CN107520464A - A kind of method for preparing iron nano-particle/major diameter carbon nano tube compound material - Google Patents
A kind of method for preparing iron nano-particle/major diameter carbon nano tube compound material Download PDFInfo
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- CN107520464A CN107520464A CN201710778856.5A CN201710778856A CN107520464A CN 107520464 A CN107520464 A CN 107520464A CN 201710778856 A CN201710778856 A CN 201710778856A CN 107520464 A CN107520464 A CN 107520464A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/34—Length
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/36—Diameter
Abstract
The present invention relates to a kind of method for preparing iron nano-particle/major diameter carbon nano tube compound material, and ferrocene is added in stainless steel autoclave, and is filled with 2~5atm nitrogen, and is heated to 480~720oC, react 68 hours, product ethanol and water washing, centrifuge and dry, that is, obtain iron nano-particle/major diameter CNT Fe NP/LD CNTs composites.The advantage of the invention is that：The present invention uses inert gas auxiliary catalysis decomposition technique; in closed system; under the protection and regulation and control of nitrogen; ferrocene magnanimity is converted into Fe NP/LD CNTs composites; reaction temperature is low compared with prior art; course of reaction is simple and easy to control, and products therefrom has that magnetic, pattern be good, pollution-free, yield is more than 95%；And the Fe NP/LD CNTs composites obtained by the inventive method, length of carbon nanotube is about tens microns, and diameter is about 400 nanometers, and the size of iron nano-particle is about 250 nanometers.
Description
Technical field
The present invention relates to a kind of method for preparing iron nano-particle/major diameter carbon nano tube compound material, more particularly to one
The method that Fe-NP/LD-CNTs composites are prepared by nitrogen assisted cryogenic magnanimity in kind autoclave.
Background technology
One of representative as nano material, CNT possess excellent mechanics, electricity because of its unique one-dimentional structure
, calorifics, optics and reactivity worth, make it in energy storage and conversion, composite, heterogeneous catalysis, environmental protection and biology
Medicine and other fields have substantial amounts of application potential (ACS Cent. Sci., 2016, 2: 162-168；ACS Appl. Mater. Interfaces, 2016, 8：6004-6010；ACS Catal., 2012, 2：223-229；ACS Appl. Mater. Interfaces, 2014, 6：8859-8867.).Although the appearance of graphene has shunted grinding for many CNTs
Study carefully attention rate, but CNT is still to study the most abundant, attention rate highest novel nano-material at present, what it was paid close attention to
Focus is also gradually from controllable preparation, structural characterization are transitioned into functionalization, performance plays and application study.
The various applications based on CNT are realized, first have to realize that structure and the controllable CNT batch of performance are made
It is standby.In past 20 years, the controllable preparation carbon such as arc discharge method, laser evaporization method and chemical vapour deposition technique is developed
Nanotube [J. Mater. Chem., 2011, 21: 15872-15884, J. Phys. Chem. B, 2006, 110:
7316-7320; Nanoscale, 2013, 5: 6662-6676.].1991, what Iijima etc. obtained in arc discharge method
Observed in carbon ash multi-walled carbon nanotube [Nature, 1991,354: 56-58.].Ebbesen and Ajayan is using improvement
Arc discharge method obtain gram quantity level scale multi-walled carbon nanotube [Nature, 1992, 358: 220-222.].Electricity
Arc method has the characteristics of fast growing, technological parameter is relatively easy to control, and obtained CNT Guan Zhi, crystallinity are high.However,
Arc process growth temperature is relatively high, and preparation facilities is relative complex, and arc discharge process is difficult to control, the production of the CNT of preparation
Rate is low, and it is high to prepare cost, its industrialized production also need further exploration [J. Mater. Chem., 2011, 21, 15872-
15884.].Laser evaporization method is the graphite target that will adulterate the transition metal such as Fe, Co, Ni, in 1200 DEG C of reaction temperature
Under, method that CNT is prepared with laser bombardment target material surface under inert gas (He) protection.The advantages of the method is system
Standby carbon nano pipe purity is high, is easy to continuous production, but high energy consumption, experimental facilities are complicated, it is high to prepare cost, are not suitable for extensive
Production [Carbon, 2012, 50: 4450-4458.].Chemical vapour deposition technique (CVD), typically at a certain temperature,
Carbonaceous gas or liquid carbon source are cracked in the presence of catalyst so as to generate CNT, so method is also known as catalytic pyrolysis
