CN108110239A - A kind of silica-base material with diatomite porous structure and its preparation method and application - Google Patents
A kind of silica-base material with diatomite porous structure and its preparation method and application Download PDFInfo
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- CN108110239A CN108110239A CN201711347938.0A CN201711347938A CN108110239A CN 108110239 A CN108110239 A CN 108110239A CN 201711347938 A CN201711347938 A CN 201711347938A CN 108110239 A CN108110239 A CN 108110239A
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/625—Carbon or graphite
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Abstract
The present invention provides a kind of silica-base materials with diatomite porous structure and its preparation method and application, preparation method provided by the invention is by selecting magnesium alloy powder and diatomite mixing and ball milling, calcining, so that oxygen element is not contained comprising carbon and element silicon in obtained silicon substrate, and the silicon substrate has diatomite porous structure, hollow and be evenly distributed, consistent appearance, size is controllable (30~100 μm)；So that the material has higher reversible capacity and excellent cyclical stability.
Description
Technical field
The present invention relates to silicon materials field more particularly to a kind of silica-base materials and its preparation with diatomite porous structure
Methods and applications.
Background technology
With the development of society, portable electric appts, hybrid vehicle, pure electric automobile are contacted with our life
Must be more and more closer, people are higher and higher to the demand of rechargeable battery.But current commercialized negative electrode of lithium ion battery material
Expect that for graphite-like carbon material, theoretical capacity is only 372mAh g-1, it is impossible to meet the needs of practical application, so research Fabrication of High Specific Capacitance
Amount, high magnification, the lithium ion battery negative material of stable cycle performance are extremely urgent.
Silicon materials are because it is up to 4200mAh g-1Specific capacity become the hot spot of research, but had very in process of intercalation
Big volume expansion crushes electrode material rupture, is peeled off from collector, and electric conductivity declines, and capacity fails rapidly, so mesh
The performance of the silicon materials of preceding offer also needs to improve, to obtain effectively inhibiting due to caused by silicon volume change
The silica-base material of mechanical stress improves the structural stability of silica-base material, so that silica-base material can be used as lithium-ion electric
Pond negative material.
The content of the invention
In view of this, the technical problems to be solved by the invention are to provide a kind of silicon substrate with diatomite porous structure
Material and its preparation method and application, silica-base material prepared by preparation method provided by the invention are the silicon substrate of porous structure
Material, and large specific surface area can be used as cell negative electrode material, improve its chemical property.
The present invention provides a kind of preparation method of the silica-base material with diatomite porous structure, including：
1) by magnesium alloy powder and the material mixing and ball milling of containing diatomite, mixture is obtained；
2) mixture for obtaining step 1) is calcined, the sample after being calcined；
3) sample after calcining and hydrochloric acid solution are reacted, obtains the silica-base material with diatomite porous structure.
Preferably, the magnesium alloy powder for AZ31 magnesium alloy powders, AM41 magnesium alloy powders, ZK61 magnesium alloy powders or
AS41 magnesium alloy powders.
Preferably, the grain size of the magnesium alloy powder is 40~100 μm.
Preferably, the material of the containing diatomite is diatomite or the composite material of diatomite and graphene.
Preferably, the rotating speed of mixing and ball milling is 500~650rpm in the step 1).
Preferably, the mass ratio of the magnesium alloy powder and the material of the containing diatomite is 4: (4.5~6).
Preferably, the temperature of calcining is 650~850 DEG C in the step 2).
Preferably, the concentration of the hydrochloric acid solution is 0.8~1.2mol/L.
The present invention also provides a kind of silica-base materials with diatomite porous structure, are had by preparation of the present invention
The method of the silica-base material of diatomite porous structure is prepared.
It is more with diatomite including preparation of the present invention the present invention also provides a kind of lithium ion battery negative material
The silica-base material with diatomite porous structure that the method for the silica-base material of pore structure is prepared.
Compared with prior art, the present invention provides a kind of silica-base material with diatomite porous structure and its preparation sides
Method and application, preparation method provided by the invention are calcined so that obtain by selecting magnesium alloy powder and diatomite mixing and ball milling
Silicon substrate in comprising carbon and element silicon do not contain oxygen element, and the silicon substrate has a diatomite porous structure, it is hollow and point
Cloth is uniform, consistent appearance, and size is controllable (30~100 μm)；So that the material has higher reversible capacity and excellent
Cyclical stability, the experimental results showed that, silica-base material provided by the invention is permanent as the lithium battery that ion cathode material lithium obtains
Current charging and discharging test loop voltage range 0.01-2.0V, current density are 100mA g-1, charge and discharge specific volume is 1787mAh g-1；After Xun Huan 100 times, charge and discharge specific volume is 805mAh g-1, capacity retention ratio is up to 45%.
