CN103915630A - Molybdenum disulfide/mesoporous carbon composite electrode material as well as preparation method and application thereof - Google Patents
Molybdenum disulfide/mesoporous carbon composite electrode material as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a molybdenum disulfide/mesoporous carbon composite electrode material as well as a preparation method and application thereof. The preparation method comprises the following steps: preparing an oleic acid molecule intercalation molybdenum disulfide precursor through a hydrothermal reaction by adopting oleic acid and sodium oleate as a structure-directing agent and sodium molybdate and thiourea as a molybdenum source and a sulfur source; introducing dopamine into an interlayer by virtue of a chemical reaction of dopamine and oleic acid molecules; self-polymerizing molybdenum disulfide interlayer dopamine to form poly(dopamine) by adopting a tri-block copolymer, polyoxyethylene-polypropylene oxide-polyxyethylene, as a soft template, and then performing a high-temperature carbonization process to prepare the mesoporous carbon-embedded molybdenum disulfide interlayer nano hybrid material. By embedding mesoporous carbon, not only can the interlayer distance of molybdenum disulfide be increased and the re-accumulation of nano-sheets be effectively prevented, but also the electronic conductivity of molybdenum disulfide can be remarkably improved. An electrochemical test result proves that as a lithium ion battery negative material, the molybdenum disulfide/mesoporous carbon composite electrode material has high specific capacity, excellent rate performance and excellent cycling performance, and can be widely applied to the field of lithium ion batteries.
Description
Technical field
The present invention relates to new energy materials field, relate to a kind of lithium ion battery electrode material and its preparation method and application, be specifically related to a kind of nano-hybrid material of mesoporous carbon embedding molybdenum bisuphide interlayer.
Background technology
Lithium ion battery is because it has the advantages such as larger energy density and longer cycle life, make its in the field such as portable electric appts, electric automobile in occupation of consequence more and more.But along with scientific and technological development, people also have higher requirement to the performance of energy storage device lithium ion battery.Electrode material is one of lithium ion battery key issue that need to solve.Material with carbon element, because of its lower cost and longer cycle life, becomes the first-selection of current commercial li-ion cell negative electrode material.But the first charge-discharge efficiency of material with carbon element is low, specific capacity is low, organic solvent embeds altogether etc., and deficiency impels people to continue to study and find the substitute of carbon negative pole material.
In recent years, two-dimensional layer molybdenum bisuphide material comes into one's own day by day as new negative electrode materials for lithium secondary batteries, because molybdenum bisuphide material has the advantages such as energy density is high, cost is low, pollution-free, there is good embedding/de-lithium performance and cyclical stability performance, but its embedding/de-lithium current potential is low compared with metal oxide, under cryogenic conditions, electrochemical reaction speed is slow, and the rate charge-discharge performance of material is undesirable, is one of Main Bottleneck limiting its development.Carry out for molybdenum bisuphide material at present that improved method mainly contains structure optimization and material with carbon element is compound.For example, the people such as Du (Du, G; Guo, Z; Wang, S.; Zeng, R.; Chen, Z.; Liu, H., Chem.Commun.2010,46:1106) by by the individual layer molybdenum disulfide nano sheet of peeling off again stacking can acquisition compared with large interlamellar spacing, discharging and recharging under density of 50mA/g, circulate and after 20 times, still kept the discharge capacity of 750mAh/g.The electron conductivity that molybdenum bisuphide is on the low side, has also limited the raising of its chemical property.The people such as Chen (Chang K.; Chen, W.X., ACS Nano, 2011,5:4720) utilize molybdenum bisuphide/graphene composite material that Cys is prepared as adjuvant to show higher capacity and good cycle performance, under the charging and discharging currents with 100mA/g, the capacity after 100 times that circulates exceedes 1100mAh/g.