Method, there is the advantages that equipment is simple, and cost is low, and yield is big, shortcoming is that degree of graphitization is not high, impurity is more, low yield.Catalyst
Generally transition metal (such as Fe, Co, Ni, Pd), carbon source can be the carbonaceous gas such as methane, CO, ethene or
The liquid such as benzene, toluene [Mater. Sci. Semicon. Proc., 2016, 41: 67-82.]。
At present, it is more to the preparation research of CNT, but many problems are still suffered from its preparation method and preparation technology
Have to be solved.First, how to produce in enormous quantities on the basis of cost is reduced and to meet the different size carbon that each field requires and receive
The problem of mitron is still limitation CNT commercialization；Secondly, the carbon nano tube growth mechanism that some preparation methods obtain is also not
Clearly, influence CNT Yield and quality and yield factor it is also unclear；The CNT that now prepared by various methods is all
The shortcomings of high impurity, low yield be present.These are all the key factors for restricting CNT research and application.Due to technically and
Economically the reason for, CNT, which leaves practical application, still suitable distance.But once its technology of preparing makes a breakthrough, must
The development of whole nanometer technology will be driven, while will also drive the rise and development of a series of related high-tech industries, is triggered
One New Sci-and Tech-Revolution, huge interests are brought to entire society.If preparing CNT with wanting to continuous batch, need
Consider how to realize the problem of transmission of catalytic process in large scale industry reactor, reactor heat and reactant.Carbon nanometer
The forming process of pipe is the departure process by a self assembly from bottom to top, but batch preparation is one and contains macroscopic flow
Dynamic, reaction, heat conveying, the continuous process of mass transfer.
Therefore, a kind of heat and the excellent simple economy reaction system of mass transport are found, preparing high quality carbon to magnanimity receives
Mitron has especially important meaning with its application aspect is expanded.
The content of the invention
The technical problem to be solved in the present invention is to provide one kind, nitrogen aids in Autocatalytic decomposition ferrocene in enclosed system
Method magnanimity prepare iron nano-particle/major diameter CNT Fe-NP/LD-CNTs composites, it is grand to solve prior art
Amount prepares the problem for the treatment of temperature existing for CNT is high, product uniformity is poor, low yield, more influence factor.
In order to solve the above technical problems, the technical scheme is that：One kind prepares iron nano-particle/major diameter carbon nanometer
The method of pipe composite, its innovative point are：Ferrocene is added in stainless steel autoclave, and is filled with 2~5atm nitrogen,
And it is heated to 480~720oC, 6-8 hours, product ethanol and water washing are reacted, centrifuge and dry, that is, obtained iron and receive
Rice grain/major diameter CNT Fe-NP/LD-CNTs composites.
Further, the addition of the ferrocene is that 150~300g is added in every liter of stainless steel autoclave.
Preferably, the addition of the ferrocene is that 200~250g, enclosed system are added in every liter of stainless steel autoclave
Middle 2~5atm of pressure because within the range, ferrocene into efficiency of carbon con version be more than 85%, wherein Fe-NP/LD-CNTs
The production rate of composite is more than 75%.
It is further preferred that the addition of the ferrocene is that 200~250 g, enclosed system are added in every liter of stainless steel autoclave
Middle 2.5~3.5atm of pressure because within the range, ferrocene into efficiency of carbon con version be more than 90%, wherein Fe-NP/LD-
The production rate of CNTs composites is more than 85%；Reaction principle is as follows：
The advantage of the invention is that：The present invention uses inert gas auxiliary catalysis decomposition technique, in closed system, in nitrogen
Protection and regulation and control under, ferrocene magnanimity is converted into Fe-NP/LD-CNTs composites, reaction temperature is compared with prior art
Low, course of reaction is simple and easy to control, and products therefrom has that magnetic, pattern be good, pollution-free, yield is more than 95%；And pass through the present invention
The Fe-NP/LD-CNTs composites that method obtains, length of carbon nanotube is about tens microns, and diameter is about 400 nanometers, and iron is received
The size of rice grain is about 250 nanometers.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the XRD spectra of the Fe-NP/LD-CNTs composites of embodiment 1.
Fig. 2 is the Raman spectrogram of the Fe-NP/LD-CNTs composites of embodiment 1.
Fig. 3 is the low power FESEM photos of the Fe-NP/LD-CNTs composites of embodiment 1.
Fig. 4 is the high power FESEM photos of the Fe-NP/LD-CNTs composites of embodiment 1.
