CN109179477A - A kind of preparation method for the ceria nanoparticles that size is controllable - Google Patents
A kind of preparation method for the ceria nanoparticles that size is controllable Download PDFInfo
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- CN109179477A CN109179477A CN201810898525.XA CN201810898525A CN109179477A CN 109179477 A CN109179477 A CN 109179477A CN 201810898525 A CN201810898525 A CN 201810898525A CN 109179477 A CN109179477 A CN 109179477A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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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Abstract
The present invention relates to a kind of preparation methods of ceria nanoparticles that size is controllable, comprising the following steps: S1 provides the alcoholic solution and carbon nanotube of the nitrate of cerium, wherein the carbon nanotube is to possess sp2The carbon material of structure；Carbon nanotube is immersed in the alcoholic solution of the nitrate of cerium by S2, so that the nitrate of cerium enters inside carbon nanotube；And S3, it is dry after filtering, so that the nitrate of cerium is decomposed to form the controllable ceria nanoparticles of size in carbon nanotube.Preparation method according to the present invention, solve it is in the prior art generally realized using strong oxidizers such as concentrated nitric acids carbon nanotube be open, with high annealing come brought by the compound of reducing metal the problem of high pollution highly energy-consuming, technology difficulty is not only greatly reduced, but also reduces energy consumption or even realizes 0 energy consumption.
Description
Technical field
The present invention relates to the preparations of nano material, relate more specifically to a kind of system of ceria nanoparticles that size is controllable
Preparation Method.
Background technique
Since the Ce element in cerium oxide can be quickly and easily in Ce4+And Ce3+Between mutually convert so that cerium oxide
With very outstanding catalytic activity (NPG Asia Materials 6, e90,2014), and then it is widely used in solid
Oxide fuel cell (Renew.Sust.Energ.Rev.6,433,2002), solar battery (Nat.Mater.3,394-
397,2004) engineering fields such as.Again because of the outstanding polishing performance of cerium oxide, it is also employed in accurate polishing material field
(Energy Environ.Sci.5,8475-8505,2012).Cerium oxide is especially extensive in catalytic field application, for example applies
In the catalytic production of organic reaction (Catal.Rev.38,439,1996).As catalyst, the size of cerium oxide particle is smaller,
Effect is better.But simultaneously in catalytic process, particle size can gradually grow up, and influence catalytic effect, so needing stably catalyzed
Agent size (Science, 329,1633-1636,2012).Therefore, how to control the size of cerium oxide particle is catalytic field face
The critical issue faced.
Carbon nanotube inner space is to prepare the oxidation of the metals such as size controllable ceria nanoparticles in nanoscale
A kind of typical nano-form (Nature, 375,564-567,1995) of composition granule.But it is prepared currently with carbon nanotube
The technique of metal oxide nano particles is mainly in the aqueous solution of the Strong oxdiatives object such as concentrated nitric acid toward filling inside carbon nanotube
The compound of certain metal, then the high temperature anneal obtains the metal oxide nano particles including cerium oxide
(Journal of Materials Chemistry, 7,545-549,1997).
Obviously, the use of strong acid allows the high production cost of nano-cerium oxide, and pollutes environment.The high temperature anneal needs
The a large amount of energy is consumed, production cost is also further increased.These all constrain the industrialization of ceria nanoparticles significantly
Production (Nature Communications, 8,1445,2017).
Summary of the invention
The problems such as preparation cost in order to solve above-mentioned ceria nanoparticles of the existing technology is high and seriously polluted,
The present invention is intended to provide a kind of preparation method for the ceria nanoparticles that size is controllable.
The preparation method of the controllable ceria nanoparticles of size of the present invention, comprising the following steps: S1 provides cerium
Nitrate alcoholic solution and carbon nanotube, wherein the carbon nanotube be possess sp2The carbon material of structure；S2, by carbon nanotube
It is immersed in the alcoholic solution of the nitrate of cerium, so that the nitrate of cerium enters inside carbon nanotube；And S3, it is done after filtering
It is dry, so that the nitrate of cerium is decomposed to form the controllable ceria nanoparticles of size in carbon nanotube.
