CN107634190A - A kind of method that silica and carbon composite are prepared by high-temperature heat treatment - Google Patents
A kind of method that silica and carbon composite are prepared by high-temperature heat treatment Download PDFInfo
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- CN107634190A CN107634190A CN201710693121.2A CN201710693121A CN107634190A CN 107634190 A CN107634190 A CN 107634190A CN 201710693121 A CN201710693121 A CN 201710693121A CN 107634190 A CN107634190 A CN 107634190A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses the nano composite material of a kind of silica and carbon, it is characterized in that, the material is formed by carbon coating nano SiO 2 particle is compound, wherein silica grain size is 10 30nm, carbon layers having thicknesses are 1 10nm, and the mass percent of silica and carbon is in the composite：(0.5~0.8):The nanocomposite applications of (0.5~0.2), the silica and carbon are in negative electrode of lithium ion battery.Present invention simultaneously provides a kind of method that above-mentioned silica and carbon composite are prepared by high-temperature heat treatment.
Description
Technical field
The present invention relates to a kind of silica and carbon nano-composite material and high-temperature heat treatment preparation method, belong to lithium ion
Secondary battery electrode material field.
Background technology
In recent years, with the fast development of the portable electric appts such as mobile phone, notebook computer, and electric automobile field
Active demand so that the lithium ion battery of research and development high-energy-density turns into domestic and international study hotspot.Answered as current
With wide lithium cell negative pole carbon material, its theoretical specific capacity is low, in complete embedding lithium state (LiC6) when capacity be only 372mAh/
G, while the problem of with organic solvent compatibilities difference also be present, these all make it that carbon material is difficult to meet high power capacity, high-power lithium
The development of electric negative pole.
The theoretical specific capacity of silicon is 4200mAh/g, is capacity highest in all alloying storage elemental lithiums.The voltage of silicon is put down
Platform is~0.4V, slightly above graphite, therefore the possibility of surface analysis lithium is small in quick embedding lithium and low temperature process of intercalation, safety
Property is higher.But silicium cathode can produce huge volumetric expansion (~300%) in electrochemical reaction process, very strong machinery is formed
Stress, cause electrode material to crush, efflorescence, or even depart from copper current collector, cause big irreversible capacity and rapid capacity
Decay.In addition, the intrinsic conductivity of silicon is 6.7 × 10-4Scm-1, poorly conductive.Compared with silicon, earth silicon material tool
There is higher theoretical specific capacity (~1965mAh/g), can be reacted when being used as lithium cell negative pole in first circle discharge process with metal Li
Generate Li2O and Li4SiO4Inert fraction, these inert materials are not involved in electrochemical reaction, are caused caused by irreversible capacity
Reason, but it is evenly distributed in electrode material, is advantageous to buffer body during earth silicon material removal lithium embedded to a certain extent
Product expansion.Therefore, the volume expansion ratio silicon materials of earth silicon material are smaller, and this also causes earth silicon material several recently
Year obtains extensive concern.
The research of earth silicon material, mostly around two problems expansion of its volumetric expansion of solution and poorly conductive.Typically
For prepare nano oxidized silicon materials, make material that there is high mechanical strength, can reduce the influence of volumetric expansion, or design is all kinds of
Hollow, porous nanobelt, nanotube etc., cushion space is provided for volumetric expansion；Furthermore using with the compound preparation of carbon material
Composite, improve silica poorly conductive the problem of.The design of same different nanostructureds, or ion and electronics
Transmission channel is provided, so as to reinforcing material electric conductivity.
Prepare silica and use organic silicon source mostly, such as tetraethyl orthosilicate, its toxicity is high, big to body harm；Respectively
The design of kind oxidation silicon nanostructure, preparation technology are complicated, it is desirable to which strict, yield is also little, limits the production of futurity industry metaplasia
Possibility；Also, generally compound also fairly simple with carbon material, carbonization treatment temperature is not high.Using simple chemical precipitation
Method prepares siliconoxide precursor and realizes carbon coating structure, then makes material in a higher temperature by high-temperature heat treatment means
Spend and carbonization is calcined under environment, finally realize the composite construction of carbon-coated nano silica dioxide granule, not only material overall structure is steady
Calmly, a yield is big, and carbon material electric conductivity is higher after high-temperature process, is the effective of lifting silica material chemical property
One of method.