Fig. 5 is the TEM photos of Fe-NP/LD-CNTs composites prepared by embodiment 1.
Fig. 6 is the TEM photos of single Fe-NP/LD-CNTs composites prepared by embodiment 1.Fig. 7 is prepared by embodiment 1
CNT HRTEM photos.
Fig. 8 is the EDX spectrograms of Fe-NP/LD-CNTs composites prepared by embodiment 1.
Fig. 9 is the STEM photos of Fe-NP/LD-CNTs composites prepared by embodiment 1.
Figure 10 is the C dispersion spectrums of Fe-NP/LD-CNTs composites prepared by embodiment 1.
Figure 11 is the Fe dispersion spectrums of Fe-NP/LD-CNTs composites prepared by embodiment 1.
Figure 12 is the hysteresis curve of the Fe-NP/LD-CNTs composites of embodiment 1.
Embodiment
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among described scope of embodiments.
Embodiment 1：
225 grams of ferrocene (Shanghai Chemical Reagent Co., Ltd., Sinopharm Group) are added in one 1 liter of stainless steel autoclave,
Nitrogen is passed through again, and after driveing the air in kettle, it is 3.0 atm to make pressure in kettle, and the electric furnace for being capable of temperature programming is put into after sealing
In, it is raised to 600 from room temperature in furnace temperature 120 minutesoC, 600oAfter 6 h are maintained under C, room temperature is naturally cooled to.In autoclave
Final product includes the deposit of black and the gas of residual.The black deposit being bonded on kettle wall inner surface is collected
About 200 grams of the sample repeatedly, obtained after filtering is washed with absolute ethyl alcohol, sample is respectively in 60 in vacuum drying chamberoC dries 6
Hour, finally collect for characterizing.
Using Japanese Rigaku D/max-γA types X-ray powder diffraction (XRD) instrument carries out material phase analysis, Cu to powderKα(λ=1.54178), graphite monochromator, pipe pressure and electric current are respectively 40 kV and 20 mA, sweep speed 10.0o·min-1。
Fig. 1 is the XRD spectra of product prepared by embodiment 1.As seen from Figure 1, in XRD spectra 2 θ in 10-80oHave 2 compared with
Strong diffraction maximum, wherein about 26oThe diffraction maximum of neighbouring low intensity and widthization can be demarcated as (002) of the graphite of hexagonal phase
Diffraction maximum (JCPDS card No. 41-1487), 45.2oWith 64.7oNeighbouring diffraction maximum can be demarcated as body-centered cubic phase
The diffraction maximum (JCPDS card No.06-0696) of (110) and (200) of iron, the miscellaneous peak of other also some low intensities are probably
The activity of the diffraction maximum of ferriferous oxide, mainly nano iron particles is very high, meets air and easily aoxidizes.
Raman spectrum is handled by the type Raman spectrometers of Spex 1403, uses the argon laser that wavelength is 514.5 nanometers
Device, powder is further confirmed that.Fig. 2 is the Raman spectrogram of product.It is observed that two apparent Ramans in figure
Peak, respectively positioned at 1594 cm-1With 1343 cm-1, corresponding to the Characteristic Raman peak of graphitized carbon nano structure.Positioned at 1594 cm-1Peak (G bands) correspond to two-dimentional graphite linings in E2gVibration mode, the sp in this peak and two-dimentional hexagonal mesh2Hydridization
Carbon atom vibration is relevant；Positioned at 1343 cm-1Peak (D bands) and two dimensional surface edge there is the vibration of the random carbon atom of dangling bond
It is relevant；Strong D bands peak shows, the crystal face existing defects of CNT.
Use field emission scanning electron microscope (FESEM, JEOL JSM-6300F), transmission electron microscope (Tecnai G2
F30 S-TWIN, accelerating potential are 200 kV) and EDXA energy disperse spectroscopies characterize the pattern of product, particle size and element composition etc..