In the present invention, the nitrate of cerium is dissolved in alcohol, and carbon nanotube keeps opening in alcohol, does not need to use concentrated nitric acid
Equal Strong oxdiatives object carries out opening processing to carbon nanotube, and breaching in the prior art must carry out opening processing to carbon nanotube
Technology prejudice.Due to possessing sp2Carbon nanotube of structure itself constitutes a kind of excellent catalyst, therefore in normal temperature and pressure
Under, the present invention does not need any energy can be so that the nitrate of cerium be decomposed to form the controllable nanometer of size in carbon nanotube
Cerium oxide particle realizes the controllable ceria nanoparticles of 0 energy consumption ground preparation size, to breach in the prior art whereby
The technology prejudice to realize decomposition must be heat-treated.It is received in addition, the ion of the nitrate of cerium in the prior art enters carbon
It is typically all to be assisted by ultrasonic wave inside mitron, still, in fact, the step S2 of preparation method of the invention can not be related to
And ultrasonic wave etc. consumes the equipment of energy to assist to complete.
In the step S1, the alcoholic solution of the nitrate of cerium is the ethanol solution of the nitrate of cerium.Preferably, the cerium
The alcoholic solution of nitrate is molten for the alcohol of ammonium ceric nitrate and its hydrate, cerous nitrate and its hydrate, cerous nitrate and its hydrate
Liquid.It is highly preferred that the alcoholic solution of the nitrate of the cerium is ammonium ceric nitrate and its hydrate, cerous nitrate and its hydrate, nitric acid
The ethanol solution of cerium and its hydrate.In a preferred embodiment, the alcoholic solution of the nitrate of the cerium is Ce (NO3)3Ethyl alcohol
Solution.In another preferred embodiment, the alcoholic solution of the nitrate of the cerium is ammonium ceric nitrate ethanol solution.
In the step S1, the concentration of the alcoholic solution of the nitrate of cerium is not less than 0.0005mol/L.Preferably, cerium
The concentration of the alcoholic solution of nitrate is 0.0005-0.11mol/L.Experiment shows the concentration even if the alcoholic solution of the nitrate of cerium
Very dilute, down to 0.0005mol/L, cerium ion and nitrate ion can still be assembled in carbon nanotube.It should be understood that cerium
The concentration of the alcoholic solution of nitrate, which is higher than 0.11mol/L, may be equally applicable in the present invention.
In the step S1, carbon nanotube is single-walled carbon nanotube or multi-walled carbon nanotube.For example, the carbon nanotube is
Carbon nanotube without the opening processing of any functional group or the carbon nanotube by opening processing.For example, the carbon nanotube is carboxylic
Base carbon nano tube, carbonyl carbon nano tube, hydroxyl carbon nano tube or aminated carbon nano tube.For example, the carbon nanotube is
Open at one end or both ends open carbon nanotube.In one embodiment, which is functionalized multi-wall carbonnanotubes.It answers
The understanding, any carbon nanotube with " enrichment " may be suitable in the present invention to realize 0 energy consumption.
The internal diameter of the carbon nanotube is between 1nm-15nm.For example, the internal diameter is between 2.3nm-6.5nm.It should be understood that
The carbon nanotube in above-mentioned inside diameter ranges is not equally applicable in the present invention.
In the step S2, soaking time 15min-20h.For example, the time is 35min-45min.
In the step S2, the ion of the nitrate of cerium is promoted to enter inside carbon nanotube by ultrasonic wave auxiliary.
It should be understood that ultrasonic wave is not necessary condition.
In the step S3, it is filtered by filter paper or aluminium net.It is highly preferred that being filtered by qualitative filter paper.
In the step S3, it is spontaneously dried in air at room temperature.Preferably, it is dried by heating, to shorten
Drying time.Preferably, drying time 20min-20h.It should be understood that when properly increasing drying temperature and can shorten dry
Between.
