted, and these two aspects is to the mass transfer in course of reaction
Or surface reaction activity adversely affects.
Liquid phase wet chemical method is equally applicable to metal-oxide and fills the preparation of carbon nano-fiber, but goes back at present
There is no document and patented technology report.
Summary of the invention
Deficiency present in preparation method and application for above metal oxide filled carbon nanotube, this
One of bright purpose is to provide the carbon nano-fiber that a kind of metal oxide nanoparticles is filled.
The two of the purpose of the present invention are to provide the system of the carbon nano-fiber that above-mentioned metal oxide nanoparticles is filled
Preparation Method.
The present invention, with carbon nano-fiber and soluble metallic salt as primary raw material, is to traditional liquid phase wet-chemical
The improvement that method is carried out.
In first aspect, the technical solution used in the present invention is:
The carbon nano-fiber that metal oxide nanoparticles is filled, is under pulverizing effect, by metal salt solution
It is filled in the pipe of carbon nano-fiber, calcines after drying and prepare；
Described metal is Fe, Co, Ni, Cu, Zn or Sn；
Described metal salt solution is nitrate or the aqueous chloride solution of above-mentioned metal, selects therein at least one
Kind；Or at least one of the ethanol solution of the acetylacetonate that described metal salt solution is above-mentioned metal；
The particle size range of described metal oxide nanoparticles is 5～30nm.
In technique scheme, carbon nano-fiber preferentially selects the folded cup-shaped using vapor growth method to prepare
Structure, its external diameter is 100nm～200nm, and internal diameter is 30nm～150nm.
Further, described carbon nano-fiber and the proportioning of metal salt solution, by carbon nano-fiber and slaine
The mass ratio that pyrolysis is the theoretical yield of oxide is that 1:0.2～2 calculates.
Pulverizing described above is wet grinding, the method that can use ball milling, rod milling and other routines, purport
By clashing into, shear, extrude, rubbing action, one is to make carbon nano-fiber rupture, it is provided that filling
Open channel, two is to promote solution moistening in pipe, improves filling rate, shortens the filling time.
The use of metal salt solution in such scheme, the situation including following:
The nitrate aqueous solution of different metal is used alone or mixed；
The aqueous chloride solution of different metal is used alone or mixed；
The nitrate aqueous solution of metal is mixed with the aqueous chloride solution of metal, the metal in nitrate therein
Can be the same or different with the metal in chloride；
Different metal acetylacetonate ethanol solution is used alone or mixed.
In yet another aspect, the preparation side of the carbon nano-fiber that the metal oxide nanoparticles of the present invention is filled
Method, comprises the steps:
(1) carry out carbon nano-fiber and metal salt solution mixing pulverizing, filter, be dried removing solvent, powder
Breakdown mill obtains the carbon nano-fiber that slaine is filled；
(2) carbon nano-fiber that the slaine obtained in step (1) is filled is 250 DEG C-800 DEG C calcinings
15min-2h, obtains target product；
Described metal is Fe, Co, Ni, Cu, Zn or Sn；
Described metal salt solution is nitrate or the aqueous chloride solution of above-mentioned metal, selects therein at least one
Kind；Or described metal salt solution selects at least one of the ethanol solution of the acetylacetonate of above-mentioned metal；
Described carbon nano-fiber and the proportioning of metal salt solution, be oxygen by carbon nano-fiber and slaine pyrolysis
The mass ratio of the theoretical yield of compound is that 1:0.2～2 calculates.
Further, mixing pulverizing selects ball milling.
Further, drum's speed of rotation is 200rpm-800rpm, and Ball-milling Time is 0.5～4h.
Further, described ball mill is the one in stirring-type, planetary or vibration type.
Specifically, the atmosphere calcined in step (2) is at least one in air, nitrogen or argon.
