CN102881872A - Method for synthesizing silicon oxide/carbon nanotube membranous lithium ion battery anode material by one step by utilizing chemical vapor deposition method - Google Patents
Method for synthesizing silicon oxide/carbon nanotube membranous lithium ion battery anode material by one step by utilizing chemical vapor deposition method Download PDFInfo
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Abstract
The invention discloses a method for synthesizing a silicon oxide/carbon nanotube membranous lithium ion battery anode material by one step by utilizing a chemical vapor deposition method. The method comprises the following steps of: weighing 1 to 16.5 mole percent of silicon source, 82 to 98.7 mole percent of carbon source, 0.2 to 1.0 mole percent of catalyst and 0.1 to 0.5 mole percent of accelerator to prepare a precursor solution; and raising the temperature of a tube furnace to 600 to 1,200 DEG C under the protection of an inert atmosphere, stopping introducing an inert gas, regulating hydrogen to be 400 to 1,000sccm, injecting the precursor solution into the tube furnace, and performing high-temperature reaction to prepare the silicon oxide/carbon nanotube membranous lithium ion battery anode material. The method has the characteristics of simple operation process, convenience and product shape uniformity, and the product has high lithium battery specific capacity and high cycling stability.
Description
Technical field
The invention relates to nano composite material, particularly a kind of chemical gas-phase method one-step synthesis silica/carbon nano-tube (SiO
2/ CNTs) membranaceous lithium ion battery negative material.
Background technology
Lithium ion battery is widely used at aspects such as mancarried electronic aid, electric automobiles because it has the operating voltage height, has extended cycle life, the advantage such as environmentally friendly, has also obtained people and has more and more paid close attention to.The most frequently used lithium ion battery negative material is graphite at present, but graphite cathode material theoretical specific capacity lower (372mAh/g) has limited its application in the high-energy-density field.Therefore, the negative material that some theoretical capacities are higher such as Sn base, Si sill also are developed gradually and pay attention to.Sn base, Si sill be during as lithium cell negative pole, in the charge and discharge process because of Li
+Embedding-Tuo embedding meeting produce very large change in volume (about 300%), cause the pulverizing of electrode material and cave in the final serious performance that reduces battery.And SiO
2During as lithium cell negative pole, the Li that generates in the charge and discharge process
2O and Li
4SiO
4Can play cushioning effect, alleviate change in volume.Crystal SiO
2Structure and chemical property are highly stable, usually lithium ion are shown as inertia.It is reported unbodied SiO
2Can be used as lithium ion battery negative material.Carbon nano-tube has good mechanical performance, the electric conductivity of excellence and high specific area, preparation SiO
2/ CNTs composite material can improve SiO
2As the electric conductivity of lithium cell negative pole material, huge change in volume in buffering embedding lithium-Tuo lithium process, thus improve SiO
2The lithium electrical property of battery during as negative material.In addition, preparation nanometer SiO
2Can shorten Li
+With the transfer distance of electronics, thereby improve the performance of battery.
At present, preparation SiO
2The method of/CNTs mainly is solwution method, mostly adopts SiO
2Powder and carbon source or CNTs and silester are primary raw material.Liquid preparation methods SiO
2Through two steps or multistep operation, process is more loaded down with trivial details, and the CNTs in the product is difficult to be uniformly dispersed mostly for/CNTs.
Summary of the invention
The objective of the invention is for the deficiency of technology now, a kind of quickly and easily synthetic SiO is provided
2The method of/CNTs lithium cell negative pole material.The present invention adopts siliceous organic substance and carbonaceous organic material respectively as silicon source and carbon source, chemical gas-phase method one-step synthesis SiO
2The membranaceous lithium cell negative pole material of/CNTs.
The present invention is achieved by following technical solution.