From the FESEM of Fig. 3 products, the yield of the Fe-NP/LD-CNTs composites obtained using the inventive method
Height, and pattern is uniform；Fig. 4 is the FESEM photos of amplification, the results showed that, the CNT in Fe-NP/LD-CNTs composites
Up to tens microns, diameter dimension is uniform, about 350 nanometers；Fig. 5 is the TEM photos of Fe-NP/LD-CNTs composites, knot
Fruit shows that product is a large amount of CNTs, and its carbon nanotube diameter is about 345 nm, and carbon nano tube surface adheres to some iron nanometers
Particle.Fig. 6 shows that the single Fe-NP/LD-CNTs composites are formed in the growth of Fe nano grain surfaces.Fig. 7 is carbon nanometer
The HRTEM photos of tube wall, clearly graphite flake layer should be apparent that by figure, its interlamellar spacing is about 0.34 nm.Fig. 8 is
The EDX spectrograms of Fe-NP/LD-CNTs composites, the results showed that, product includes two kinds of elements of carbon and iron, further demonstrates,
Product is the composite of iron and carbon.Fig. 9 is the STEM photos of product, the results showed that, internal diameter and the external diameter difference of CNT
About 135nm and 340 nm, the diameter of catalyst iron nano-particle is about 275 nm.Figure 10 and 11 is Fe-NP/LD- respectively
CNTs C and Fe element mapping spectrogram.
By superconducting quantum interference device (SQUID) (SQUID) (MPMS 5, Quantum Design) to Fe-NP/LD-CNTs composite woods
The magnetic property of material is measured, and measurement temperature is 298 K, and intensity is 10000 Oe.
Under room temperature condition, in the range of being -10000 Oe to 10000 Oe in magnetic field, it is compound to investigate Fe-NP/LD-CNTs
The magnetic property of material, as a result as shown in figure 12.Hysteresis curve shows that Fe-NP/LD-CNTs composites have ferromagnetic property,
Its saturated magnetization rate and coercivity are respectively 75.7 emu/g and 190.6 Oe.From characterization result as can be seen that with block iron
Saturated magnetization rate and coercivity (220 emu g-1, 0.9 Oe) compare, the saturated magnetization of Fe-NP/LD-CNTs composites
Rate is less than the saturated magnetization rate of block iron, is primarily due to the presence of CNT;In addition, this Fe-NP/LD-CNTs
The coercivity of composite is bigger than the coercivity of block iron, mainly due to caused by different size and pattern.
Analysis confirms above, aids in Autocatalytic decomposition ferrocene to obtain consistent appearance, chi with magnanimity by inert gas
Iron/carbon nano tube compound material that very little uniform and yield is about 94%.
Embodiment 2：
Difference from Example 1 is, 150 grams of ferrocene is added in 1 L stainless steel autoclave, then be passed through nitrogen
Gas, it is 3.0 atm to make pressure in kettle, and the yield of products therefrom is 85%, but the yield of Fe-NP/LD-CNTs composites is about
For 70%, basic parameter：The Average Particle Diameters of iron particle are about 122 nm, the length of CNT is about tens microns, carbon
The diameter of nanotube is about 320 nm.
Embodiment 3：
Difference from Example 1 is, 300 grams of ferrocene is added in 1 L stainless steel autoclave, then be passed through nitrogen
Gas, it is 3.0 atm to make pressure in kettle, and products therefrom yield is about 95%, but the yield of Fe-NP/LD-CNTs composites is about
For 80%, basic parameter：The Average Particle Diameters of iron particle are about 286 nm, the length of CNT is about tens microns, carbon
The diameter of nanotube is about 380 nm.
Embodiment 4：
Difference from Example 1 is, 225 grams of ferrocene is added in 1 L stainless steel autoclave, then be passed through nitrogen
Gas, it is 2 atm to make pressure in kettle, and gained composite yield is 85%, but the yield of Fe-NP/LD-CNTs composites is about
For 75%, basic parameter：The Average Particle Diameters of iron particle are about 262 nm, the length of CNT is about tens microns, carbon
The diameter of nanotube is about 325 nm.
Embodiment 5：
Difference from Example 1 is, 225 grams of ferrocene is added in 1 L stainless steel autoclave, then be passed through nitrogen
Gas, it is 5 atm to make pressure in kettle, and the yield of products therefrom is 88%, but Fe-NP/LD-CNTs yield is about 79%, substantially
Parameter：The Average Particle Diameters of iron particle are about 283 nm, the length of CNT is about tens microns, CNT it is straight
Footpath is about 400 nm.
Embodiment 6：
Difference from Example 1 is, 225 grams of ferrocene is added in 1 L stainless steel autoclave, then be passed through nitrogen
Gas, it is 2.5 atm to make pressure in kettle, and the yield of products therefrom is 92%, but Fe-NP/LD-CNTs yield is about 84%, base
This parameter：The Average Particle Diameters of iron particle are about 265 nm, the length of CNT is about tens microns, CNT
Diameter is about 325nm.