The content of the invention
It is an object of the invention to provide a kind of method that high-temperature heat treatment prepares silica and carbon composite.This is compound
Material has good stable circulation performance as lithium ion battery negative material, has a extensive future, and preparation method is simple, behaviour
It is few to make process, can mass production.The present invention is to be realized by the following technical programs,
A kind of nano composite material of silica and carbon, it is characterised in that the material is received by carbon coating silica
The compound composition of rice grain, wherein silica grain size are 10-30nm, carbon layers having thicknesses 1-10nm, in the composite
The mass percent of silica and carbon is：(0.5~0.8):The nano composite material of (0.5~0.2), the silica and carbon
Applied to negative electrode of lithium ion battery.
Present invention simultaneously provides a kind of method that above-mentioned silica and carbon composite are prepared by high-temperature heat treatment, its
It is characterised by comprising the following steps：
(1) is reacted using non-hydrate sodium metasilicate as silicon source using chemical precipitation, by non-hydrate sodium metasilicate, absolute ethyl alcohol, is gone
Ionized water and concentrated hydrochloric acid mol ratio are (12~15)：(32~36)：(886~892)：(320~325) count, silicon source is dissolved in second
Alcohol is with water mixed solution, quick stirring addition concentrated hydrochloric acid, after standing a period of time, obtaining colloidal mixture；Use deionized water
Jelly is repeatedly rinsed, it is in neutrality to make mixed solution, uniform through ultrasonic disperse, does carbon source with dopamine hydrochloride, by silicon source most
The SiO obtained eventually2It is (0.8~1.2) with dopamine mass ratio：(0.3~0.6) count, under Tris-HCl buffer conditions, even
Continuous stirring carries out dopamine oxidative polymerization, by washing centrifugation, drying and grinding, obtains mixed-powder.
(2) mix powder made from step (1) is laid in quartzy Noah's ark, is placed in pipe by after crossing 100-300 mesh sieves
Calcined formula stove flat-temperature zone：With N2, He and a kind of gas in Ar or mixed gas as inert gas source, first using flow as
200-400mL/min is passed through inert gas 10-30min to drain air in tube；Again using Ar as protection gas, gas flow is consolidated
It is set to 50-200mL/min, 400 DEG C is warming up to 1-2 DEG C/min programming rate, insulation 3h carries out the cracking of poly-dopamine, then
1100 DEG C are warming up to 5-10 DEG C/min heating rates, insulation 2h is carbonized, and is reacted after terminating with room temperature is furnace-cooled to, is obtained carbon
Coated silica nano composite material.
The present invention has advantages below：The present invention is that silicon source prepares silica using non-hydrate sodium metasilicate cheap and easy to get
With the nano composite material of carbon, cost is cheap, and course of reaction is simple, controllability is strong.Silica is compound uniformly with carbon, dispersiveness
Good, overall structure is stable, and excellent performance has good specific capacity and cycle performance for negative electrode of lithium ion battery,
Remain to keep more than 542mAh/g specific capacity under 100mA/g current density after circulating 90 times.
Brief description of the drawings
Fig. 1 is that the obtained silica after 1100 DEG C of high-temperature process of the embodiment of the present invention 1 shines with carbon composite SEM
Piece.From this view it is apparent that the pattern of the silica and carbon composite under low power.
Fig. 2 is that the obtained silica after 1100 DEG C of high-temperature process of the embodiment of the present invention 1 shines with carbon composite TEM
Piece.From this view it is apparent that the pattern of silica and carbon composite.
Fig. 3 is the obtained silica after 1100 DEG C of high-temperature process of the embodiment of the present invention 1 and carbon composite HRTEM
Photo.From this view it is apparent that the size of silica dioxide granule.
Fig. 4 is the obtained silica after 1100 DEG C of high-temperature process of the embodiment of the present invention 1 and carbon composite XRD
Spectrum.
Fig. 5 is the obtained silica after 1100 DEG C of high-temperature process of the embodiment of the present invention 1 and carbon composite Raman
Collection of illustrative plates.
