CN106129345A - Multilayered structure material that a kind of silicon dioxide microsphere is embedded in continuous poriferous silicon matrix and preparation method thereof - Google Patents
Multilayered structure material that a kind of silicon dioxide microsphere is embedded in continuous poriferous silicon matrix and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses multilayered structure material that a kind of silicon dioxide microsphere is embedded in continuous poriferous silicon matrix and preparation method thereof.This silicon hybridization material is the hybrid structure that silicon dioxide microsphere is embedded in continuous poriferous silicon matrix；Above-mentioned silicon hybridization material uses stober method single dispersing 80～800nm preparing spherical SiO 2 nanoparticle to be silicon source, is placed in and by magnesiothermic reduction, part of silica is reduced to elemental silicon at 700～800 DEG C and is prepared from.The inventive method uses stober method silicon dioxide with low cost simple and easy to get to be raw material, combined process is ripe, the magnesiothermic reduction technology that energy consumption is relatively low, obtain the hybrid material that silicon dioxide microsphere is embedded in continuous poriferous silicon matrix, this scantling is evenly distributed, size is adjustable, can effectively alleviate the Volumetric expansion of silicon as lithium ion battery negative material, improves cyclical stability.
Description
Technical field
The invention belongs to the preparation field of inorganic nano porous material, be specifically related to a kind of silicon dioxide microsphere and be embedded in continuously
Multilayered structure material in porous silicon substrate and preparation method thereof, is to use magnesiothermic reduction to prepare silicon dioxide microsphere to be embedded in even
The method of continuous porous silicon substrate.
Background technology
All the time, utilize cheap silicon dioxide or silicate to prepare silicon materials and be required for higher reaction temperature.Mesh
The method of front industrial employing is still that pyrocarbon thermal reduction (> 1700 DEG C), prepared silicon is mostly bulk, it is difficult to application
In lithium ion battery negative material.The appearance of magnesiothermic reduction technology in 2007 greatly reduces the reduction temperature of silicon dioxide, with
Time can also prepare the silicon materials of nano-scale, therefore suffered from paying close attention to widely.
Patent 201510011852.5 discloses a kind of method that nano silicon material is prepared in magnesiothermic reduction, raw materials used SiO2
Being a length of 300～800nm, width is the rod-like nano material of 20～40nm, and patent 201310059792.5 discloses one
Magnesiothermic reduction preparation has the order mesoporous silicon nano material of MCM-41 molecular sieve structure, raw materials used SiO2Mesoporous for MCM-41
Molecular sieve.
Comparing these silicon materials, the cellular porous silicon of continuous structure has special advantage.On the one hand, it may be possible to provide higher
Specific surface area, still further aspect, possess higher tap density, have at lithium ion battery and catalytic field and preferably should
Use prospect.But the nearly no report of synthesis of the most three-dimensional continuous cellular porous silicon.Further, silicon dioxide microsphere is uniform
The multilayered structure material being embedded in three-dimensional continuous cellular porous silicon possesses more special as lithium ion battery negative material
Other advantage.Silicon dioxide microsphere can effectively absorb the stress that three-dimensional continuous poriferous silicon produces during removal lithium embedded, thus
Change kind lithium ion battery negative material cycle performance.
It is the most cellular porous that patent of the present invention mainly provides a kind of synthetic silica microsphere to be uniformly embedded in three-dimensional
The synthetic method of the multilayered structure material in silicon.
The present invention proposes to use stober method Nano particles of silicon dioxide as raw material, by magnesiothermic reduction, prepares dioxy
SiClx microsphere is embedded in the hybrid material in continuous poriferous silicon matrix, and for lithium ion battery negative material.Prepared by Stober method
Nanometer titanium dioxide silicon technology classics are ripe, and product presents regular monodisperse spherical structure, size adjustable, silicon dioxide microsphere
Surface reaction activity is high, and preparation method simplicity can industrialized production.