Preparation method according to the present invention can realize system of the ceria nanoparticles inside carbon nanotube at normal temperature
Standby, the size of thus obtained ceria nanoparticles is mainly controlled by the inner diameter size of carbon nanotube, i.e., is closed by selecting
The carbon nanotube of suitable internal diameter accurately to control the full-size of the controllable ceria nanoparticles of ceria nanoparticles size.Always
It, preparation method according to the present invention solves in the prior art generally realizes carbon nanometer using strong oxidizers such as concentrated nitric acids
Tube opening the problem of high pollution highly energy-consuming, not only greatly reduces work brought by the compound of reducing metal with high annealing
Skill difficulty, and reduce energy consumption or even realize 0 energy consumption.
Detailed description of the invention
Fig. 1 is the TEM photo of the sample of first preferred embodiment according to the present invention；
Fig. 2 is the high angle annular dark field photo of the sample of first preferred embodiment according to the present invention；
Fig. 3 is the energy spectrum diagram in the circle of Fig. 1；
Fig. 4 is the Fourier transform infrared spectroscopy figure of the sample of first preferred embodiment according to the present invention；
Fig. 5 is the X-ray diffractogram of the sample of first preferred embodiment according to the present invention；
Fig. 6 is the TEM photo of sample according to the second, preferred embodiment of the present invention；
Fig. 7 is the TEM photo of the sample of third preferred embodiment according to the present invention；
Fig. 8 is the TEM photo of the sample of the 4th preferred embodiment according to the present invention；
Fig. 9 is the energy spectrum diagram in the circle of Fig. 8；
Figure 10 is the high-resolution photo of the nano particle filler of Fig. 8；
Figure 11 is the TEM photo of the sample of the 5th preferred embodiment according to the present invention；
Figure 12 is the EDAX results of nano particle in the sample of the 5th preferred embodiment according to the present invention.
Specific embodiment
With reference to the accompanying drawing, presently preferred embodiments of the present invention is provided, and is described in detail.
Embodiment 1
With the Ce (NO of 0.034mol/L3)3Functionalized multi-wall carbonnanotubes after alcohol solution dipping, at room temperature air
In environment after drying, the filling situation of its internal nano-cerium oxide is observed with TEM, with the infrared variation of Fourier to nano-cerium oxide
Main component be determined, with XRD test nano-cerium oxide lattice structure.
Processing stage: the functionalized multi-wall carbonnanotubes bought by Beijing Deco island King Company are immersed directly in
Ce (the NO of 0.034mol/L3)316h in ethanol solution, is then filtered out with qualitative filter paper, is done naturally in air at room temperature
It is dry, obtain the present embodiment sample.
Flied emission transmission electron microscope (Transmission Electron Microscope, TEM) test phase: it uses
TEM observes the grown form of the nano-cerium oxide in functionalized multi-wall carbonnanotubes, analyzes carboxylic with TEM Surface scan (mapping)
Ion (C, O and Ce) distribution situation inside and outside base multi-walled carbon nano-tube roughly determines whole elements of nano-cerium oxide with EDS
Composition and ratio.Fig. 1 is the TEM photo of the present embodiment sample, it can be seen that there is black at the intermediate position in carbon nanotube
Granular little particle, the diameter of these particles are less than the internal diameter of carbon nanotube.Fig. 2 is the high angle annular of the present embodiment sample
Dark field photo, it can be seen that the position in the middle part of carbon nanotube has diameter less than the bright granular substance of the internal diameter of carbon nanotube
Matter, wherein (b)-(d) is the mapping photo in the box of (a), it can be seen that the signal strength of Ce and O is all very strong, and
Its width and the internal diameter of carbon nanotube are suitable, and in position among carbon nanotube, this illustrates that these particles are to be filled in carbon nanometer
Inside pipe.Fig. 3 is power spectrum (EDS) figure in the circle of Fig. 1, it can be seen that the main component of these particles is Ce and two kinds of O
Element.