Summary of the invention
The object of this invention is to provide a kind of mesoporous carbon and embed molybdenum bisuphide interlayer nano-hybrid material and its preparation method and application, the defect existing to overcome above-mentioned existing electrode material.Mentality of designing is as follows:
Utilize hydro thermal method to prepare the molybdenum bisuphide ultrathin nanometer sheet of oleic acid molecular intercalation, then by the chemical reaction of oleic acid molecular and dopamine, dopamine is introduced to interlayer, dopamine auto polymerization under the effect of dissolved oxygen, make it form poly-dopamine layer at interlayer, high temperature cabonization again, formation mesoporous carbon embeds the nano-hybrid material of molybdenum bisuphide interlayer.In prepared hybrid material, the embedding of carbon-coating has not only expanded molybdenum bisuphide interlamellar spacing, improves the electro-chemical activity utilance of material, and is conducive to improve its conductance, guarantees the power-performance that it is high.
The present invention is achieved by the following technical solutions:
A kind of molybdenum bisuphide/mesoporous carbon composite electrode material, the structure of described combination electrode material is: monatomic carbon-coating is embedded between molybdenum disulfide nano sheet layer equably; Wherein, the diameter of described molybdenum disulfide nano sheet layer is that 200～300nm, thickness are 10～20nm, and the interlamellar spacing of adjacent described molybdenum disulfide nano sheet layer is 0.76～1.04nm.
A preparation method for molybdenum bisuphide/mesoporous carbon composite electrode material, comprises the steps:
(1) 1.5～3.0g enuatrol, 1.0～2.0g sodium molybdate, 0.93～1.86g thiocarbamide are dissolved in the mixed solvent of 15～30ml deionized water, 15～30ml ethanol and 2～40ml oleic acid, be less than 1 to it with nitre acid for adjusting pH value, after stirring, carry out hydro-thermal reaction 24～36h at 140～180 ℃, can be cooled to after room temperature and clean and collecting reaction product;
(2) 0.2～0.6g triblock copolymer polyoxyethylene-poly-oxypropylene polyoxyethylene is dissolved in 200～600ml water, then add 0.25～0.75g tromethamine to stir and obtain cushioning liquid, again the product obtaining in step (1) is scattered in described cushioning liquid to cool to room temperature after ultrasonic 30～90min;
(3) in the end product of step (2), add while stirring 250～500mg dopamine, stirring reaction 3～24h at 10～40 ℃, filters centrifuge washing collecting reaction product;
(4) by the product obtaining in step (3) in inert atmosphere at 600～900 ℃ carburizing reagent 2～4h, can obtain described molybdenum bisuphide/mesoporous carbon composite electrode material.
The structure of described combination electrode material is: monatomic carbon-coating is embedded between molybdenum disulfide nano sheet layer equably; Wherein, the diameter of described molybdenum disulfide nano sheet layer is that 200～300nm, thickness are 10～20nm, and the interlamellar spacing of adjacent described molybdenum disulfide nano sheet layer is 0.76～1.04nm.
The weight ratio of described sodium molybdate and dopamine is 2:1～4:1.
Described inert atmosphere is argon gas.
The application of described molybdenum bisuphide/mesoporous carbon composite electrode material, that is, described combination electrode material is applied to lithium ion battery as negative material.
From above technical scheme and implementation method, molybdenum bisuphide/mesoporous carbon composite electrode material (mesoporous carbon embeds the nano-hybrid material of molybdenum bisuphide interlayer) prepared by the present invention can show excellent chemical property as lithium ion battery negative material.The embedding of carbon-coating (has for example not only expanded molybdenum bisuphide interlamellar spacing, expand 0.98nm to by original 0.64nm), improve the electro-chemical activity utilance of material, and be conducive to improve its conductance, guarantee the power-performance that it is high, be applied in lithium ion battery negative material field and there is excellent high rate performance and cyclical stability.
Accompanying drawing explanation
Fig. 1 is the XRD curve of embodiment 1 product;
Fig. 2 is the transmission electron microscope photo of embodiment 1 product;
Fig. 3 is the Electrochemical results of the prepared product of embodiment 1 as lithium ion battery negative material.