Metal oxide nanoparticles that the present invention prepares fills carbon nano-fiber, refer to Fe, Co, Ni,
The oxide of the metals such as Cu, Zn, Sn is filled in the nano composite material in carbon nano-fiber pipe.This preparation side
The ultimate principle of method is: under the effect of mixing pulverizing, the soluble salt solutions of above-mentioned metal is in carbon Nanowire
Dimension pipe there occurs effectively filling, then the carbon nano-fiber being filled with metal salt solution is existed after drying
Calcining under the high temperature of 250～800 DEG C, slaine thermally decomposes, and generates the metal-oxide of correspondence.The party
Method falls within liquid phase wet chemical method, is to introduce mixer mill powder craft with art methods difference.
In the filling process, by clashing into, shear, extruding, rubbing action, mixing pulverizing achieves two purposes,
One is to make carbon nano-fiber rupture, it is provided that filling open channel, two is to promote solution moistening in pipe,
Improve filling rate, shorten the filling time significantly.
The beneficial effects of the present invention is:
(1) avoid use strong acid oxidation processes carbon nano-fiber, the surface texture of carbon nano-fiber is destroyed
More weak, also make technique more environmental protection.
(2) filling process significantly shortens, and improves preparation efficiency, and is obtained in that higher filling rate.
(3) compared with the metal oxide nanoparticles filling carbon nano-pipe that prior art provides, burning
Thing nano-particles filled carbon nano-fiber internal diameter is big, using the teaching of the invention it is possible to provide more free space, beneficially mass transfer and
Play the functional characteristic of metal oxide nanoparticles, be easily dispersed simultaneously, use technique simply, comprehensively become
This is low.
The metal-oxide that the method that the present invention provides prepares fills carbon nano-fiber, in catalysis, sensing
The fields such as device, electromagnetic shielding material, new energy materials, biotechnology and high-performance composite materials have good
Good application prospect.
Accompanying drawing explanation
Fig. 1 is that the transmission filling ferriferrous oxide nano-particle carbon nano-fiber prepared by embodiment 1 is micro-
Mirror photo.
Fig. 2 is that the scanning of the filling ferric oxide nanoparticles carbon nano-fiber prepared by embodiment 2 is micro-
Mirror photo.
Fig. 3 is that the transmission microscopy filling NiO nanoparticle carbon nano-fiber prepared by embodiment 3 shines
Sheet.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment 1
(1) at room temperature by 1g carbon nano-fiber (trade mark PR-19-XT-PS, PPI company of the U.S.) and
The aqueous solution (theoretical decomposition ferroso-ferric oxide amount is 1g) of 30ml ferric nitrate loads planetary high-energy ball mill and fits
In the ball grinder joined, the ball-milling technology carrying out 30min under 400rpm rotating speed processes, and removes through filtering, being dried
Go moisture, attrition grinding to obtain ferric nitrate and fill carbon nano-fiber；
(2) ferric nitrate obtained in step (1) filling carbon nano-fiber is forged in 500 DEG C in a nitrogen atmosphere
Burn 30min, obtain target product: ferriferrous oxide nano-particle fills carbon nano-fiber.
The transmission microscopy photo display carbon nano-fiber pipe of Fig. 1 has splitting traces, port open, connects in pipe
Being filled with ferriferrous oxide nano-particle, particle diameter, at about 10nm, has higher filling rate continuously, at pipe
Obvious free space is had around interior nanoparticle.
Embodiment 2
(1) at room temperature by 1g carbon nano-fiber (trade mark PR-19-XT-PS, PPI company of the U.S.) and
The aqueous solution (theoretical decomposition iron sesquioxide amount is 0.5g) of 30ml ferric nitrate loads planetary high-energy ball mill
In adaptive ball grinder, the ball-milling technology carrying out 2h under 200rpm rotating speed processes, and removes through filtering, being dried
Go moisture, attrition grinding to obtain ferric nitrate and fill carbon nano-fiber；
(2) ferric nitrate obtained in step (1) filling carbon nano-fiber is forged in 250 DEG C in a nitrogen atmosphere
Burn 1h, calcine 1h in 350 DEG C the most in air atmosphere, obtain target product: iron sesquioxide nanoparticle
Son fills carbon nano-fiber.