Embodiment 7：
Difference from Example 1 is, 225 grams of ferrocene is added in 1 L stainless steel autoclave, then be passed through nitrogen
Gas, pressure is set in kettle to be 3.0 atm, reaction temperature 580oC, gained composite yield is 95%, but Fe-NP/LD-
The yield of CNTs composites is about 89%, basic parameter：The Average Particle Diameters of iron particle are about 265nm, the length of CNT
About tens microns of degree, the diameter of CNT is about 335 nm.
Embodiment 8：
Difference from Example 1 is, 225 grams of ferrocene is added in 1 L stainless steel autoclave, then be passed through nitrogen
Gas, pressure is set in kettle to be 3.0 atm, reaction temperature 620oC, gained composite yield is 95%, but Fe-NP/LD-
The yield of CNTs composites is about 90%, basic parameter：The Average Particle Diameters of iron particle are about 275 nm, CNT
Length is about tens microns, and the diameter of CNT is about 355nm.
Embodiment 9：
Difference from Example 1 is, 225 grams of ferrocene is added in 1 L stainless steel autoclave, then be passed through nitrogen
Gas, pressure is set in kettle to be 3.0 atm, reaction temperature 600oC, 4 hours reaction time, gained composite yield are 85%,
But the yield of Fe-NP/LD-CNTs composites is about 85%, basic parameter：The Average Particle Diameters of iron particle are about 275
Nm, the length of CNT are about tens microns, and the diameter of most of CNT is about 340 nm, also have some diameters compared with
Small CNT.
Implement 10：
Difference from Example 1 is, 225 grams of ferrocene is added in 1 L stainless steel autoclave, then be passed through nitrogen
Gas, pressure is set in kettle to be 3.0 atm, reaction temperature 600oC, in 8 hours reaction time, the yield of products therefrom is 95%, but
The yield for being Fe-NP/LD-CNTs composites is about 90%, basic parameter：The Average Particle Diameters of iron particle be about 270 nm,
The length of CNT is about tens microns, and the diameter of most of CNT is about 340 nm.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The skill of the industry
For art personnel it should be appreciated that the present invention is not limited to the above embodiments, described in above-described embodiment and specification is explanation
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (4)
- A kind of 1. method for preparing iron nano-particle/major diameter carbon nano tube compound material, it is characterised in that：Ferrocene is added In stainless steel autoclave, and 2~5atm nitrogen is filled with, and is heated to 480~720oC, react 6-8 hours, product ethanol And water washing, centrifuge and dry, that is, obtain iron nano-particle/major diameter CNT Fe-NP/LD-CNTs composites.
- 2. the method according to claim 1 for preparing iron nano-particle/major diameter carbon nano tube compound material, its feature exist In：The addition of the ferrocene is that 150~300g is added in every liter of stainless steel autoclave.
- 3. the method according to claim 2 for preparing iron nano-particle/major diameter carbon nano tube compound material, its feature exist In：The addition of the ferrocene is that 200~250g is added in every liter of stainless steel autoclave.
- 4. the method according to claim 3 for preparing iron nano-particle/major diameter carbon nano tube compound material, its feature exist In：2.5~3.5atm nitrogen is filled with into stainless steel autoclave.
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Citations (5)
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|---|---|---|---|---|
| CN1507972A (en) * | 2002-12-18 | 2004-06-30 | 北京化工大学 | Method for preparing carbon-coated metal nano crystal |
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| CN101837287A (en) * | 2009-03-21 | 2010-09-22 | 清华大学 | Carbon nano-tube nano-particle composite material and preparation hereof |
| CN102303126A (en) * | 2011-06-20 | 2012-01-04 | 浙江师范大学 | Method for manufacturing flower-shaped nickel-carbon nanotube composite material |
| CN103232031A (en) * | 2013-04-19 | 2013-08-07 | 江苏科技大学 | Method for treating waste polyolefin plastics |
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|---|---|---|---|---|
| CN1507972A (en) * | 2002-12-18 | 2004-06-30 | 北京化工大学 | Method for preparing carbon-coated metal nano crystal |
| CN100434210C (en) * | 2005-01-17 | 2008-11-19 | 武汉科技大学 | Carbon-clad metal nano particle and its preparing method |
| CN101837287A (en) * | 2009-03-21 | 2010-09-22 | 清华大学 | Carbon nano-tube nano-particle composite material and preparation hereof |
| CN102303126A (en) * | 2011-06-20 | 2012-01-04 | 浙江师范大学 | Method for manufacturing flower-shaped nickel-carbon nanotube composite material |
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