Description of the drawings
Fig. 1 is the SEM figures for the silica-base material with diatomite porous structure that the embodiment of the present invention 1 obtains；
Fig. 2 is the XRD diagram for the silica-base material with diatomite porous structure that the embodiment of the present invention 1 obtains；
Fig. 3 is the SEM figures for the silica-base material with diatomite porous structure that the embodiment of the present invention 2 obtains；
Fig. 4 is the XRD diagram for the silica-base material with diatomite porous structure that the embodiment of the present invention 2 obtains；
Fig. 5 is the SEM for the silicon-based/graphecomposite composite with diatomite porous structure that the embodiment of the present invention 3 obtains
Figure；
Fig. 6 is the EDS for the silicon-based/graphecomposite composite with diatomite porous structure that the embodiment of the present invention 3 obtains
Elemental analysis result；
Fig. 7 is the compound BET of the obtained silica-base material/graphene with diatomite porous structure of the embodiment of the present invention 3
Characterization result；
Fig. 8 is the volt-ampere cycle of silica-base material of the present invention and the lithium battery of silicon-based/graphecomposite composite preparation
Graph；
Fig. 9 is the electrochemistry capacitance test result of lithium battery prepared by silicon-based/graphecomposite composite of the present invention；
Figure 10 is the stable circulation of silica-base material of the present invention and the lithium battery of silicon-based/graphecomposite composite preparation
Property test result；
Figure 11 is the electrochemistry resistance of silica-base material of the present invention and the lithium battery of silicon-based/graphecomposite composite preparation
Anti- spectrum.
Specific embodiment
The present invention provides a kind of preparation method of the silica-base material with diatomite porous structure, including：
1) by magnesium alloy powder and the material mixing and ball milling of containing diatomite, mixture is obtained；
2) mixture for obtaining step 1) is calcined, the sample after being calcined；
3) sample after calcining and hydrochloric acid solution are reacted, obtains the silica-base material with diatomite porous structure.
According to the present invention, magnesium alloy powder and diatomite mixing and ball milling are obtained mixture by the present invention；Wherein, the magnesium
Alloy powder is preferably AZ31 magnesium alloy powders, AM41 magnesium alloy powders, ZK61 magnesium alloy powders or AS41 magnesium alloy powders, more
Preferably AZ31 magnesium alloy powders；The grain size of the magnesium alloy powder is preferably 40-100 μm, more preferably 50~80 μm, optimal
Elect 60~70 μm as；The present invention does not have the source of magnesium alloy powder particular/special requirement, and the present invention is preferably prepared in accordance with the following methods：
Magnesium alloy scurf is placed in ball grinder, when ball milling 8~12 is small under the conditions of 500~800rpm of rotating speed, obtains magnesium alloy powder,
In, the rotating speed is preferably 600~700rpm.The material of the containing diatomite is compound for diatomite or diatomite and graphene
Material；The present invention does not have diatomaceous source particular/special requirement, commercially available diatomite, and general diatomite is white solid powder
End, diatom shell size are 30 μm or so, and abundant macropore is contained on diatom shell surface, it contains a small amount of mesoporous and micro- in addition
Hole so that diatomite has unique multi-stage artery structure, specific surface area 2.73m2/ g, diatomite main matter are SiO2,
Middle SiO2Content is 86% or so, and other impurities include Al2O3、Fe2O3, MgO etc., it is preferred that diatomaceous silicon of the present invention
Frustule body is preferably dimensioned to be 20~50 μm, more preferably 30~40 μm；The magnesium alloy powder and the material of the containing diatomite
Mass ratio be preferably 4: (4.5~6), more preferably 4: 5.
In the present invention, the magnesium alloy powder and the rotating speed of diatomite mixing and ball milling are preferably 500~650rpm, more preferably
For 550~600rpm.
According to the present invention, the present invention will also calcine the mixture that step 1) obtains, the sample after being calcined；The present invention
There is no particular/special requirement, calcining manners well known in the art to the environment and mode of calcining；It is specifically, of the invention by mixture
It being placed in quartz ampoule, then Vacuum Package is calcined in Muffle furnace, wherein, the calcining heat is preferably 650~850 DEG C, more
Preferably 700~800 DEG C；When the calcination time is preferably 10~18 small, more preferably 12~16 it is small when；Before the calcining also
Including by calcination environment with 8~10 it is small when temperature programming to 700 DEG C.