The method of the membranaceous lithium ion battery negative material of a kind of chemical gaseous phase one-step synthesis silica/carbon nano-tube, concrete steps are as follows:
(1) configuration precursor mixed solution
Be 1～16.5% silicon source, 82～98.7% carbon sources, 0.2～1.0% catalyst, 0.1～0.5% promoter by raw material components and mole percent level thereof, take by weighing silicon source, carbon source, catalyst and promoter, ultrasonic mixing obtains precursor solution;
Described silicon source is any one or the multiple mixture in silester, silane coupler and the dimethicone;
Described carbon source is any one or the multiple mixture in carbonaceous organic material ethanol, acetone, cyclohexane, ether, benzene and the n-hexane;
Described catalyst is one or more the mixture in ferrocene, ferric oxalate, nickel acetate, cobalt acetate and the ammonium molybdate;
Described promoter is one or both the mixture in thiophene and the water;
(2) high temperature synthetic reaction
Tube furnace is warmed up to 600～1200 ℃ under inert atmosphere, stop logical inert gas, inputting hydrogen, the adjusting hydrogen flowing quantity is 400～1000sccm, the mixing precursor solution that obtains in the step (1) is injected tube furnace with the speed of 2～15ml/h, make the membranaceous lithium ion battery negative material of silica/carbon nano-tube through pyroreaction;
Inert gas is wherein one or both the gaseous mixture of nitrogen, argon gas.
Preferred synthesis temperature scope is 1000～1200 ℃ in the described step (2).
The preferred charge velocity that mixes precursor solution is 6～12ml/h in the described step (2).
Preferred hydrogen flowing quantity is 500～800sccm in the described step (2).
Beneficial effect of the present invention is take siliceous and carbonaceous organic material as primary raw material, the uniform SiO of vapor phase method one-step synthesis microstructure
2The membranaceous lithium ion battery negative material of/CNTs.This method operating process is simple and convenient, and the CNTs in the product is woven into mutually netted, and has obtained the SiO of nano-scale
2The performance test results shows that product has higher specific capacity and good cycle performance.
Description of drawings
Fig. 1 is the SiO of embodiment 1 preparation
2/ CNTs film X-ray diffraction spectrogram;
Fig. 2 is the SiO of embodiment 1 preparation
2The transmission microscopy photo of/CNTs film;
Fig. 3 is the SiO of embodiment 1 preparation
2The high power transmission microscopy photo of CNTs in the/CNTs film;
Fig. 4 is the SiO of embodiment 1 preparation
2The specific capacity of/CNTs film-cycle performance curve;
Fig. 5 is the SiO of embodiment 2 preparations
2The flying-spot microscope photo of/CNTs film;
Fig. 6 is the SiO of embodiment 2 preparations
2The transmission microscopy photo of/CNTs film.
Embodiment
The present invention is further illustrated below by embodiment, and raw materials used being of embodiment analyzed pure raw material, and specific embodiment is as follows.
Embodiment 1
(1) take by weighing silester (TEOS) 5.437g, ethanol 12.000g, thiophene 0.110g, ferrocene 0.353g, ultrasonic 30min mixes it, obtains yellow precursor mixed solution.
(2) under argon shield atmosphere, tube furnace is warmed up to 1170 ℃; stop in stove, leading to argon gas; change logical hydrogen; the adjusting hydrogen flowing quantity is 700sccm; after gas is stable; with disposing to such an extent that the mixing precursor solution is transferred in the syringe of 50ml in the step (1), by syringe pump precursor solution is injected reacting furnace, one-step synthesis SiO with the speed of 8ml/h
2/ CNTs lithium cell negative pole material.
The SiO of the present invention's preparation
2/ CNTs composite material, carried out following signs:
Phase characterizes: the phase that adopts Japanese D/max-2500 type X-ray diffractometer to measure product forms.
Morphology characterization: adopt Dutch Tecnai G2-F20 type field transmission electron microscope observation product microscopic appearance.
Performance characterization: adopt NEWARE lithium electrical testing system to carry out the lithium electric performance test (voltage range is 0.005-3.000V) of composite electrode.
Fig. 1 is the SiO of embodiment 1 preparation
2The X-ray diffraction spectrogram of/CNTs film.20-25 ° diffraction maximum is corresponding to (002) crystal face and the SiO of CNT
2, the broadening at peak shows SiO simultaneously
2Be amorphous Si O
244.5 ° diffraction maximum corresponding to (110) crystal face of CNT.
Fig. 2 is the SiO of embodiment 1 preparation
2The transmission microscopy photo of/CNTs film.Thin straight CNTs and CNTs bundle are interweaved and reticulate nanometer SiO
2Be attached to the CNT outer wall and form composite membrane.