Summary of the invention
It is an object of the present invention to provide a kind of simple and easy to do silicon dioxide microsphere to be embedded in continuous poriferous silicon matrix
Hybrid material.
Silicon hybridization material of the present invention, is the silicon dioxide microsphere hybrid structure that is embedded in continuous poriferous silicon matrix；Wherein dioxy
The mass content of SiClx microsphere is 10～90 controlled；
Above-mentioned silicon hybridization material uses stober method single dispersing 80～800nm preparing spherical SiO 2 nanoparticle to be silicon source,
It is placed in and by magnesiothermic reduction, part of silica is reduced to elemental silicon at 700～800 DEG C and is prepared from.
It is a further object to provide the hydridization material that above-mentioned silicon dioxide microsphere is embedded in continuous poriferous silicon matrix
The preparation method of material.
The present invention to the effect that uses stober method monodisperse silica nanoparticle to be silicon source, by regulation and control magnesium heat
Reducing silica, in the range of 700～800 DEG C, is elemental silicon by the temperature of reduction, due to the no thoroughness of reaction, the most completely
The part of silica of reduction is spherical in shape to be dispersed in three-dimensional continuous poriferous silicon matrix, washes by-product magnesium oxide off with dilute hydrochloric acid
After, i.e. can get the hybrid material that silicon dioxide microsphere is embedded in continuous poriferous silicon matrix.
Comprising the concrete steps that of the inventive method:
Step (1). prepare silicon dioxide: employing Stober method is in alcohol phase medium, with ammonia-catalyzed positive silicic acid four butyl ester
(TEOS), form monodispersed preparing spherical SiO 2 particles through hydrolysis-condensation, by regulation pH value control particle diameter 80～
800 nanometers；
Step (2). under room temperature by above-mentioned silicon dioxide with magnesium powder according to mass ratio 1:(0.5～1.5) mix, in mortar
Hand-ground 5～10 minutes, obtain the mixture of silicon dioxide and magnesium；
Step (3). the mixture of above-mentioned silicon dioxide Yu magnesium is packaged in crucible and is placed in tube furnace control intensification speed
Rate is that 0.1～5 DEG C/min heats up and is heated to 700～800 DEG C, and room is down in isothermal reaction 1～24 hours under inert atmosphere then
Temperature, obtains reduction crude product.
Described inert atmosphere can be nitrogen, argon, argon/hydrogen gas mixture (volume ratio 95/5).
Step (4). reduction crude product is placed in the dilute hydrochloric acid that concentration is 0.5～2mol/L under room temperature that to stir 4～24 little
Time, it is centrifuged and obtains solid product, washed several times with water, the most i.e. can get silicon dioxide microsphere and be embedded in continuous poriferous silicon matrix
Hybrid material.
The inventive method uses stober method silicon dioxide with low cost simple and easy to get to be raw material, and combined process is ripe,
The magnesiothermic reduction technology that energy consumption is relatively low, obtains the hybrid material that silicon dioxide microsphere is embedded in continuous poriferous silicon matrix, this material
Even size distribution, size is adjustable, can effectively alleviate the Volumetric expansion of silicon as lithium ion battery negative material, and raising follows
Ring stability.
Accompanying drawing explanation
Fig. 1 is the scanning that the silicon dioxide microsphere obtained by embodiment 1 is embedded in the hybrid material in continuous poriferous silicon matrix
Electronic Speculum figure (high power).
Fig. 2 is the scanning electricity of the hybrid material that the silicon dioxide microsphere of embodiment 1 gained is embedded in continuous poriferous silicon matrix
Mirror figure (low power).
Fig. 3 is that the hybrid material that is embedded in continuous poriferous silicon matrix of the silicon dioxide microsphere of embodiment 1 gained is through hydrogen fluorine
The scanning electron microscope (SEM) photograph of the continuous poriferous silicon materials of cellular three-dimensional obtained after acid etch.