The transmission microscopy photo display carbon nano-fiber tube-surface of Fig. 2 is etched with pore structure, and (lower right corner is amplified
Figure arrow locations), it is filled with ferric oxide nanoparticles in pipe.
Embodiment 3
(1) at room temperature by 1g carbon nano-fiber (trade mark PR-19-XT-PS, PPI company of the U.S.) and
The aqueous solution (theoretical decomposition amount of nickel oxide is 1g) of 30ml nickel nitrate loads the ball grinder that high energy vibration machine is adaptive
In, the ball-milling technology carrying out 1h processes, and through filtering, be dried removing moisture, attrition grinding obtains nickel nitrate and fills out
Fill carbon nano-fiber；
(2) ferric nitrate obtained in step (1) filling carbon nano-fiber is forged in 450 DEG C in a nitrogen atmosphere
Burn 30min, obtain target product: NiO nanoparticle fills carbon nano-fiber.
The transmission microscopy photo display carbon nano-fiber pipe of Fig. 3 has splitting traces, port open, connects in pipe
It is filled with NiO nanoparticle continuously, there is higher filling rate, have substantially around nanoparticle in pipe
Free space.
Embodiment 4
(1) at room temperature by 1g carbon nano-fiber (trade mark PR-19-XT-PS, PPI company of the U.S.) and
The ethanol solution (theoretical decomposition iron sesquioxide amount is 0.5g) of 30ml ferric acetyl acetonade loads planetary high energy
In the ball grinder that ball mill is adaptive, the ball-milling technology carrying out 1h under 300rpm rotating speed processes, through filtering,
Be dried and remove ethanol, attrition grinding obtains ferric acetyl acetonade and fills carbon nano-fiber；
(2) ferric acetyl acetonade obtained in step (1) is filled carbon nano-fiber in a nitrogen atmosphere in 250
DEG C calcining 1h, obtains target product: ferric oxide nanoparticles fills carbon nano-fiber.
Embodiment 5
(1) at room temperature by 1g carbon nano-fiber (trade mark PR-19-XT-PS, PPI company of the U.S.) and
The aqueous solution (theoretical decomposition amount of nickel oxide is 1g) of 30ml cobalt nitrate loads the ball that high-energy ball milling machine is adaptive
In grinding jar, the ball-milling technology carrying out 1h processes, and through filtering, be dried removing moisture, attrition grinding obtains nitric acid
Cobalt fills carbon nano-fiber；
(2) ferric nitrate obtained in step (1) filling carbon nano-fiber is forged in 600 DEG C under an argon atmosphere
Burn 30min, obtain target product: cobalt black nano-particles filled carbon nano-fiber.
Embodiment 6
(1) at room temperature by 1g carbon nano-fiber (trade mark PR-19-XT-PS, PPI company of the U.S.) and
It is adaptive that the aqueous solution (theoretical decomposition Red copper oxide amount is 2g) of 30ml copper nitrate loads high-speed stirred formula ball mill
Ball grinder in, the ball-milling technology carrying out 1h processes, and removes moisture, attrition grinding obtain through filtering, being dried
Copper nitrate fills carbon nano-fiber；
(2) ferric nitrate obtained in step (1) filling carbon nano-fiber is forged in 800 DEG C under an argon atmosphere
Burn 15min, obtain target product: the particle-filled carbon nano-fiber of cuprous nano.