According to the present invention, the present invention also reacts the sample after calcining and hydrochloric acid solution, obtains having diatomite porous knot
The silica-base material of structure；Wherein, the concentration of the hydrochloric acid solution is preferably 0.8~1.2mol/L, more preferably 1~1.1mol/L；
The amount ratio of sample and hydrochloric acid solution after the calcining is preferably 1g: (150~180) mL, more preferably 1g: (160~170)
mL；The temperature of the reaction is preferably 25~50 DEG C, more preferably 30~40 DEG C；The time of the reaction is preferably 1~1.5h.
The present invention also provides a kind of silica-base material with diatomite porous structure, preparation methods provided by the present invention
It is prepared.
The present invention also provides a kind of lithium ion battery negative materials, have diatomite porous knot including of the present invention
The silica-base material of structure.
The present invention provides a kind of silica-base material with diatomite porous structure and its preparation method and application, the present invention
The preparation method of offer is calcined so that included in obtained silicon substrate by selecting magnesium alloy powder and diatomite mixing and ball milling
Carbon and element silicon and do not contain oxygen element, and the silicon substrate has diatomite porous structure, hollow and be evenly distributed, pattern one
It causes, size is controllable (30~100 μm)；So that the lithium battery of the material preparation has higher reversible capacity and excellent follows
Ring stability.In addition, the preparation method is simple, product quality is controllable, has broad application prospects.
It is clearly and completely described below in conjunction with the technical solution of the embodiment of the present invention, it is clear that described implementation
Example is only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's all other embodiments obtained without making creative work belong to the model that the present invention protects
It encloses.
Embodiment 1
In typical preparation process, weigh 1.2g AZ31 magnesium chips and add in spheroidal graphite tank, be filled under the conditions of argon gas, rotating speed
600rpm, time 10h；The diatomite for weighing 1.5g purifications is added in above-mentioned ball grinder, is filled under the conditions of argon gas, rotating speed
800rpm, time 0.5h；Mixture is taken out after finishing, is put into vacuum bag and is preserved；1.0g diatomite and magnesium powder mixture are weighed,
It is put into the quartz ampoule after the carbonization treatment of bottom, completes Vacuum Package；Quartz ampoule after Vacuum Package, is put into Muffle furnace, journey
Sequence is warming up to 600 DEG C of used time 10h, 600 DEG C of calcination time 6h, completes magnesium thermit, obtains the sample after magnesium thermit.
The sample 0.6g after magnesium thermit is taken, is added in the 1mol/L HCl solutions of 100mL, 30 DEG C of temperature reacts 1h
Afterwards, after pure water filtration washing 3 times, 60 DEG C of drying 8h obtain the silica-base material with diatomite porous structure.
Obtained silica-base material is detected, the result is shown in Figure 1 and Fig. 2, Fig. 1 have for what the embodiment of the present invention 1 obtained
The SEM figures of the silica-base material of diatomite porous structure, Fig. 2 be the embodiment of the present invention 1 obtain there is diatomite porous structure
The XRD diagram of silica-base material；It will be seen from figure 1 that rotational speed of ball-mill is too fast, structure of diatomite is destroyed, figure it is seen that
Under 600 DEG C of temperature conditionss, not fully, impurity is more for the reduction of silica.
Embodiment 2：
It weighs 1.2g magnesium chips and adds in spheroidal graphite tank, be filled under the conditions of argon gas, rotating speed 600rpm, time 10h；Weigh 1.5g purifications
Diatomite add in above-mentioned ball grinder, be filled under the conditions of argon gas, rotating speed 600rpm, time 0.5h；Mixture is taken out after finishing,
It is put into vacuum bag and preserves；1.0g diatomite and magnesium powder mixture are weighed, is put into the quartz ampoule after the carbonization treatment of bottom, is completed
Vacuum Package；Quartz ampoule after Vacuum Package, is put into Muffle furnace, temperature programming to 700 DEG C of used time 10h, 700 DEG C of calcination times
12h completes magnesium thermit.The sample 0.6g after magnesium thermit is taken, is added in the 1mol/L HCl solutions of 100mL, temperature 30
DEG C, after reacting 1h, after pure water filtration washing 3 times, 60 DEG C of drying 8h obtain the silica-base material with diatomite porous structure.
