CN106115708A - A kind of continuous poriferous silicon materials of cellular three-dimensional and preparation method thereof - Google Patents
A kind of continuous poriferous silicon materials of cellular three-dimensional and preparation method thereof Download PDFInfo
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- CN106115708A CN106115708A CN201610439451.4A CN201610439451A CN106115708A CN 106115708 A CN106115708 A CN 106115708A CN 201610439451 A CN201610439451 A CN 201610439451A CN 106115708 A CN106115708 A CN 106115708A
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Abstract
The present invention discloses a kind of continuous poriferous silicon materials of cellular three-dimensional and preparation method thereof.Silicon materials of the present invention, are continuous, loose structures cellular, three-dimensional；Above-mentioned silicon hybridization material uses stober method single dispersing 80～800nm preparing spherical SiO 2 nanoparticle to be silicon source, is placed in after part of silica being reduced to elemental silicon by magnesiothermic reduction at 700～900 DEG C, finally uses hf etching to be prepared from after processing.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, it is aided with hf etching simultaneously, preparing the continuous poriferous silicon materials of cellular three-dimensional, this material hole is evenly distributed, size adjustable, and Stability Analysis of Structures, it is expected to extensively apply in fields such as lithium ion battery, photoelectric material, biological medicines.
Description
Technical field
The invention belongs to the preparation field of inorganic nano porous material, be specifically related to a kind of magnesiothermic reduction and prepare cellular three
Tie up continuous poriferous silicon materials and preparation method thereof.
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 synthesis of the most three-dimensional continuous cellular porous silicon is seldom reported.
Patent of the present invention mainly provides a kind of synthetic method synthesizing three-dimensional continuous cellular porous silicon.
Patent of the present invention employing Stober method silicon dioxide is as silicon precursor, in conjunction with magnesiothermic reduction and hf etching
Technology, the three-dimensional continuous cellular porous silicon of preparation.It is ripe that Stober method prepares nanometer titanium dioxide silicon technology classics, and product presents
Regular monodisperse spherical structure, size adjustable, preparation method is easy, can industrialized production.
Summary of the invention
It is an object of the present invention to provide a kind of continuous poriferous silicon materials of cellular three-dimensional.
Silicon materials of the present invention, are continuous, loose structures cellular, three-dimensional, and are mutually connected, present micron-scale；
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 after part of silica being reduced to elemental silicon by magnesiothermic reduction at 700～900 DEG C, finally uses at hf etching
It is prepared from after reason.
It is a further object to provide the preparation method of above-mentioned silicon materials.
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 700～900 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, then with Fluohydric acid. by therein lazy
Property silica composition etches away, and i.e. can get the continuous poriferous silicon materials of cellular three-dimensional.
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 700～900 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.
Step (5). above-mentioned pressed powder is placed in the diluted hydrofluoric acid that mass fraction is 1～5 under room temperature soak 0.5～
2 hours, it is centrifuged solid product, washed several times with water, obtains the continuous poriferous silicon materials of cellular three-dimensional after drying.
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, is aided with hf etching simultaneously, prepares the continuous poriferous silicon materials of cellular three-dimensional, this material
Hole is evenly distributed, size adjustable, and Stability Analysis of Structures, is expected in fields such as lithium ion battery, photoelectric material, biological medicines extensive
Application.
Accompanying drawing explanation
Fig. 1 is that in embodiment 1, the i.e. silicon dioxide microsphere of step (5) gained intermediate product is embedded in continuous poriferous silicon matrix
The scanning electron microscope (SEM) photograph of hybrid material.
Fig. 2 is that the scanning electron microscope (SEM) photograph of the continuous poriferous silicon materials of the most cellular three-dimensional of the end product obtained by embodiment 1 is (high
Times).
Fig. 3 is that the scanning electron microscope (SEM) photograph of the continuous poriferous silicon materials of the most cellular three-dimensional of the end product obtained by embodiment 1 is (low
Times).
Fig. 4 is circulations when doing lithium ion battery negative material of the embodiment 1 gained cellular three-dimensional continuous poriferous silicon materials
Performance chart.
Detailed description of the invention
Below in conjunction with the accompanying drawings the present invention is further analyzed.
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, then with Fluohydric acid. by therein lazy
Property silica composition etches away, and i.e. can get the continuous poriferous silicon materials of cellular three-dimensional.
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 700～900 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.
Step (5). above-mentioned pressed powder is placed in the diluted hydrofluoric acid that mass fraction is 1～5 under room temperature soak 0.5～
2 hours, it is centrifuged solid product, washed several times with water, obtains the continuous poriferous silicon materials of cellular three-dimensional after drying.
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 1 gram of silicon dioxide and 1 gram of magnesium powder hand mix under room temperature, obtain 2 grams of silicon dioxide and magnesium
Mixture；
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 multilamellar in continuous poriferous silicon matrix
Secondary sandwich.
Step (5). above-mentioned pressed powder is placed in the diluted hydrofluoric acid that mass fraction is 5% and soaks 1.5 hours under room temperature,
It is centrifuged solid product, washes 5 times, obtain the about 0.2g continuous poriferous silicon materials of cellular three-dimensional after drying.