Fig. 4 be the hybrid material that is embedded in continuous poriferous silicon matrix of the silicon dioxide microsphere of embodiment 1 gained as lithium from
Electrochemistry cyclic curve during sub-cell negative electrode material.
Detailed description of the invention
Below in conjunction with the accompanying drawings the present invention is further analyzed.
Inventive silica microsphere is embedded in the preparation method of the hybrid material in continuous poriferous silicon matrix, as follows:
Step (1). prepare silicon dioxide: employing Stober method is in alcohol phase medium, with ammonia-catalyzed positive silicic acid four butyl ester
(TEOS), form monodispersed preparing spherical SiO 2 particles through hydrolysis-condensation, by regulation pH value control particle diameter 80～
800 nanometers；
Step (2). under room temperature by above-mentioned silicon dioxide with magnesium powder according to mass ratio 1:(0.5～1.5) mix, in mortar
Hand-ground 5～10 minutes, obtain the mixture of silicon dioxide and magnesium；
Step (3). the mixture of above-mentioned silicon dioxide Yu magnesium is packaged in crucible and is placed in tube furnace control intensification speed
Rate is that 0.1～5 DEG C/min heats up and is heated to 700～800 DEG C, and room is down in isothermal reaction 1～24 hours under inert atmosphere then
Temperature, obtains reduction crude product.
Described inert atmosphere can be nitrogen, argon, argon/hydrogen gas mixture (volume ratio 95/5).
Step (4). reduction crude product is placed in the dilute hydrochloric acid that concentration is 0.5～2mol/L under room temperature that to stir 4～24 little
Time, it is centrifuged and obtains solid product, washed several times with water, the most i.e. can get silicon dioxide microsphere and be embedded in continuous poriferous silicon matrix
Hybrid material.
Above-mentioned silicon hybridization material, is the silicon dioxide microsphere hybrid structure that is embedded in continuous poriferous silicon matrix；Wherein titanium dioxide
The mass content of silicon microsphere is 10～90 controlled.
Embodiment 1
Step (1). prepare silicon dioxide: employing Stober method is in alcohol phase medium, with ammonia-catalyzed positive silicic acid four butyl ester
(TEOS), form monodispersed preparing spherical SiO 2 particles through hydrolysis-condensation, control particle diameter by regulation pH value and receive 400
Rice；
Step (2). take above-mentioned 1g silicon dioxide and 1g magnesium powder hand mix under room temperature, obtain the mixed of 2g silicon dioxide and magnesium
Compound；
Step (3). the mixture of above-mentioned silicon dioxide Yu magnesium is packaged in crucible and is placed in tube furnace control intensification speed
Rate is that 5 DEG C/min intensification is heated to 700 DEG C, and room temperature is down in isothermal reaction 4 hours under argon gas atmosphere then, obtains reducing and slightly produces
Thing.
Step (4). reduction crude product is placed in the dilute hydrochloric acid that concentration is 1mol/L and stirs 4 hours under room temperature, centrifugal
To solid product, wash 5 times, the most i.e. can obtain about 0.3g silicon dioxide microsphere and be embedded in the hydridization in continuous poriferous silicon matrix
Material.
As shown in Figure 1, 2, the hybrid material that embodiment 1 obtains is the spherical of inter-adhesive, size uniformity (400 nanometer),
Seem the monodisperse spherical structure maintaining raw material, actually pass after hf etching falls unreacted silicon dioxide, hydridization
Material becomes the continuous poriferous silicon of cellular three-dimensional (shown in Fig. 3), the spheroidal particle actually silicon dioxide before illustrating, and
It is connected with each other the most integral.Fig. 4 illustrates that this material still has as capacity after circulating 100 circles during lithium ion battery negative material
More than 800mAh/g, good cycling stability.