Embodiment 7
(1) at room temperature by 1g carbon nano-fiber (trade mark PR-19-XT-PS, PPI company of the U.S.) and
It is adaptive that the aqueous solution (theoretical decomposition zinc oxide amount is 0.2g) of 30ml zinc nitrate loads high-speed stirred formula ball mill
Ball grinder in, the ball-milling technology carrying out 1h processes, and removes moisture, attrition grinding obtain through filtering, being dried
Zinc nitrate fills carbon nano-fiber；
(2) zinc nitrate obtained in step (1) filling carbon nano-fiber is forged in 450 DEG C under an argon atmosphere
Burn 30min, obtain target product: zinc oxide nano-particle fills carbon nano-fiber.
Embodiment 8
(1) at room temperature by 1g carbon nano-fiber (trade mark PR-19-XT-PS, PPI company of the U.S.) and
The aqueous solution (theoretical decomposition tin ash amount is 0.5g) of 30ml stannous chloride loads high-energy planetary ball mill machine and fits
In the ball grinder joined, the ball-milling technology carrying out 1h under the conditions of 800rpm processes, and removes through filtering, being dried
Moisture, attrition grinding obtain stannous chloride and fill carbon nano-fiber；
(2) stannous chloride obtained in step (1) is filled carbon nano-fiber in air atmosphere in 350
DEG C calcining 30min, obtains target product: tin dioxide nano-particle fills carbon nano-fiber.
Claims (8)
1. the carbon nano-fiber that metal oxide nanoparticles is filled, is under pulverizing effect, and slaine is molten
Liquid is filled in the pipe of carbon nano-fiber, calcines after drying and prepares；
Described metal is Fe, Co, Ni, Cu, Zn or Sn；
Described metal salt solution is nitrate or the aqueous chloride solution of above-mentioned metal, selects therein at least one
Kind；Or at least one of the ethanol solution of the acetylacetonate that described metal salt solution is above-mentioned metal；
The particle size range of described metal oxide nanoparticles is 5～30nm.
The carbon nano-fiber that metal oxide nanoparticles the most according to claim 1 is filled, its feature
It is: carbon nano-fiber selects the folded cup-like structure using vapor growth method to prepare.
The carbon nano-fiber that metal oxide nanoparticles the most according to claim 1 is filled, its feature
It is: described carbon nano-fiber and the proportioning of metal salt solution to be oxygen by carbon nano-fiber and slaine pyrolysis
The mass ratio of the theoretical yield of compound is that 1:0.2～2 calculates.
4. the preparation method of the carbon nano-fiber that metal oxide nanoparticles is filled, comprises the steps:
(1) carry out carbon nano-fiber and metal salt solution mixing pulverizing, filter, be dried removing solvent, powder
Breakdown mill obtains the carbon nano-fiber that slaine is filled；
(2) carbon nano-fiber that the slaine obtained in step (1) is filled is 250 DEG C-800 DEG C calcinings
15min-2h, obtains target product；
Described metal is Fe, Co, Ni, Cu, Zn or Sn；
Described metal salt solution is nitrate or the aqueous chloride solution of above-mentioned metal, selects therein at least one
Kind；Or described metal salt solution selects at least one of the ethanol solution of the acetylacetonate of above-mentioned metal；
Described carbon nano-fiber and the proportioning of metal salt solution, be oxygen by carbon nano-fiber and slaine pyrolysis
The mass ratio of the theoretical yield of compound is that 1:0.2～2 calculates.
Preparation method the most according to claim 4, is characterized in that: mixing pulverizing selects ball milling.
Preparation method the most according to claim 5, is characterized in that: drum's speed of rotation is
200rpm-800rpm, Ball-milling Time is 0.5～4h.
7. according to the preparation method described in claim 5 or 6, it is characterized in that: described ball mill is stirring
One in formula, planetary or vibration type.
Preparation method the most according to claim 4, is characterized in that: the atmosphere calcined in step (2)
For at least one in air, nitrogen or argon.
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| CN111470492A (en) * | 2019-11-21 | 2020-07-31 | 中山大学 | Preparation method of one-dimensional carbon chain |
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