Fig. 3 is the SiO of embodiment 1 preparation
2The high power transmission microscopy photo of CNT in the/CNTs film.CNT is few-wall carbon nanotube, and diameter is 3-5nm, and outer wall is attached with a small amount of other forms of carbon.
Fig. 4 is the SiO of embodiment 1 preparation
2The specific capacity of/CNTs film-cycle performance curve.SiO
2The membranaceous lithium cell negative pole material of/CNTs discharged and recharged respectively for 10 weeks when current density is followed successively by 20mA/g, 50mA/g, 100mA/g, reversible specific capacity is respectively 709mAh/g, 494mAh/g, 317mAh/g.Be 200mA/g when current density raises, specific capacity is stable at 106mAh/g after 30 weeks of circulation.When again current density being reverted to 50mA/g, specific capacity also reverts to 445mAh/g, and the SiO of preparation is described
2/ CNTs film has good lithium electricity cycle performance.Along with the rising of current density, the specific capacity of material reduces simultaneously.
(1) take by weighing TEOS 5.446g, ethanol 12.000g, thiophene 0.110g, ferrocene 0.352g, ultrasonic 30min mixes it, obtains yellow precursor mixed solution.
(2) under argon shield atmosphere, tube furnace is warmed up to 1150 ℃; stop in stove, leading to argon gas; change logical hydrogen; the adjusting hydrogen flowing quantity is 700sccm; after gas is stable; with disposing to such an extent that the mixing precursor solution is transferred in the syringe of 50ml in the step (1), by syringe pump precursor solution is injected reacting furnace, one-step synthesis SiO with the speed of 8ml/h
2/ CNTs lithium cell negative pole material.
Fig. 5 is the SiO of embodiment 2 preparations
2The flying-spot microscope photo of/CNTs film.The product uniform microstructure, CNTs is interweaved, a large amount of SiO
2Particle is compound with it, part SiO
2Particle has slight reunion.
Fig. 6 is the SiO of embodiment 2 preparations
2The transmission microscopy photo of/CNTs film.CNT in the product is without specific orientation, and is interlaced, and diameter is about 10-20nm, a large amount of SiO
2Particle mixes with it, SiO
2Be enclosed with minimum dark catalyst Fe particle in the particle.
Embodiment 3
(1) take by weighing TEOS 2.971g, benzene 22.277g, thiophene 0.110g, ferrocene 0.210g, ultrasonic 30min mixes it, obtains yellow precursor mixed solution.
(2) under nitrogen protection atmosphere, tube furnace is warmed up to 600 ℃; stop in stove, leading to nitrogen; change logical hydrogen; the adjusting hydrogen flowing quantity is 400sccm; after gas is stable; with disposing to such an extent that the mixing precursor solution is transferred in the syringe of 50ml in the step (1), by syringe pump precursor solution is injected reacting furnace, one-step synthesis SiO with the speed of 2ml/h
2/ CNTs lithium cell negative pole material.
Embodiment 4
(1) take by weighing TEOS 10.979g, ethanol 12.024g, thiophene 0.135g, ferric oxalate 1.491g, ultrasonic 30min mixes it, obtains yellow precursor mixed solution.
(2) under argon shield atmosphere, tube furnace is warmed up to 1200 ℃; stop in stove, leading to argon gas; change logical hydrogen; the adjusting hydrogen flowing quantity is 1000sccm; after gas is stable; with disposing to such an extent that the mixing precursor solution is transferred in the syringe of 50ml in the step (1), by syringe pump precursor solution is injected reacting furnace, one-step synthesis SiO with the speed of 12ml/h
2/ CNTs lithium cell negative pole material.
Embodiment 5
(1) take by weighing TEOS 0.542g, ethanol 12.000g, thiophene 0.025g, nickel acetate 0.137g, ultrasonic 30min mixes it, obtains yellow precursor mixed solution.
(2) under argon shield atmosphere, tube furnace is warmed up to 1000 ℃; stop in stove, leading to argon gas; change logical hydrogen; the adjusting hydrogen flowing quantity is 900sccm; after gas is stable; with disposing to such an extent that the mixing precursor solution is transferred in the syringe of 50ml in the step (1), by syringe pump precursor solution is injected reacting furnace, one-step synthesis SiO with the speed of 15ml/h
2/ CNTs lithium cell negative pole material.