Obtained silica-base material is detected, the result is shown in Fig. 3 and Fig. 4, Fig. 3 has for what the embodiment of the present invention 2 obtained
The SEM figures of the silica-base material of diatomite porous structure, Fig. 4 be the embodiment of the present invention 2 obtain there is diatomite porous structure
The XRD diagram of silica-base material；From fig. 4, it can be seen that by controlling rotational speed of ball-mill, under the premise of ensureing that structure of diatomite is complete,
Diatomaceous silica is reduced into elemental silicon；From fig. 4, it can be seen that by acid cleaning process, remaining magnesia etc. is reacted
Substance is removed, and remaining substance is the elemental silicon with structure of diatomite.
Embodiment 3
It weighs 1.2g magnesium chips and adds in spheroidal graphite tank, be filled under the conditions of argon gas, rotating speed 600rpm, time 10h；Weigh 1.5g diatoms
Soil/grapheme material is added in above-mentioned ball grinder, is filled under the conditions of argon gas, rotating speed 600rpm, time 0.5h；It takes out after finishing mixed
Object is closed, is put into vacuum bag and preserves；1.0g diatomite/grapheme material and magnesium powder mixture are weighed, is put into bottom carbonization treatment
In quartz ampoule afterwards, Vacuum Package is completed；Quartz ampoule after Vacuum Package, is put into Muffle furnace, temperature programming to 700 DEG C of used times
10h, 700 DEG C of calcination time 12h complete magnesium thermit, obtain the sample after magnesium thermit.
The sample 0.6g after magnesium thermit is taken, is added in the 1mol/L HCl solutions of 100mL, 30 DEG C of temperature reacts 1h
Afterwards, after pure water filtration washing 3 times, 60 DEG C of drying 8h obtain the silica-base material with diatomite porous structure.
Obtained silica-base material is detected, the result is shown in Fig. 5~7, Fig. 5 has silicon for what the embodiment of the present invention 3 obtained
The SEM figures of the silica-base material of diatomaceous earth porous structure, Fig. 6 are the silicon with diatomite porous structure that the embodiment of the present invention 3 obtains
The EDS elemental analysis results of sill；Fig. 7 is the silicon substrate with diatomite porous structure that the embodiment of the present invention 3 obtains
The BET characterization results of material.From fig. 5, it can be seen that the silica-base material pattern with diatomite porous structure that the present invention obtains
Structural integrity；As seen in Figure 6, the element in silica-base material of the present invention only includes carbon and silicon, and is distributed equal
Even, pattern is complete, and as seen in Figure 7, elemental silicon/carbon composite of structure of diatomite has porous structure, specific surface
Product is big, up to 25m2/ g is conducive to the promotion of chemical property.
Embodiment 4
The chemical property of the silica-base material of diatomite porous structure
Respectively lithium electrical testing is carried out using the material of embodiment 2~3 as test material
The preparation of electrode and battery assembling
Silica-base material prepared by Example is mixed with conductive black and sodium carboxymethylcellulose, and is equably coated in copper foil
On；The copper foil for having applied slurry is put into vacuum drying chamber, dry 12h, is subsequently cooled to room temperature at a temperature of 80 DEG C, takes out copper
Paper tinsel；Copper foil is struck out to the electrode slice of several a diameter of 14mm, weighs the quality of each disk, splitting installs, and takes glove box to
The middle cathode as battery.
The negative plate prepared is put into spare in the glove box full of argon gas；In glove box, first anode cover is placed on
Bottom.Negative plate is put into anode cover middle, instills electrolyte (1M LiPF6Solution), then membrane is put above successively, lithium
Piece, gasket, spring leaf, then adding in a certain amount of electrolyte makes it finally cover negative electrode casing full of entire anode cover；It will assembling
Good battery pond sealing machine is pressed and sealed under the pressure of 50Mpa；Take out the rubbish in glove box and the battery organized, electricity
Pond carries out electrochemical property test after placing for 24 hours fully activation.
