CN107032356B - A kind of preparation method of porous nano silicon - Google Patents
A kind of preparation method of porous nano silicon Download PDFInfo
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- CN107032356B CN107032356B CN201710280081.9A CN201710280081A CN107032356B CN 107032356 B CN107032356 B CN 107032356B CN 201710280081 A CN201710280081 A CN 201710280081A CN 107032356 B CN107032356 B CN 107032356B
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- C01B33/00—Silicon; Compounds thereof
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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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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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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
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of preparation methods of porous nano silicon, comprising the following steps: chemical vapour deposition technique prepares two silicon powder crude product of magnesium, then handles two silicon powder crude product of magnesium with hydro-thermal method again, then will obtain porous nano silicon after hydro-thermal method treated product purification.The preparation method of porous nano silicon provided by the invention realizes the porous nano technology of bulky grain silicon, considerably reduces the preparation cost of porous nano silicon using simple equipment under the conditions of relatively low temperature.
Description
Technical field
The invention belongs to technical field of material, and in particular to a kind of preparation method of porous nano silicon.
Background technique
It is more and more important to the exploitation of green energy resource since environment and energy problem are got worse, thus research and development
The technology of electrochemical energy storage is also opposite to become researchers' general orientation of interest.Since nineteen seventies,
Many researchers because lithium ion battery has, energy density is big, self discharge is low, average output voltage is high, service life for using is long and
And many merits such as memory-less effect expand research work to it.From the development history of lithium ion battery, lithium ion battery
The research of negative electrode material play the role of to the development of lithium ion battery vital, and the appearance of carbon electrode is to lithium metal
The safety of electrode brings Gospel, so that application of the lithium ion battery in terms of commercialization be enable to have obtained development at full speed.
On the other hand for the science and technology grown rapidly at present, the theoretical capacity of graphite cathode material is relatively low, only
372mAh/g, although actual capacity is no longer satisfied the demand of present society very close to theoretical capacity, because
This, it is extremely urgent for the exploitation of the ion cathode material lithium of high capacity.The study found that the theoretical specific capacity of silicon is very high
, up to 4200mAh/g becomes most capable one of the high-capacity cathode material for replacing graphite.But, unique disadvantage of silicon
Be exactly that there is bulk effect strongly in charge and discharge process, caused the dusting of conductive particle, can to battery system into
Row destroys, so the cyclical stability of silicon electrode is poor, limits silicon as the application in terms of electrode material.But silicon
Nanosizing and porous silicon can effectively reduce its bulk effect, the cyclical stability of silicon electrode material be improved, to realization
Silicon electrode battery plays very important effect in commercialized development.
For at present, the preparation method of nano-silicon it is most be to silane etc. with the method for chemical vapor deposition containing silicon
The preparation of organic matter vapor-phase thermal cracking, this prepares the method for nano-silicon, and not only cost is very high, and may have the danger exploded；Separately
Outside, there are also magnesiothermic reduction, this method first has to prepare nano silicon oxide the preparation method of nano-silicon powder, then mainly according to
Under hot conditions prepared by magnesium-reduced silica, and process is more many and diverse and there is the silica being not sufficiently reacted in preparation process
It needs to be eroded with hydrofluoric acid, easily causes environmental pollution and preparation cost is high.
Summary of the invention
The present invention provides a kind of preparation methods of porous nano silicon, solve existing using silane as silicon source use
It is very high that chemical vapor deposition prepares nano-silicon cost, and the problem of be easy to happen explosion, and is received using magnesium reduction process preparation
Rice silicon process is more many and diverse and needs to be eroded with hydrofluoric acid in the presence of the silica being not sufficiently reacted during the preparation process, Yi Zao
At environmental pollution and the high problem of preparation cost.