Embodiment
Below in conjunction with drawings and Examples, specific embodiments of the present invention are further described in detail, but should not limit the scope of the invention with this.
Embodiment 1
1.5g enuatrol, 1.0g sodium molybdate, 0.9g thiocarbamide are dissolved in the mixed solvent of 15ml deionized water, 15ml ethanol and 2ml oleic acid, be less than 1 to it with nitre acid for adjusting pH value, stir, at 140 ℃, carry out hydro-thermal reaction 24h, be cooled to after room temperature and clean and collecting reaction product.
0.2g P123 is dissolved in 200ml water, then add 0.25g tromethamine to stir and obtain cushioning liquid, again above-mentioned product is scattered in described cushioning liquid 200ml, cool to room temperature after ultrasonic 30min, add while stirring 250mg dopamine, stirring reaction 3h at 10 ℃, filters centrifuge washing collecting reaction product.
The product obtaining is carried out in argon gas atmosphere to high temperature cabonization, react 2h at 600 ℃ to obtain molybdenum bisuphide/mesoporous carbon composite electrode material, mesoporous carbon embeds the nano-hybrid material of molybdenum bisuphide interlayer.Product X RD curve as shown in Figure 1, the transmission electron microscope photo of product as shown in Figure 2.Wherein, the diameter of molybdenum disulfide nano sheet layer is that 200～300nm, thickness are 10～20nm, and the interlamellar spacing of adjacent molybdenum disulfide nano sheet layer is approximately 0.98nm.
Used as lithium ion battery negative material, adopt CR2016 type button cell to test its chemical property.Fig. 3 is the rate charge-discharge test result figure of material, and as can be seen from the figure, along with the increase of current density, its capacity loss is slower, illustrates that this material has good rate charge-discharge performance.And circulation volume several times under each multiplying power keeps stable, in the time that current density is returned to low range, capacity can well recover, and proves that this material has good cyclical stability.
Embodiment 2
2g enuatrol, 1.5g sodium molybdate, 1.4g thiocarbamide are dissolved in the mixed solvent of 20ml deionized water, 20ml ethanol and 3ml oleic acid, be less than 1 to it with nitre acid for adjusting pH value, stir, carry out hydro-thermal reaction 30h at 160 ℃, be cooled to after room temperature and clean and collecting reaction product.
0.3g P123 is dissolved in 300ml water, then add 0.5g tromethamine to stir and obtain cushioning liquid, again above-mentioned products therefrom is scattered in described cushioning liquid 100ml, cool to room temperature after ultrasonic 60min, add while stirring 350mg dopamine, stirring reaction 16h at 250 ℃, filters centrifuge washing collecting reaction product.
The product obtaining is carried out in argon gas atmosphere to high temperature cabonization, react 34h at 850 ℃ and obtain mesoporous carbon and embed the nano-hybrid material of molybdenum bisuphide interlayer.Electro-chemical test part is with embodiment 1, prepared materials show the experimental result almost identical with embodiment 1.
Embodiment 3
3.0g enuatrol, 2.0g sodium molybdate, 2.0g thiocarbamide are dissolved in the mixed solvent of 30ml deionized water, 30 ethanol and 2ml oleic acid, be less than 1 to it with nitre acid for adjusting pH value, stir, carry out hydro-thermal reaction 36h at 180 ℃, be cooled to after room temperature and clean and collecting reaction product.
0.6g P123 is dissolved in 600ml water, then add 0.75g tromethamine to stir and obtain cushioning liquid, again above-mentioned products therefrom is scattered in described cushioning liquid 200ml, cool to room temperature after ultrasonic 90min, add while stirring 500mg dopamine, stirring reaction 24h at 40 ℃, filters centrifuge washing collecting reaction product.
The product obtaining is carried out in argon gas atmosphere to high temperature cabonization, react 4h at 900 ℃ and obtain mesoporous carbon and embed the nano-hybrid material of molybdenum bisuphide interlayer.Electro-chemical test part is with embodiment 1, prepared materials show the experimental result almost identical with embodiment 1.