Embodiment 6
(1) take by weighing TEOS 5.437g, cyclohexane 21.957g, thiophene 0.110g, ferrocene 0.210g, ultrasonic 30min mixes it, obtains yellow precursor mixed solution.
(2) under argon shield atmosphere, tube furnace is warmed up to 800 ℃; stop in stove, leading to argon gas; change logical hydrogen; the adjusting hydrogen flowing quantity is 600sccm; after gas is stable; with disposing to such an extent that the mixing precursor solution is transferred in the syringe of 50ml in the step (1), by syringe pump precursor solution is injected reacting furnace, one-step synthesis SiO with the speed of 6ml/h
2/ CNTs lithium cell negative pole material.
Embodiment 7
(1) take by weighing silane coupler kh5505.779g, ethanol 12.000g, thiophene 0.050g, ferrocene 0.210g, ultrasonic 30min mixes it, obtains yellow precursor mixed solution.
(2) under argon shield atmosphere, tube furnace is warmed up to 1100 ℃; stop in stove, leading to argon gas; change logical hydrogen; the adjusting hydrogen flowing quantity is 800sccm; after gas is stable; with disposing to such an extent that the mixing precursor solution is transferred in the syringe of 50ml in the step (1), by syringe pump precursor solution is injected reacting furnace, one-step synthesis SiO with the speed of 10ml/h
2/ CNTs lithium cell negative pole material.
Above-mentioned description to embodiment is to be convenient to those skilled in the art can understand and apply the invention, and the invention is not restricted to the embodiment here, and various raw materials and various technological parameter that the present invention is cited can both be realized the present invention.Those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (4)
1. the method for the membranaceous lithium ion battery negative material of chemical gaseous phase one-step synthesis silica/carbon nano-tube, concrete steps are as follows:
(1) configuration precursor mixed solution
Be 1～16.5% silicon source, 82～98.7% carbon sources, 0.2～1.0% catalyst, 0.1～0.5% promoter by raw material components and mole percent level thereof, take by weighing silicon source, carbon source, catalyst and promoter, ultrasonic mixing obtains precursor solution;
Described silicon source is any one or the multiple mixture in silester, silane coupler and the dimethicone;
Described carbon source is any one or the multiple mixture in carbonaceous organic material ethanol, acetone, cyclohexane, ether, benzene and the n-hexane;
Described catalyst is one or more the mixture in ferrocene, ferric oxalate, nickel acetate, cobalt acetate and the ammonium molybdate;
Described promoter is one or both the mixture in thiophene and the water.
(2) high temperature synthetic reaction
Tube furnace is warmed up to 600～1200 ℃ under inert atmosphere, stop logical inert gas, inputting hydrogen, the adjusting hydrogen flowing quantity is 400～1000sccm, the mixing precursor solution that obtains in the step (1) is injected tube furnace with the speed of 2～15ml/h, make the membranaceous lithium ion battery negative material of silica/carbon nano-tube through pyroreaction;
Inert gas is wherein one or both the gaseous mixture of nitrogen, argon gas.
2. according to claim 1 the method for the membranaceous lithium ion battery negative material of chemical gas-phase method one-step synthesis silica/carbon nano-tube is characterized in that preferred synthesis temperature scope is 1000～1200 ℃ in the described step (2).
3. according to claim 1 the method for the membranaceous lithium ion battery negative material of chemical gas-phase method one-step synthesis silica/carbon nano-tube is characterized in that the preferred charge velocity that mixes precursor solution is 6～12ml/h in the described step (2).
4. according to claim 1 the method for the membranaceous lithium ion battery negative material of chemical gas-phase method one-step synthesis silica/carbon nano-tube is characterized in that preferred hydrogen flowing quantity is 500～800sccm in the described step (2).