For test result as shown in Fig. 8~Figure 11, Fig. 8 is that the volt-ampere of lithium battery prepared by silica-base material of the present invention follows
Ring graph, wherein, sweep speed 0.1mVs-1, scanning voltage scope is 0.01~2V.Fig. 9 is silicon of the present invention
The electrochemistry capacitance test result of lithium battery prepared by sill, Figure 10 are lithium battery prepared by silica-base material of the present invention
Cyclical stability test result, wherein, current density be 100mA g-1, charge and discharge blanking voltage is 0.01-2.0V.Figure 11 is
The electrochemical impedance spectroscopy of lithium battery prepared by silica-base material of the present invention；In addition, the elemental silicon in Fig. 8, Figure 10 and Figure 11
Material refers to the data result of the silica-base material of embodiment 2；Silicon substrate/grapheme material refers to the silicon substrate that embodiment 3 obtains
The data result of material.
Show that silica-base material prepared by embodiment 3 can be effective as lithium cell cathode material by electrochemical test data
To alleviate volume expansion, improve electric conductivity, the cycle performance of material, the transmission rate of lithium ion and electronics is also improved,
Its chemical property is better than the silicon materials of existing structure of diatomite, and charge and discharge specific volume is respectively 1787mAh g-1With 1357mAh g-1；And the cyclical stability of the lithium battery is preferable, after cycling 100 times, charge and discharge specific volume is 805mAh g-1, and capacity retention ratio reaches
45%.
The explanation of above example is only intended to help to understand method and its core concept of the invention.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Several improvement and modification, these improvement and modification are also fallen into the protection domain of the claims in the present invention.
Claims (10)
1. a kind of preparation method of the silica-base material with diatomite porous structure, including：
1) by magnesium alloy powder and the material mixing and ball milling of containing diatomite, mixture is obtained；
2) mixture for obtaining step 1) is calcined, the sample after being calcined；
3) sample after calcining and hydrochloric acid solution are reacted, obtains the silica-base material with diatomite porous structure.
2. preparation method according to claim 1, which is characterized in that the magnesium alloy powder for AZ31 magnesium alloy powders,
AM41 magnesium alloy powders, ZK61 magnesium alloy powders or AS41 magnesium alloy powders.
3. preparation method according to claim 1, which is characterized in that the grain size of the magnesium alloy powder is 40~100 μm.
4. preparation method according to claim 1, which is characterized in that the material of the containing diatomite is diatomite or diatom
The composite material of soil and graphene.
5. preparation method according to claim 1, which is characterized in that the rotating speed of mixing and ball milling is 500 in the step 1)
~650rpm.
6. preparation method according to claim 1, which is characterized in that the magnesium alloy powder and the material of the containing diatomite
The mass ratio of material is 4: (4.5~6).
7. preparation method according to claim 1, which is characterized in that the temperature of calcining is 650~850 in the step 2)
℃。
8. preparation method according to claim 1, which is characterized in that the concentration of the hydrochloric acid solution is 0.8~1.2mol/
L。
9. a kind of silica-base material with diatomite porous structure, as the preparation method system described in claim 1~8 any one
It is standby to obtain.
10. a kind of lithium ion battery negative material is prepared including the preparation method described in claim 1~8 any one
The silica-base material with diatomite porous structure.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102208636A (en) * | 2011-05-12 | 2011-10-05 | 北京科技大学 | Method for preparing porous silicon/carbon composite material by using diatomite as raw material and application |
| CN105845911A (en) * | 2016-05-15 | 2016-08-10 | 东北电力大学 | Method for preparing porous silicon carbon nanotube composite negative electrode material of lithium ion battery by diatomite |
| CN106532008A (en) * | 2016-12-22 | 2017-03-22 | 东北电力大学 | Method for preparing porous silicon/graphene composite lithium ion battery anode material by using diatomite as raw material |
| CN106602022A (en) * | 2016-12-24 | 2017-04-26 | 东北电力大学 | Method for preparing porous silicon/TiO2 composite negative electrode material by taking diatomite as raw material |
-
2017
- 2017-12-15 CN CN201711347938.0A patent/CN108110239A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102208636A (en) * | 2011-05-12 | 2011-10-05 | 北京科技大学 | Method for preparing porous silicon/carbon composite material by using diatomite as raw material and application |
| CN105845911A (en) * | 2016-05-15 | 2016-08-10 | 东北电力大学 | Method for preparing porous silicon carbon nanotube composite negative electrode material of lithium ion battery by diatomite |
| CN106532008A (en) * | 2016-12-22 | 2017-03-22 | 东北电力大学 | Method for preparing porous silicon/graphene composite lithium ion battery anode material by using diatomite as raw material |
| CN106602022A (en) * | 2016-12-24 | 2017-04-26 | 东北电力大学 | Method for preparing porous silicon/TiO2 composite negative electrode material by taking diatomite as raw material |
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