The present invention provides a kind of preparation methods of porous nano silicon, comprising the following steps:
Step 1, high-purity silicon powder and magnesium powder are weighed respectively according to the mass ratio of 1:4-5, the high-purity silicon powder weighed is tiled
In crucible bottom with cover, then the open pot equipped with magnesium powder is put into crucible with cover, then will be put into after sealed crucible with cover
In vacuum tube furnace, control vacuum degree is 0.05-0.1Pa, keeps the temperature 15-60min at 500-650 DEG C, cools to room temperature with the furnace
After take out, obtain two silicon powder crude product of magnesium；
Step 2, at room temperature, two silicon powder crude product of magnesium obtained in step 1 is immersed into equipped with the anti-of saturation KCl aqueous solution
It answers in kettle, then reaction kettle is placed in air dry oven, taken out after keeping the temperature 30-300min at 120-180 DEG C, be cooled to room
Product is obtained after temperature, it is spare after product is washed with deionized water, is dried；
Step 3, product obtained in step 2 being put into vacuum tube furnace, control vacuum degree is 0.05-0.1Pa,
60-240min is kept the temperature at 550-750 DEG C, is taken out after cooling to room temperature with the furnace, the mixing of porous nano silicon powder and magnesia is obtained
Object, by the mixture of porous nano silicon powder and magnesia with concentration be 25% hydrochloric acid clean removing magnesia after, then spend from
Sub- water cleaning, is dried to get the porous nano silicon is arrived filtering.
Preferably, the purity of the high-purity silicon powder is 99.99%.
Preferably, the partial size of the high-purity silicon powder is 1-75 μm.
Compared with prior art, the beneficial effects of the present invention are:
The present invention uses bulky grain silicon powder for silicon source, then will be anti-by two silicon of chemical vapour deposition technique in-situ preparation magnesium
After the two silicon hydrothermal treatment of magnesium that should be obtained, by low temperature resintering technology in-situ preparation porous nano silicon and the composite wood of magnesia
Material will obtain porous nano Si powder after the processing of magnesia acid.The present invention can be under environmentally friendly simple condition by bulky grain silicon powder
Porous nano silicon materials are prepared into, is overcome and is used vapor-phase thermal cracking method in the prior art there are environmental pollution and be easy explosion
Defect, and after hydro-thermal process and low temperature resintering technology, the impurity in porous nano silicon is converted to magnesia substantially, thus
It can be washed by acid, improve the purity of product.
Detailed description of the invention
Fig. 1 is the device figure that the present invention prepares two silicon powder of chemical vapor deposition magnesium using chemical vapour deposition technique；
Fig. 2 is the macrograph of high-purity silicon powder used in the embodiment of the present invention 1 and the porous nano silicon prepared；
Fig. 3 is the X-ray powder diffraction comparison diagram for the porous nano silicon that the embodiment of the present invention 1 is prepared；
Fig. 4 is the scanning electron microscope (SEM) photograph for the porous nano silicon that the embodiment of the present invention 1 is prepared；
Fig. 5 is the macrograph for the porous nano silicon that the embodiment of the present invention 2 is prepared；
Fig. 6 is the Raman spectrogram for the porous nano silicon that the embodiment of the present invention 2 is prepared；
Fig. 7 is the scanning electron microscope (SEM) photograph for the porous nano silicon that the embodiment of the present invention 2 is prepared；
Fig. 8 is the macrograph of high-purity silicon powder used in the embodiment of the present invention 3 and the porous nano silicon prepared；
Fig. 9 is the Raman spectrogram for the porous nano silicon that the embodiment of the present invention 3 is prepared；
Figure 10 is the scanning electron microscope (SEM) photograph for the porous nano silicon that the embodiment of the present invention 3 is prepared；
Figure 11 is the macrograph of high-purity silicon powder used in the embodiment of the present invention 4 and the porous nano silicon prepared；
Figure 12 is the Raman spectrogram for the porous nano silicon that the embodiment of the present invention 4 is prepared；
Figure 13 is the scanning electron microscope (SEM) photograph for the porous nano silicon that the embodiment of the present invention 4 is prepared.