The foregoing is only preferred embodiment of the present invention, be not used for limiting practical range of the present invention.Under any, in technical field, have and conventionally know the knowledgeable, without departing from the spirit and scope of the present invention, when doing various variations and retouching, therefore protection scope of the present invention is when being as the criterion with claims institute confining spectrum.
Claims (6)
1. molybdenum bisuphide/mesoporous carbon composite electrode material, is characterized in that, the structure of described combination electrode material is: monatomic carbon-coating is embedded between molybdenum disulfide nano sheet layer equably; Wherein, the diameter of described molybdenum disulfide nano sheet layer is that 200～300nm, thickness are 10～20nm, and the interlamellar spacing of adjacent described molybdenum disulfide nano sheet layer is 0.76～1.04nm.
2. a preparation method for molybdenum bisuphide/mesoporous carbon composite electrode material, is characterized in that, comprises the steps:
(1) 1.5～3.0g enuatrol, 1.0～2.0g sodium molybdate, 0.93～1.86g thiocarbamide are dissolved in the mixed solvent of 15～30ml deionized water, 15～30ml ethanol and 2～40ml oleic acid, be less than 1 to it with nitre acid for adjusting pH value, after stirring, carry out hydro-thermal reaction 24～36h at 140～180 ℃, obtain product;
(2) 0.2～0.6g triblock copolymer polyoxyethylene-poly-oxypropylene polyoxyethylene is dissolved in 200～600ml water, then add 0.25～0.75g tromethamine to stir and obtain cushioning liquid, again the product obtaining in step (1) is scattered in described cushioning liquid to cool to room temperature after ultrasonic 30～90min;
(3) in the end product of step (2), add while stirring 250～500mg dopamine, stirring reaction 3～24h at 10～40 ℃, filters centrifuge washing collecting reaction product;
(4) by the product obtaining in step (3) in inert atmosphere at 600～900 ℃ carburizing reagent 2～4h, can obtain described molybdenum bisuphide/mesoporous carbon composite electrode material.
3. preparation method according to claim 2, is characterized in that, the structure of described combination electrode material is: monatomic carbon-coating is embedded between molybdenum disulfide nano sheet layer equably; Wherein, the diameter of described molybdenum disulfide nano sheet layer is that 200～300nm, thickness are 10～20nm, and the interlamellar spacing of adjacent described molybdenum disulfide nano sheet layer is 0.76～1.04nm.
4. preparation method according to claim 2, is characterized in that, the weight ratio of described sodium molybdate and dopamine is 2:1～4:1.
5. preparation method according to claim 2, is characterized in that, described inert atmosphere is argon gas.
6. the application of molybdenum bisuphide/mesoporous carbon composite electrode material claimed in claim 1, is characterized in that, described combination electrode material is applied to lithium ion battery as negative material.
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| CN104466105A (en) * | 2014-11-12 | 2015-03-25 | 中国科学院深圳先进技术研究院 | Molybdenum disulfide/polyaniline composite material, preparation method thereof and lithium ion battery |
| CN104681815A (en) * | 2015-02-11 | 2015-06-03 | 深圳新宙邦科技股份有限公司 | Spherical molybdenum disulfide composite material and preparation method and application thereof |
| CN104934602A (en) * | 2015-06-19 | 2015-09-23 | 上海交通大学 | Molybdenum disulfide/carbon composite material and preparation method thereof |
| CN105060347A (en) * | 2015-07-20 | 2015-11-18 | 清华大学 | Method for synthesizing ultrathin molybdenum disulfide nanocrystals |
| CN105098151A (en) * | 2015-06-19 | 2015-11-25 | 上海交通大学 | Molybdenum disulfide-carbon hollow ball hybrid material and preparation method thereof |
| CN105148945A (en) * | 2015-09-17 | 2015-12-16 | 上海大学 | Hydro-thermal synthesis method for molybdenum-sulphur co-doped mesoporous nano titanium dioxide visible-light-driven photocatalyst |
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