Fig. 6 is the lithium of the obtained silica and carbon composite after 1100 DEG C of high-temperature process of the embodiment of the present invention 1
The charge-discharge performance figure of ion battery negative pole.
Embodiment
The particular content of the present invention is described as follows with reference to specific embodiment：
Embodiment 1：
3.784g non-hydrate sodium metasilicates are weighed, are dissolved in the mixed solution of 16mL deionized waters and 2mL ethanol, to stir speed
Spend 300r/min magnetic stirring apparatus, stirring and dissolving wiring solution-forming, the then ultrasonic device ultrasound 15min using power as 400W again,
It is well mixed.Mixed liquor is placed on mixing speed 400r/min magnetic stirring apparatus and quickly stirred, is rapidly added thereto
10mL concentrated hydrochloric acids, continue to stop after stirring 10min, normal temperature is stood.After approximately passing through 3-4h, mixed solution is changed into gluey, adds
200-300mL deionized waters wash away unnecessary hydrochloric acid, and repeated washing 6 times, in neutrality, then adds 50mL into solution and gone to mixed liquor
Ionized water and 15mL ethanol, the ultrasonic device ultrasound 60-90min using power as 400W, are uniformly dispersed.Take 1mL concentration for 1mol/L,
The Tris-HCl buffer solutions that PH is 8.8 add mixed liquor, after being well mixed, 200mg dopamine hydrochlorides are added, with 300r/min
Speed magnetic agitation 24h, obtain dark-brown mixed liquor, washing through 3 deionized waters and 3 alcohol, after centrifugation, in 60 DEG C
12h is dried in constant temperature oven, grinds and powder is made.Powder is placed in corundum Noah's ark, is put into tube furnace, is passed through 200mL/min
Ar inert gases drain air after, continue to be passed through 100mL/min Ar inert gases, first with 2 DEG C/min programming rate liter
Temperature is to 400 DEG C, and insulation 3h carries out the cracking of poly-dopamine, then is warming up to 1100 DEG C with 5 DEG C/min programming rate, and insulation 2h enters
Row carbonization, reaction are cooled to room temperature under Ar atmosphere protections after terminating, obtain calcined product, i.e., silica and carbon is nano combined
Material.
0.08g silica and carbon composite, 0.0171g conductive black, 0.1714g PVDF mixing is equal
Even, stirring, which is made slurry and is coated uniformly in copper foil current collector, is used as cathode of lithium battery, with 1M LiPF6In containing volume ratio be
1:1:1 EC/DMC/DEC using lithium metal as positive pole, is assembled into half-cell, its electric current in 100mA/g is close as electrolyte
The lower circle of circulation 100 of degree remains to keep 542mAh/g or so specific capacity, as shown in Figure 6.
Embodiment 2：
5g non-hydrate sodium metasilicates are weighed, are dissolved in 15mL deionized waters, with mixing speed 300r/min magnetic stirring apparatus,
Stirring and dissolving wiring solution-forming, then the ultrasonic device ultrasound 15min using power as 400W again, is well mixed.Mixed liquor is placed in and stirred
Mix and quickly stirred on speed 400r/min magnetic stirring apparatus, be rapidly added 10mL concentrated hydrochloric acids thereto, continue after stirring 10min
Stop, normal temperature is stood.After approximately passing through 3-4h, mixed solution is changed into gluey, adds 200-300mL deionized waters and washes away unnecessary salt
Acid, repeated washing 6 times to mixed liquor is in neutrality, then 50mL deionized waters and 15mL ethanol are added into solution, using power as
400W ultrasonic device ultrasound 60-90min, is uniformly dispersed.It is that the Tris-HCl buffer solutions that 1mol/L, PH are 8.8 add to take 1mL concentration
Enter mixed liquor, after being well mixed, add 200mg dopamine hydrochlorides, with 300r/min speed magnetic agitation 24h, obtain depth
Brown mixture, after the washing, centrifugation through 3 deionized waters and 3 alcohol, 12h, grinding system are dried in 60 DEG C of constant temperature ovens
Obtain powder.Powder is placed in corundum Noah's ark, is put into tube furnace, be passed through 200mL/min Ar inert gases drain air after, after
The continuous Ar inert gases for being passed through 100mL/min, 400 DEG C first are warming up to 2 DEG C/min programming rate, insulation 3h carries out poly- DOPA
The cracking of amine, then 1100 DEG C are warming up to 5 DEG C/min programming rate, insulation 2h is carbonized, and is reacted after terminating in Ar atmosphere
It is cooled to room temperature under protection, obtains the nano composite material of calcined product, i.e. silica and carbon.