Specific embodiment
In order to enable those skilled in the art to more fully understand, technical solution of the present invention is practiced, below with reference to specific
The invention will be further described for embodiment and attached drawing, but illustrated embodiment is not as a limitation of the invention.
Experimental method and detection method described in following each embodiments are unless otherwise specified conventional method；The examination
Agent and material can be commercially available on the market unless otherwise specified.
Embodiment 1
A kind of preparation method of porous nano silicon, comprising the following steps:
Step 1, the high-purity silicon powder and magnesium powder that partial size is 1 μm, purity is 99.99% are weighed respectively according to the mass ratio of 1:4,
By the evenly laid out interior bottom in corundum crucible with cover of silicon powder, then the open corundum crucible equipped with excessive magnesium powder is put into cover
In corundum crucible, by corundum crucible with cover close the lid sealing after be put into vacuum tube furnace, through vacuumizing-be passed through high-purity argon
Gas-vacuum recycles 2 times, keeps the temperature 15min after being warming up to 600 DEG C under vacuum degree is 0.05Pa, cools to room temperature with the furnace
After take out, obtain two silicon powder crude product of magnesium；
Step 2, two silicon powder crude product of magnesium obtained in step 1 is immersed into the reaction kettle equipped with saturation KCl aqueous solution, so
Reaction kettle is placed in air dry oven afterwards, is warming up to 120 DEG C, is taken out after keeping 300min, obtains product after being cooled to room temperature,
It is spare after product is washed with deionized water, is dried；
Step 3, product obtained in step 2 is put into vacuum tube furnace, control vacuum degree is 0.05Pa, at 550 DEG C
Lower heat preservation 240min, takes out after cooling to room temperature with the furnace, obtains the mixture of porous nano silicon and magnesia, by porous nano silicon
Clean with the mixture of magnesia with the hydrochloric acid that concentration is 25% after removing magnesia, then is cleaned with deionized water, filter, do
It is dry to get arrive the porous nano silicon.
The phenetic analysis result for the porous nano silicon that embodiment 1 is prepared is as in Figure 2-4, and (a) figure is embodiment in Fig. 2
The macrograph of 1 μm of high-purity silicon powder used in 1, in Fig. 2 shown in (a) figure, high-purity silicon powder gray；(b) figure is embodiment 1 in Fig. 2
The macrograph for the porous nano silicon prepared, in Fig. 2 shown in (b) figure, khaki is presented in the porous nano silicon prepared；Fig. 3
The X-ray diffraction comparison diagram of the porous nano silicon and raw material high-purity silicon powder prepared for embodiment 1, wherein a curve indicates high-purity
Silicon powder, b curve indicates the porous nano silicon prepared with the high-purity silicon powder, it can be seen from the figure that the two goodness of fit is very high,
The porous nano impurity levels for illustrating that embodiment 1 is prepared are few, purity is high；Fig. 4 is the porous nano silicon that embodiment 1 is prepared
Scanning electron microscope (SEM) photograph, as shown in Figure 4, the nano-silicon for using this method to prepare to be porous, and size be less than 100nm.