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103531753A (en) * | 2013-09-22 | 2014-01-22 | 天津大学 | Continuous carbon nanotube-titanium dioxide composite membrane/fiber for electrode material |
| CN105448535A (en) * | 2015-11-30 | 2016-03-30 | 天津大学 | Preparation method of metal sulfide/carbon nanotube film super capacitor electrode material |
| CN105789575A (en) * | 2016-03-08 | 2016-07-20 | 北京理工大学 | Silicon dioxide carbon composite negative electrode material, modified silicon dioxide carbon composite negative electrode material and preparation methods and application of silicon dioxide carbon composite negative electrode material and modified silicon dioxide carbon composite negative electrode material |
| CN105895880A (en) * | 2016-05-18 | 2016-08-24 | 河南田园新能源科技有限公司 | Preparation method of silicon dioxide composite material for negative electrode of lithium-ion battery |
| CN106188614A (en) * | 2016-07-12 | 2016-12-07 | 苏州赛福德备贸易有限公司 | CNT SiO2the preparation method of composite |
| CN107623110A (en) * | 2016-07-15 | 2018-01-23 | 微宏动力系统（湖州）有限公司 | Silicon substrate composite negative pole material, preparation method and lithium rechargeable battery |
| CN108624052A (en) * | 2017-03-24 | 2018-10-09 | 天津大学 | A method of improving phenyl siloxane rubber mechanical property |
| CN110518224A (en) * | 2019-09-09 | 2019-11-29 | 厦门大学 | A kind of preparation method of lithium ion battery carbon silicon anode material |
| CN111261849A (en) * | 2018-12-03 | 2020-06-09 | 成都市银隆新能源有限公司 | Method for preparing solid spherical material for negative electrode of lithium ion battery by using microfluidic technology |
| CN112467092A (en) * | 2020-10-23 | 2021-03-09 | 合肥国轩高科动力能源有限公司 | Silicon cathode for lithium ion battery and preparation method thereof |
| CN112938940A (en) * | 2021-03-01 | 2021-06-11 | 浙江清华柔性电子技术研究院 | Preparation method and equipment of silicon-carbon nanotube and silicon-carbon nanotube composite film, silicon-carbon nanotube composite film and lithium battery |
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| CN103531753A (en) * | 2013-09-22 | 2014-01-22 | 天津大学 | Continuous carbon nanotube-titanium dioxide composite membrane/fiber for electrode material |
| CN105448535A (en) * | 2015-11-30 | 2016-03-30 | 天津大学 | Preparation method of metal sulfide/carbon nanotube film super capacitor electrode material |
| CN105448535B (en) * | 2015-11-30 | 2017-10-27 | 天津大学 | The preparation method of metal sulfide/carbon nano-tube film electrode material for super capacitor |
| CN105789575A (en) * | 2016-03-08 | 2016-07-20 | 北京理工大学 | Silicon dioxide carbon composite negative electrode material, modified silicon dioxide carbon composite negative electrode material and preparation methods and application of silicon dioxide carbon composite negative electrode material and modified silicon dioxide carbon composite negative electrode material |
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| CN106188614A (en) * | 2016-07-12 | 2016-12-07 | 苏州赛福德备贸易有限公司 | CNT SiO2the preparation method of composite |
| CN107623110A (en) * | 2016-07-15 | 2018-01-23 | 微宏动力系统（湖州）有限公司 | Silicon substrate composite negative pole material, preparation method and lithium rechargeable battery |
| CN107623110B (en) * | 2016-07-15 | 2022-04-12 | 微宏动力系统（湖州）有限公司 | Silicon-based composite negative electrode material, preparation method and lithium ion secondary battery |
| CN108624052A (en) * | 2017-03-24 | 2018-10-09 | 天津大学 | A method of improving phenyl siloxane rubber mechanical property |
| CN111261849A (en) * | 2018-12-03 | 2020-06-09 | 成都市银隆新能源有限公司 | Method for preparing solid spherical material for negative electrode of lithium ion battery by using microfluidic technology |
| CN111261849B (en) * | 2018-12-03 | 2022-10-21 | 成都市银隆新能源有限公司 | Method for preparing solid spherical material for negative electrode of lithium ion battery by using microfluidic technology |
| CN110518224A (en) * | 2019-09-09 | 2019-11-29 | 厦门大学 | A kind of preparation method of lithium ion battery carbon silicon anode material |
| CN112467092A (en) * | 2020-10-23 | 2021-03-09 | 合肥国轩高科动力能源有限公司 | Silicon cathode for lithium ion battery and preparation method thereof |
| CN112938940A (en) * | 2021-03-01 | 2021-06-11 | 浙江清华柔性电子技术研究院 | Preparation method and equipment of silicon-carbon nanotube and silicon-carbon nanotube composite film, silicon-carbon nanotube composite film and lithium battery |
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Application publication date: 20130116 |