Embodiment 2
Step (1). prepare silicon dioxide: employing Stober method is in alcohol phase medium, with ammonia-catalyzed positive silicic acid four butyl ester
(TEOS), form monodispersed preparing spherical SiO 2 particles through hydrolysis-condensation, control particle diameter by regulation pH value and receive 80
Rice；
Step (2). under room temperature, above-mentioned for 10g silicon dioxide is mixed according to mass ratio 1:0.5 with 5g magnesium powder, hands in mortar
Dynamic grinding 5 minutes, obtains the mixture of silicon dioxide and magnesium；
Step (3). the mixture of above-mentioned silicon dioxide Yu magnesium is packaged in crucible and is placed in tube furnace control intensification speed
Rate is that 0.1 DEG C/min intensification is heated to 720 DEG C, and then isothermal reaction 24 hours under nitrogen atmosphere are down to room temperature, are obtained reduction thick
Product.
Step (4). reduction crude product is placed in the dilute hydrochloric acid that concentration is 0.5mol/L and stirs 24 hours under room temperature, centrifugal
Obtain solid product, washed several times with water, the most i.e. can get the hydridization material that silicon dioxide microsphere is embedded in continuous poriferous silicon matrix
Material.
Embodiment 3
Step (1). prepare silicon dioxide: employing Stober method is in alcohol phase medium, with ammonia-catalyzed positive silicic acid four butyl ester
(TEOS), form monodispersed preparing spherical SiO 2 particles through hydrolysis-condensation, control particle diameter by regulation pH value and receive 800
Rice；
Step (2). under room temperature, above-mentioned for 5g silicon dioxide is mixed according to mass ratio 1:1.5 with 7.5g magnesium powder, in mortar
Hand-ground 5 minutes, obtains the mixture of silicon dioxide and magnesium；
Step (3). the mixture of above-mentioned silicon dioxide Yu magnesium is packaged in crucible and is placed in tube furnace control intensification speed
Rate is that 5 DEG C/min intensification is heated to 800 DEG C, and room temperature is down in isothermal reaction 1 hour under argon gas atmosphere then, obtains reducing and slightly produces
Thing.
Step (4). reduction crude product is placed in the dilute hydrochloric acid that concentration is 2mol/L and stirs 4 hours under room temperature, centrifugal
To solid product, washed several times with water, the most i.e. can get the hybrid material that silicon dioxide microsphere is embedded in continuous poriferous silicon matrix.
Embodiment 4
Step (1). prepare silicon dioxide: employing Stober method is in alcohol phase medium, with ammonia-catalyzed positive silicic acid four butyl ester
(TEOS), form monodispersed preparing spherical SiO 2 particles through hydrolysis-condensation, control particle diameter by regulation pH value and receive 300
Rice；
Step (2). under room temperature, above-mentioned for 5g silicon dioxide is mixed according to mass ratio 1:1 with 5g magnesium powder, in mortar manually
Grind 5～10 minutes, obtain the mixture of silicon dioxide and magnesium；
Step (3). the mixture of above-mentioned silicon dioxide Yu magnesium is packaged in crucible and is placed in tube furnace control intensification speed
Rate is that 2 DEG C/min intensification is heated to 750 DEG C, isothermal reaction 15 hours under argon/hydrogen gas mixture (volume ratio 95/5) atmosphere,
Then it is down to room temperature, obtains reduction crude product.
Step (4). reduction crude product is placed in the dilute hydrochloric acid that concentration is 1.5mol/L and stirs 15 hours under room temperature, centrifugal
Obtain solid product, washed several times with water, the most i.e. can get the hydridization material that silicon dioxide microsphere is embedded in continuous poriferous silicon matrix
Material.
Claims (5)
1. a silicon hybridization material, it is characterised in that be the silicon dioxide microsphere hybrid structure that is embedded in continuous poriferous silicon matrix；On
State silicon hybridization material use stober method single dispersing 80～800nm preparing spherical SiO 2 nanoparticle be silicon source, be placed in 700～
By magnesiothermic reduction, part of silica is reduced to elemental silicon at 800 DEG C be prepared from.