Embodiment 2
A kind of preparation method of porous nano silicon, which comprises the following steps:
Step 1, the high-purity silicon powder and magnesium that partial size is 1 μm, purity is 99.99% are weighed respectively according to the mass ratio of 1:4.5
Then open corundum crucible equipped with excessive magnesium powder is put by powder by the evenly laid out interior bottom in corundum crucible with cover of silicon powder
In corundum crucible with cover, by corundum crucible with cover close the lid sealing after be put into vacuum tube furnace, through vacuumizing-be passed through height
Pure argon-vacuum recycles 2 times, keeps the temperature 60min after being warming up to 500 DEG C under vacuum degree is 0.08Pa, cools to the furnace
It is taken out after room temperature, obtains two silicon powder crude product of magnesium；
Step 2, two silicon powder crude product of chemical vapor deposition magnesium obtained in step 1 is immersed into equipped with saturation KCl aqueous solution
Reaction kettle in, then reaction kettle is placed in air dry oven, is warming up to 160 DEG C, is taken out after keeping 100min, is cooled to room
Product is obtained after temperature, it is spare after product is washed with deionized water, is dried；
Step 3, product obtained in step 2 is put into vacuum tube furnace, control vacuum degree is 0.08Pa, at 650 DEG C
Lower heat preservation 120min, takes out after cooling to room temperature with the furnace, obtains the mixture of porous nano silicon and magnesia, by porous nano silicon
Clean with the mixture of magnesia with the hydrochloric acid that concentration is 25% after removing magnesia, then is cleaned with deionized water, filter, do
It is dry to get arrive the porous nano silicon.
As illustrated in figs. 5-7, Fig. 5 is that embodiment 2 is prepared to the phenetic analysis result for the porous nano silicon that embodiment 2 is prepared
Porous nano silicon macrograph, the porous nano silicon be khaki；Fig. 6 is the drawing for the porous nano silicon that embodiment 2 is prepared
Graceful spectrogram coincide substantially with the Raman base peak of silicon；Fig. 7 is the scanning electron microscope (SEM) photograph for the porous nano silicon that embodiment 2 is prepared,
The nano-silicon that example 2 is prepared as shown in Figure 7 is porous and in Nano grade.
Embodiment 3
Step 1, the high-purity silicon powder and magnesium that partial size is 10 μm, purity is 99.99% are weighed respectively according to the mass ratio of 1:4.5
Then open corundum crucible equipped with excessive magnesium powder is put by powder by the evenly laid out interior bottom in corundum crucible with cover of silicon powder
In corundum crucible with cover, by corundum crucible with cover close the lid sealing after be put into vacuum tube furnace, through vacuumizing-be passed through height
Pure argon-vacuum recycles 2 times, keeps the temperature 60min after being warming up to 550 DEG C under vacuum degree is 0.1Pa, cools to room with the furnace
It is taken out after temperature, obtains two silicon powder crude product of magnesium；
Step 2, two silicon powder crude product of chemical vapor deposition magnesium obtained in step 1 is immersed into equipped with saturation KCl aqueous solution
Reaction kettle in, then reaction kettle is placed in air dry oven, is warming up to 180 DEG C, is taken out after keeping 30min, is cooled to room
Product is obtained after temperature, it is spare after product is washed with deionized water, is dried；
Step 3, product obtained in step 2 is put into vacuum tube furnace, control vacuum degree is 0.1Pa, at 700 DEG C
Keep the temperature 60min, taken out after cooling to room temperature with the furnace, obtain the mixture of porous nano silicon and magnesia, by porous nano silicon with
The mixture of magnesia clean with the hydrochloric acid that concentration is 25% remove magnesia after, then cleaned with deionized water, filtered, dried,
Obtain the porous nano silicon.
As seen in figs. 8-10, Fig. 8 (a) is 3 institute of embodiment to the phenetic analysis result for the porous nano silicon that embodiment 3 is prepared
With the macrograph of 10 μm of high-purity silicon powders, by shown in Fig. 8 (a), high-purity silicon powder is in grey black；Fig. 8 (b) is what embodiment 3 was prepared
Khaki is presented by the porous nano silicon shown in Fig. 8 (b), prepared in the macrograph of porous nano silicon；Fig. 9 is the preparation of embodiment 3
The Raman spectrogram of porous nano silicon out coincide with the Raman peaks of standard silicon；Figure 10 is the porous nano that embodiment 3 is prepared
The scanning electron microscope (SEM) photograph of silicon is porous nanometer structure.