As it is shown in figure 1, the intermediate product of embodiment 1 step (5) gained presents continuous micro-sphere structure, and through step (5)
The end product pattern later obtained as shown in Figure 2,3, presents the continuous poriferous structure of cellular three-dimensional, whereupon it may be inferred that middle
Product actually silicon dioxide microsphere is embedded in the multi-level sandwich in continuous poriferous silicon matrix；Fig. 4 illustrates that this material is made
During for lithium ion battery negative material, discharge capacity is up to 2700mAh/g first, and after circulation 100 circle, capacity also has 1200mAh/g
Above, 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 800 DEG C, and then isothermal reaction 1 hour under nitrogen atmosphere is down to room temperature, is 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.
Step (5). above-mentioned pressed powder is placed in the diluted hydrofluoric acid that mass fraction is 1 and soaks 2 hours under room temperature, from
The heart, to solid product, washed several times with water, obtains the continuous poriferous silicon materials of cellular three-dimensional after drying.
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 10 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 700 DEG C, and room temperature is down in isothermal reaction 24 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 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.
Step (5). above-mentioned pressed powder is placed in the diluted hydrofluoric acid that mass fraction is 5 and soaks 0.5 hour under room temperature,
It is centrifuged solid product, washed several times with water, obtains the continuous poriferous silicon materials of cellular three-dimensional after drying.
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 500
Rice；
Step (2). under room temperature, above-mentioned for 10g silicon dioxide is mixed according to mass ratio 1:1 with 10g magnesium powder, hands in mortar
Dynamic grinding 6 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 2 DEG C/min intensification is heated to 900 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 1mol/L and stirs 15 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.
Step (5). above-mentioned pressed powder is placed in the diluted hydrofluoric acid that mass fraction is 2 and soaks 1 hour under room temperature, from
The heart, to solid product, washed several times with water, obtains the continuous poriferous silicon materials of cellular three-dimensional after drying.
Claims (4)
1. silicon materials, it is characterised in that in continuous, loose structure cellular, three-dimensional；
Above-mentioned silicon hybridization material uses stober method single dispersing 80～800nm preparing spherical SiO 2 nanoparticle to be silicon source, is placed in
After part of silica being reduced to elemental silicon by magnesiothermic reduction at 700～900 DEG C, after finally using hf etching to process
It is prepared from.
2. the preparation method of silicon materials, 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 700～900 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.
Step (5), above-mentioned pressed powder is placed in the diluted hydrofluoric acid that mass fraction is 1～5 under room temperature to soak 0.5～2 little
Time, it is centrifuged solid product, washed several times with water, obtains the continuous poriferous silicon materials of cellular three-dimensional after drying.
The preparation method of a kind of silicon materials the most as claimed in claim 2, it is characterised in that described inert atmosphere can be nitrogen,
Argon, argon/hydrogen gas mixture.
4. a kind of silicon materials as claimed in claim 1, as the application in lithium cell cathode material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107565118A (en) * | 2017-08-30 | 2018-01-09 | 山东大学 | A kind of preparation method of high-performance lithium ion nano-silicon negative material |
| CN109659529A (en) * | 2018-12-17 | 2019-04-19 | 潍坊汇成新材料科技有限公司 | A kind of preparation process of silicon-carbon cathode material |
| CN110054192A (en) * | 2019-05-06 | 2019-07-26 | 燕山大学 | A kind of extra small nano SiO 2 particle of monodisperse and preparation method thereof |
| CN113800523A (en) * | 2021-09-09 | 2021-12-17 | 哈尔滨工业大学 | Layered porous silicon material and preparation method and application thereof |
| CN114044519A (en) * | 2021-11-11 | 2022-02-15 | 上海大学 | Method for preparing porous silicon material by reducing agent in controllable manner |
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| CN104466117A (en) * | 2014-11-05 | 2015-03-25 | 昆明理工大学 | Preparation method of three-dimensional porous silica powder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107565118A (en) * | 2017-08-30 | 2018-01-09 | 山东大学 | A kind of preparation method of high-performance lithium ion nano-silicon negative material |
| CN109659529A (en) * | 2018-12-17 | 2019-04-19 | 潍坊汇成新材料科技有限公司 | A kind of preparation process of silicon-carbon cathode material |
| CN110054192A (en) * | 2019-05-06 | 2019-07-26 | 燕山大学 | A kind of extra small nano SiO 2 particle of monodisperse and preparation method thereof |
| CN110054192B (en) * | 2019-05-06 | 2020-09-11 | 燕山大学 | Preparation method of monodisperse ultra-small silicon dioxide nanoparticles |
| CN113800523A (en) * | 2021-09-09 | 2021-12-17 | 哈尔滨工业大学 | Layered porous silicon material and preparation method and application thereof |
| CN114044519A (en) * | 2021-11-11 | 2022-02-15 | 上海大学 | Method for preparing porous silicon material by reducing agent in controllable manner |
| CN114044519B (en) * | 2021-11-11 | 2023-10-20 | 上海大学 | Method for preparing porous silicon material by controllable reducing agent |
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