Embodiment 3：
1.892g non-hydrate sodium metasilicates are weighed, are dissolved in the mixed solution of 16mL deionized waters and 2mL ethanol, to stir speed
Spend 300r/min magnetic stirring apparatus, stirring and dissolving wiring solution-forming, the then ultrasonic device ultrasound 15min using power as 400W again,
It is well mixed.Mixed liquor is placed on mixing speed 400r/min magnetic stirring apparatus and quickly stirred, is rapidly added thereto
10mL concentrated hydrochloric acids, continue to stop after stirring 10min, normal temperature is stood.After approximately passing through 3-4h, mixed solution is changed into gluey, adds
200-300mL deionized waters wash away unnecessary hydrochloric acid, and repeated washing 6 times, in neutrality, then adds 50mL into solution and gone to mixed liquor
Ionized water and 15mL ethanol, the ultrasonic device ultrasound 60-90min using power as 400W, are uniformly dispersed.Take 1mL concentration for 1mol/L,
The Tris-HCl buffer solutions that PH is 8.8 add mixed liquor, after being well mixed, 200mg dopamine hydrochlorides are added, with 300r/min
Speed magnetic agitation 24h, obtain dark-brown mixed liquor, washing through 3 deionized waters and 3 alcohol, after centrifugation, in 60 DEG C
12h is dried in constant temperature oven, grinds and powder is made.Powder is placed in corundum Noah's ark, is put into tube furnace, is passed through 200mL/min
Ar inert gases drain air after, continue to be passed through 100mL/min Ar inert gases, first with 2 DEG C/min programming rate liter
Temperature is to 400 DEG C, and insulation 3h carries out the cracking of poly-dopamine, then is warming up to 1100 DEG C with 5 DEG C/min programming rate, and insulation 2h enters
Row carbonization, reaction are cooled to room temperature under Ar atmosphere protections after terminating, obtain calcined product, i.e., silica and carbon is nano combined
Material.
Embodiment 4：
1.892g non-hydrate sodium metasilicates are weighed, are dissolved in the mixed solution of 8mL deionized waters and 1mL ethanol, to stir speed
Spend 300r/min magnetic stirring apparatus, stirring and dissolving wiring solution-forming, the then ultrasonic device ultrasound 15min using power as 400W again,
It is well mixed.Mixed liquor is placed on mixing speed 400r/min magnetic stirring apparatus and quickly stirred, is rapidly added thereto
10mL concentrated hydrochloric acids, continue to stop after stirring 10min, normal temperature is stood.After approximately passing through 3-4h, mixed solution is changed into gluey, adds
200-300mL deionized waters wash away unnecessary hydrochloric acid, and repeated washing 6 times, in neutrality, then adds 50mL into solution and gone to mixed liquor
Ionized water and 15mL ethanol, the ultrasonic device ultrasound 60-90min using power as 400W, are uniformly dispersed.Take 1mL concentration for 1mol/L,
The Tris-HCl buffer solutions that PH is 8.8 add mixed liquor, after being well mixed, 200mg dopamine hydrochlorides are added, with 300r/min
Speed magnetic agitation 24h, obtain dark-brown mixed liquor, washing through 3 deionized waters and 3 alcohol, after centrifugation, in 60 DEG C
12h is dried in constant temperature oven, grinds and powder is made.Powder is placed in corundum Noah's ark, is put into tube furnace, is passed through 200mL/min
Ar inert gases drain air after, continue to be passed through 100mL/min Ar inert gases, first with 2 DEG C/min programming rate liter
Temperature is to 400 DEG C, and insulation 3h carries out the cracking of poly-dopamine, then is warming up to 1100 DEG C with 5 DEG C/min programming rate, and insulation 2h enters
Row carbonization, reaction are cooled to room temperature under Ar atmosphere protections after terminating, obtain calcined product, i.e., silica and carbon is nano combined
Material.