Embodiment 4
Step 1, the high-purity silicon powder and magnesium that partial size is 75 μm, purity is 99.99% are weighed respectively according to the mass ratio of 1:5
Then open corundum crucible equipped with excessive magnesium powder is put by powder by the evenly laid out interior bottom in corundum crucible with cover of silicon powder
In corundum crucible with cover, by corundum crucible with cover close the lid sealing after be put into vacuum tube furnace, through vacuumizing-be passed through height
Pure argon-vacuum recycles 2 times, keeps the temperature 60min after being warming up to 650 DEG C under vacuum degree is 0.1Pa, cools to room with the furnace
It is taken out after temperature, obtains two silicon powder crude product of magnesium；
Step 2, two silicon powder crude product of magnesium obtained in step 1 is immersed into the reaction kettle equipped with saturation KCl aqueous solution, so
Reaction kettle is placed in air dry oven afterwards, is warming up to 180 DEG C, is taken out after keeping 240min, product is obtained after being cooled to room temperature, it will
Product is spare after being washed with deionized water, drying；
Step 3, two silicon powder crude product of hydro-thermal process magnesium obtained in step 2 is put into vacuum tube furnace, controls vacuum degree
For 0.1Pa, 240min is kept the temperature at 750 DEG C, is taken out after cooling to room temperature with the furnace, the mixing of porous nano silicon and magnesia is obtained
Object after the mixture of porous nano silicon and magnesia is cleaned removing magnesia with the hydrochloric acid that concentration is 25%, then uses deionization
Water cleaning, is dried to get the porous nano silicon is arrived filtering.
As figs 11-13, Figure 11 (a) is embodiment 4 to the phenetic analysis result for the porous nano silicon that embodiment 4 is prepared
The macrograph of 75 μm of high-purity silicon powders used, as shown in Figure 11 (a), high-purity silicon powder is in grey black and has metallic luster；Figure 11 (b) is
The macrograph for the porous nano silicon that embodiment 4 is prepared, as shown in Figure 11 (b), khaki is presented in the porous nano silicon prepared；
Figure 12 is the Raman spectrum picture for the porous nano silicon that embodiment 4 is prepared, and is coincide with the Raman peaks of standard silicon；Figure 13 is to implement
The scanning electron microscopic picture for the porous nano silicon that example 4 is prepared is porous nanometer structure.
Embodiment 1-4 has prepared porous nano silicon of good performance.The present invention is in the chemical vapour deposition technique system of use
When standby two silicon powder of chemical vapor deposition magnesium, the device of use is as shown in Figure 1, from figure 1 it appears that excessive magnesium powder list
Solely in open corundum crucible after, then the open corundum crucible equipped with magnesium powder is put into the corundum equipped with high-purity silicon powder with cover
In crucible, vacuum degree be 0.05-0.1Pa, temperature be 500-650 DEG C under conditions of, magnesium powder can gasify, the magnesium powder after gasification from
Evolution in open corundum crucible, then reacts with the high-purity silicon powder in corundum crucible with cover.Using this reactive mode, on the one hand
The contact area of magnesium powder and high-purity silicon powder after gasification is bigger, and reaction efficiency is higher, on the other hand after completion of the reaction, remains in product
The content of remaining magnesium powder is less, is conducive to the purifying of product and the recycling of magnesium powder.
The present invention increases hydro-thermal legal system after using chemical vapour deposition technique preparation two silicon powder of chemical vapor deposition magnesium again
The step of standby two silicon powder of hydro-thermal process magnesium, hydro-thermal process convert hydroxide for a part residue magnesium powder in two silicon of magnesium at low temperature
Magnesium is conducive to product and further purifies, it is even more important that hydro-thermal process can make on the basis of chemical vapor deposition
Occur more small nano aperture structures in two silicon powder of magnesium prepared, so that the nano-silicon finally prepared be made to have more
More, more small nano aperture structure, greatly improves the performance of product.