Fourier transform infrared spectroscopy test phase: the Ce (NO of 0.034mol/L is used with Infrared Reflective Spectra test3)3Second
Functionalized multi-wall carbonnanotubes, original functionalized multi-wall carbonnanotubes and 300 DEG C of heating Ce after alcoholic solution immersion
(NO3)3·6H2Product CeO after O 30min2The infrared spectrum spectrogram of (rare earth, 1988 (4): 33-37) three kinds of samples carries out pair
Than to analyze its ingredient.Fig. 4 gives Fourier transform infrared spectroscopy figure, wherein the curve of the top corresponds to the present embodiment
Sample, intermediate curve correspond to original functionalized multi-wall carbonnanotubes, and the curve of bottom corresponds to product CeO2.By
Figure is it is found that the present embodiment sample has original functionalized multi-wall carbonnanotubes and CeO simultaneously2Characteristic peak, i.e. the present embodiment
It include CeO in sample2。
X-ray diffraction (XRD) test phase: the Ce (NO of 0.034mol/L is used with XRD test3)3After alcohol solution dipping
Functionalized multi-wall carbonnanotubes and standard CeO2Two kinds of samples.Fig. 5 gives XRD spectrum, wherein (a) is full spectrum, and (b)-(c) is
(a) enlarged drawing of two shadow regions in left and right, wherein upper layer curve corresponds to the present embodiment sample, and bottom plot line corresponds to
Standard CeO2.As seen from the figure, peak of the present embodiment sample with cerium oxide (200), (220) and (420) three crystal faces, one
Ce2O3Unimodal, a Ce (NO3)3Unimodal, the peak of two carbon nanotubes.
The experimental results showed that with the Ce (NO of 0.034mol/L3)3Ethanol solution simply immersing functionalized multi-wall carbonnanotubes,
The controllable ceria nanoparticles of a large amount of size are formd inside carbon nanotube.
Embodiment 2
With the Ce (NO of 0.034mol/L3)3The functionalized multi-wall carbonnanotubes of ethanol solution simply immersing different inner diameters.
Processing stage: the functionalized multi-wall carbonnanotubes of 2.3nm, 2.5nm, 4nm, 5nm, 6.5nm internal diameter are direct
It is immersed in the Ce (NO of 0.034mol/L3)312h in ethanol solution, is then filtered out with qualitative filter paper, at room temperature in air
It spontaneously dries, obtains the present embodiment sample.
TEM test phase: with the distribution feelings of the ceria nanoparticles inside TEM observation functionalized multi-wall carbonnanotubes
Condition, and the lattice structure and crystalline substance of the functionalized multi-wall carbonnanotubes inside nano-cerium oxide with high-resolution observation different inner diameters size
Particle size.Fig. 6 is the TEM photo of the present embodiment sample, wherein the internal diameter of carbon nanotube is 2.3nm and 2.5nm in (a), (b)
The internal diameter of middle carbon nanotube be 4nm, (c) in carbon nanotube internal diameter be 5nm, (d) in carbon nanotube internal diameter be 6.5nm.It can
To see, the internal diameter of carbon nanotube where the diameter for the cerium oxide nanoparticles filled inside carbon nanotube is both less than it.
The experimental results showed that the size of the ceria nanoparticles formed inside carbon nanotube is because inside carbon nanotube
The limitation of space size cannot be greater than the internal diameter of carbon nanotube, i.e., be determined by the internal diameter size of carbon nanotube.Under high-resolution
The interplanar distance that can easily observe ceria nanoparticles is 0.31nm or so, this corresponds to CeO2(111) face.
Embodiment 3
With handled without any functional group single-walled carbon nanotube, multi-walled carbon nanotube, with carboxyl handle multi wall carbon receive
Mitron and the multi-walled carbon nanotube interrupted are separately immersed in Ce (NO3)3In ethanol solution.
Processing stage: without any functional group processing single-walled carbon nanotube, multi-walled carbon nanotube and with carboxyl handle
Multi-walled carbon nanotube is separately immersed in the Ce (NO of 0.034mol/L3)312h in ethanol solution, is then filtered out with qualitative filter paper
Come, is spontaneously dried in air at room temperature, obtain the present embodiment sample.