Claims (2)
1. the nano composite material of a kind of silica and carbon, it is characterised in that the material is by carbon coating silica nanometer
Particles dispersed is formed, and wherein silica grain size is 10-30nm, carbon layers having thicknesses 1-10nm, two in the composite
The mass percent of silica and carbon is：(0.5~0.8):The nano composite material of (0.5~0.2), the silica and carbon should
For negative electrode of lithium ion battery.
A kind of 2. method that silica and carbon composite are prepared by high-temperature heat treatment, it is characterised in that including following step
Suddenly：
(1) is reacted using non-hydrate sodium metasilicate as silicon source using chemical precipitation, by non-hydrate sodium metasilicate, absolute ethyl alcohol, deionization
Water and concentrated hydrochloric acid mol ratio are (12~15)：(32~36)：(886~892)：(320~325) count, by silicon source be dissolved in ethanol with
In water mixed solution, quick stirring adds concentrated hydrochloric acid, after standing a period of time, obtains colloidal mixture；It is multiple with deionized water
Jelly is rinsed, it is in neutrality to make mixed solution, uniform through ultrasonic disperse, and carbon source is done with dopamine hydrochloride, final by silicon source
The SiO arrived2It is (0.8~1.2) with dopamine mass ratio：(0.3~0.6) count, under Tris-HCl buffer conditions, continuously stir
Mix and carry out dopamine oxidative polymerization, by washing centrifugation, drying and grinding, obtain mixed-powder.
(2) mix powder made from step (1) is laid in quartzy Noah's ark, is placed in tube furnace by after crossing 100-300 mesh sieves
Calcined flat-temperature zone：With N2, He and a kind of gas in Ar or mixed gas as inert gas source, first using flow as 200-
400mL/min is passed through inert gas 10-30min to drain air in tube；Again using Ar as protection gas, gas flow is fixed as
50-200mL/min, 400 DEG C being warming up to 1-2 DEG C/min programming rate, insulation 3h carries out the cracking of poly-dopamine, then with 5-
10 DEG C/min heating rates are warming up to 1100 DEG C, and insulation 2h is carbonized, and is reacted after terminating with room temperature is furnace-cooled to, is obtained carbon coating
Silicon dioxide nano composite material.
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Cited By (5)
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| CN108689715A (en) * | 2018-04-18 | 2018-10-23 | 山东国瓷功能材料股份有限公司 | A kind of aluminium nitride powder and preparation method thereof |
| CN110828818A (en) * | 2019-09-29 | 2020-02-21 | 郑州大学 | Preparation method and application of carbon-coated manganese selenide hollow cubic three-dimensional material |
| CN112452355A (en) * | 2020-12-10 | 2021-03-09 | 浙江海洋大学 | Preparation method of carbon material catalyst applied to styrene preparation |
| CN113809296A (en) * | 2021-09-08 | 2021-12-17 | 生态环境部华南环境科学研究所 | Porous silicon-carbon composite material capable of reducing carbon emission and preparation method thereof |
| CN113921794A (en) * | 2021-10-11 | 2022-01-11 | 福建蓝海黑石新材料科技有限公司 | Silicon-carbon composite material and preparation method and application thereof |
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| CN110828818B (en) * | 2019-09-29 | 2021-03-19 | 郑州大学 | Preparation method and application of carbon-coated manganese selenide hollow cubic three-dimensional material |
| CN112452355A (en) * | 2020-12-10 | 2021-03-09 | 浙江海洋大学 | Preparation method of carbon material catalyst applied to styrene preparation |
| CN113809296A (en) * | 2021-09-08 | 2021-12-17 | 生态环境部华南环境科学研究所 | Porous silicon-carbon composite material capable of reducing carbon emission and preparation method thereof |
| CN113809296B (en) * | 2021-09-08 | 2022-08-30 | 生态环境部华南环境科学研究所 | Porous silicon-carbon composite material and preparation thereof |
| CN113921794A (en) * | 2021-10-11 | 2022-01-11 | 福建蓝海黑石新材料科技有限公司 | Silicon-carbon composite material and preparation method and application thereof |
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