2. the preparation method of a silicon hybridization material, it is characterised in that the method comprises the following steps:
Step (1), prepare silicon dioxide: use Stober method in alcohol phase medium, with ammonia-catalyzed positive silicic acid four butyl ester
(TEOS), form monodispersed preparing spherical SiO 2 particles through hydrolysis-condensation, by regulation pH value control particle diameter 80～
800 nanometers；
Under step (2), room temperature by above-mentioned silicon dioxide with magnesium powder according to mass ratio 1:(0.5～1.5) mix, in mortar manually
Grind 5～10 minutes, obtain the mixture of silicon dioxide and magnesium；
Step (3), the mixture of above-mentioned silicon dioxide with magnesium is packaged in crucible be placed in tube furnace control heating rate be
0.1～5 DEG C/min heats up and is heated to 700～800 DEG C, isothermal reaction 1～24 hours under inert atmosphere, is then down to room temperature,
To reduction crude product；
Step (4), reduction crude product is placed in the dilute hydrochloric acid that concentration is 0.5～2mol/L under room temperature and stirs 4～24 hours, from
Gains in depth of comprehension, to solid product, washed several times with water, the most i.e. can get the hydridization that silicon dioxide microsphere is embedded in continuous poriferous silicon matrix
Material.
3. silicon hybridization material as claimed in claim 1 a kind of, it is characterised in that the mass content of silicon dioxide microsphere be 10～
90 is controlled.
The preparation method of a kind of silicon hybridization material the most as claimed in claim 2, it is characterised in that described inert atmosphere can be
Nitrogen, argon, argon/hydrogen gas mixture.
5. a kind of silicon hybridization material as claimed in claim 1, as the application on lithium ion battery negative material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110336003A (en) * | 2019-06-28 | 2019-10-15 | 浙江工业大学 | A kind of porous silicon-base composite material and preparation method and application |
| WO2024152919A1 (en) * | 2023-01-17 | 2024-07-25 | 宁德时代新能源科技股份有限公司 | Negative electrode material, negative electrode plate, electrode assembly, battery, and electric device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259858A (en) * | 2011-06-07 | 2011-11-30 | 同济大学 | Method for preparing porous silicon by magnesiothermic reduction |
| CN104577066A (en) * | 2014-12-29 | 2015-04-29 | 南开大学 | Silicon oxide composite negative pole material for lithium ion secondary battery and preparation method thereof |
| WO2015196092A1 (en) * | 2014-06-20 | 2015-12-23 | Wei Wang | Porous silicon nanostructured electrode and method |
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2016
- 2016-06-17 CN CN201610444246.7A patent/CN106129345A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102259858A (en) * | 2011-06-07 | 2011-11-30 | 同济大学 | Method for preparing porous silicon by magnesiothermic reduction |
| WO2015196092A1 (en) * | 2014-06-20 | 2015-12-23 | Wei Wang | Porous silicon nanostructured electrode and method |
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| DANFENG QIU ET AL.: ""Mesoporous silicon microspheres fabricated via in situ magnesiothermic reduction of silicon oxide as a high-performance anode material for lithium–ion batteries"", 《J SOLID STATE ELECTROCHEM》 * |
| HAI ZHONG ET AL.: ""Synthesis of nanosized mesoporous silicon by magnesium-thermal method used as anode material for lithium ion battery"", 《JOURNAL OF POWER SOURCES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110336003A (en) * | 2019-06-28 | 2019-10-15 | 浙江工业大学 | A kind of porous silicon-base composite material and preparation method and application |
| WO2024152919A1 (en) * | 2023-01-17 | 2024-07-25 | 宁德时代新能源科技股份有限公司 | Negative electrode material, negative electrode plate, electrode assembly, battery, and electric device |
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Application publication date: 20161116 |