It should be noted that involved in claims of the present invention when numberical range, it is thus understood that each numberical range
Any one numerical value can be selected between two endpoints and two endpoints, due to step method and the embodiment 1-4 phase of use
Together, it repeats in order to prevent, description of the invention preferred embodiment, once a person skilled in the art knows basic
Creative concept, then additional changes and modifications may be made to these embodiments.It is wrapped so the following claims are intended to be interpreted as
It includes preferred embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within be also intended to include these modifications and variations.
Claims (3)
1. a kind of preparation method of porous nano silicon, which comprises the following steps:
Step 1, high-purity silicon powder and magnesium powder are weighed respectively according to the mass ratio of 1:4-5, the high-purity silicon powder weighed is laid in band
Then open pot equipped with magnesium powder is put into crucible with cover, then will be put into vacuum after sealed crucible with cover by lid crucible bottom
In tube furnace, control vacuum degree is 0.05-0.1Pa, keeps the temperature 15-60min at 500-650 DEG C, takes after cooling to room temperature with the furnace
Out, two silicon powder crude product of magnesium is obtained；
Step 2, at room temperature, two silicon powder crude product of magnesium obtained in step 1 is immersed into the reaction kettle equipped with saturation KCl aqueous solution
In, then reaction kettle is placed in air dry oven, is taken out after keeping the temperature 30-300min at 120-180 DEG C, after being cooled to room temperature
Product is obtained, it is spare after product is washed with deionized water, is dried；
Step 3, product obtained in step 2 is put into vacuum tube furnace, control vacuum degree is 0.05-0.1Pa, in 550-
60-240min is kept the temperature at 750 DEG C, is taken out after cooling to room temperature with the furnace, the mixture of porous nano silicon powder and magnesia is obtained, it will
After the mixture of porous nano silicon powder and magnesia cleans removing magnesia with the hydrochloric acid that concentration is 25%, then it is clear with deionized water
It washes, filter, drying to get the porous nano silicon is arrived.
2. the preparation method of porous nano silicon according to claim 1, which is characterized in that the purity of the high-purity silicon powder is
99.99%.
3. the preparation method of porous nano silicon according to claim 2, which is characterized in that the partial size of the high-purity silicon powder is
1-75μm。
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306818A (en) * | 2008-07-01 | 2008-11-19 | 浙江理工大学 | Method for preparing magnesium silicide and device |
| CN102237519A (en) * | 2011-07-11 | 2011-11-09 | 三峡大学 | Fluorine-free preparation method for three-dimensional porous silica powder anode material of lithium ion battery |
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2017
- 2017-04-26 CN CN201710280081.9A patent/CN107032356B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306818A (en) * | 2008-07-01 | 2008-11-19 | 浙江理工大学 | Method for preparing magnesium silicide and device |
| CN102237519A (en) * | 2011-07-11 | 2011-11-09 | 三峡大学 | Fluorine-free preparation method for three-dimensional porous silica powder anode material of lithium ion battery |
Non-Patent Citations (1)
| Title |
|---|
| Hydrothermal synthesis of nano-silicon from a silica sol and its use in lithium ion batteries;Jianwen Liang等;《Nano Research》;20151231;第8卷(第5期);全文 |
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Inventor after: Zhu Congxu Inventor after: Yue Hongwei Inventor after: Liu Haofeng Inventor after: Li Tingting Inventor after: Gao Yuanhao Inventor after: Yang Xiaogang Inventor after: Wu Xiwang Inventor after: Liu Chuang Inventor after: Tie Weiwei Inventor after: Zhao Hongxiao Inventor before: Zhu Congxu Inventor before: Yue Hongwei Inventor before: Liu Haofeng Inventor before: Li Tingting Inventor before: Gao Yuanhao Inventor before: Yang Xiaogang Inventor before: Wu Xiwang Inventor before: Liu Chuang Inventor before: Tie Weiwei Inventor before: Zhao Hongxiao |
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