TEM test phase: with the distribution feelings of the ceria nanoparticles inside TEM observation functionalized multi-wall carbonnanotubes
Condition.Fig. 7 is the TEM photo of the present embodiment sample, wherein (a) corresponds to single-walled carbon nanotube, as seen from the figure, without any
Ceria nanoparticles, and the diameter of these ceria nanoparticles are filled in the single-walled carbon nanotube of functional group's opening processing
The internal diameter of carbon nanotube where being slightly less than；(b) correspond to multi-walled carbon nanotube, as seen from the figure, be open without any functional group
Ceria nanoparticles are filled in the multi-walled carbon nanotube of processing, and the diameter of these ceria nanoparticles is slightly less than place
The internal diameter of carbon nanotube；(c) correspond to the multi-walled carbon nanotube of carboxyl processing, as seen from the figure, the single wall carbon of carboxyl opening processing
Ceria nanoparticles are filled in nanotube, and the diameter of these ceria nanoparticles is slightly less than the interior of place carbon nanotube
Diameter；(d) correspond to the multi-walled carbon nanotube interrupted and be filled with nano-cerium oxide in the multi-walled carbon nanotube interrupted as seen from the figure
Particle, and the diameter of these ceria nanoparticles is slightly less than the internal diameter of place carbon nanotube.Therefore, no matter carbon nanotube whether
Opening processing by function dough, the single-walled carbon nanotube or internal diameter that also no matter carbon nanotube be internal diameter is about 1nm arrive greatly
The multi-walled carbon nanotube of 10nm, also no matter the length of carbon nanotube, a large amount of nano oxygen can be formed inside carbon nanotube
Change cerium particle.
The experimental results showed that can all be formed in the interior thereof a large amount of ruler whether no matter carbon nano tube surface has functional group
Very little controllable ceria nanoparticles.
Embodiment 4
It is empty at room temperature with the functionalized multi-wall carbonnanotubes after the ammonium ceric nitrate alcohol solution dipping of 0.0005mol/L
In compression ring border after drying, the filling situation of its internal nano-cerium oxide is observed with TEM, with the infrared variation of Fourier to nano oxidized
The main component of cerium is determined, and with the lattice structure of XRD test nano-cerium oxide, obtains the present embodiment sample.
Processing stage: the functionalized multi-wall carbonnanotubes bought by Beijing Deco island King Company are immersed directly in
16h in the ammonium ceric nitrate ethanol solution of 0.0005mol/L, is then filtered out with qualitative filter paper, natural in air at room temperature
It is dry.
TEM test phase: with the grown form of the nano-cerium oxide in TEM observation functionalized multi-wall carbonnanotubes, TEM is used
Surface scan (mapping) analyzes ion (C, O and Ce) distribution situation inside and outside functionalized multi-wall carbonnanotubes, roughly true with EDS
Determine the whole elements composition and ratio of nano-cerium oxide.Fig. 8 is the TEM photo of the present embodiment sample, as seen from the figure, internal diameter about
To form nano particle filler inside the carbon nanotube of 15nm.Fig. 9 is the EDS spectrogram in the circle of Fig. 8, as seen from the figure, this
The main component of a little nano particle fillers is Ce and O.Figure 10 is the high-resolution photo of the nano particle filler of Fig. 8, can be with
See that its spacing of lattice is 0.31nm, is CeO2(111) face.
Fourier transform infrared spectroscopy test phase: the ammonium ceric nitrate of 0.0005mol/L is used with Infrared Reflective Spectra test
Functionalized multi-wall carbonnanotubes after alcohol solution dipping, original functionalized multi-wall carbonnanotubes and 300 DEG C of heating cerous nitrates
Product CeO after ammonium 30min2The infrared spectrum spectrogram of (rare earth, 2001 (22): 69-72) three kinds of samples compares, to analyze
Its ingredient.
XRD test phase: more with the carboxylated after the ammonium ceric nitrate alcohol solution dipping of XRD test 0.0005mol/L
Wall carbon nano tube and standard CeO2Two kinds of samples.
The experimental results showed that with the ammonium ceric nitrate ethanol solution simply immersing carboxylated multi-wall carbon nano-tube of 0.0005mol/L
Pipe, forms the controllable ceria nanoparticles of a large amount of size inside carbon nanotube.
Embodiment 5
With the functionalized multi-wall carbonnanotubes after the cerous nitrate alcohol solution dipping of 0.11mol/L, air at room temperature
After middle drying, with the filling situation of nano-cerium oxide inside TEM observer, the ratio of two kinds of elements of Ce and O is had studied with EDS.
Processing stage: the functionalized multi-wall carbonnanotubes bought by Beijing Deco island King Company are immersed directly in
40min in the ammonium ceric nitrate ethanol solution of 0.11mol/L, is then filtered out with qualitative filter paper, natural in air at room temperature
It is dry.
TEM test phase: with the grown form of the nano-cerium oxide in TEM observation functionalized multi-wall carbonnanotubes, EDS is used
Rough whole elements composition that nano-cerium oxide has been determined and ratio.Figure 11 is the TEM photo of this example, can by figure
Know there is nano particle filler inside carbon nanotube, these packing sizes are limited by carbon nanotube internal diameter.Figure 12 is
These nano particles are carried out that EDS is analyzed as a result, showing the element group of these nano particles becomes two kinds of members of Ce and O
Element, and the ratio of two kinds of elements of Ce, O is close to 1:2, these nano particles of indirect proof are CeO2Nano particle.
The experimental results showed that with the cerous nitrate alcohol solution dipping functionalized multi-wall carbonnanotubes of 0.11mol/L, in carbon
The controllable ceria nanoparticles of a large amount of size are formd inside nanotube.
Above-described, only presently preferred embodiments of the present invention, the range being not intended to limit the invention, of the invention is upper
Stating embodiment can also make a variety of changes.Made by i.e. all claims applied according to the present invention and description
Simply, equivalent changes and modifications fall within the claims of the invention patent.The not detailed description of the present invention is
Routine techniques content.
Claims (10)
1. a kind of preparation method for the ceria nanoparticles that size is controllable, which comprises the following steps:
S1 provides the alcoholic solution and carbon nanotube of the nitrate of cerium, wherein the carbon nanotube is to possess sp2The carbon material of structure；
Carbon nanotube is immersed in the alcoholic solution of the nitrate of cerium by S2, so that the nitrate of cerium enters inside carbon nanotube；
And
S3, it is dry after filtering, so that the nitrate of cerium is decomposed to form the controllable ceria nanoparticles of size in carbon nanotube.
2. preparation method according to claim 1, which is characterized in that the alcoholic solution of the nitrate of cerium is the nitrate of cerium
Ethanol solution.
3. preparation method according to claim 1, which is characterized in that the alcoholic solution of the nitrate of cerium be ammonium ceric nitrate and its
The alcoholic solution of hydrate, cerous nitrate and its hydrate, cerous nitrate and its hydrate.
4. preparation method according to claim 1, which is characterized in that the concentration of the alcoholic solution of the nitrate of cerium is not less than
0.0005mol/L。
5. preparation method according to claim 1, which is characterized in that carbon nanotube is that single-walled carbon nanotube or multi wall carbon are received
Mitron.
6. preparation method according to claim 1, which is characterized in that carbon nanotube is carboxylic carbon nano-tube, carbonylation
Carbon nanotube, hydroxyl carbon nano tube or aminated carbon nano tube.
7. preparation method according to claim 1, which is characterized in that the internal diameter of carbon nanotube is between 1nm-15nm.
8. preparation method according to claim 1, which is characterized in that in the step S2, by ultrasonic wave auxiliary come
The ion of the nitrate of cerium is promoted to enter inside carbon nanotube.
9. preparation method according to claim 1, which is characterized in that in the step S3, by filter paper or aluminium net into
Row filtering.
10. preparation method according to claim 1, which is characterized in that in the step S3, at room temperature in air certainly
It is so dry.
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| CN1948157A (en) * | 2006-11-09 | 2007-04-18 | 上海大学 | Hollow bead shaped nano-cerium oxide and its preparation method |
| CN101264883A (en) * | 2008-04-21 | 2008-09-17 | 上海大学 | Method for preparing rare earth metal oxide and carbon nano-tube composite material of core-shell structure |
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