CN105185994A - Graphene-doped porous carbon/ferroferric oxide nano-fiber lithium battery anode material and preparation method thereof - Google Patents
Graphene-doped porous carbon/ferroferric oxide nano-fiber lithium battery anode material and preparation method thereof Download PDFInfo
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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Abstract
The invention relates to a graphene-doped porous carbon/ferroferric oxide nano-fiber lithium battery anode material and a preparation method thereof. The preparation method comprises the following steps of preparing ferric salt and graphene-doped polyacrylonitrile/polymethyl methacrylate nano-fibers by utilizing electro-spinning technique, and obtaining the graphene-doped porous carbon/ferroferric oxide nano-fiber lithium battery anode material through pre-oxidization and high-temperature carbonization. The specific preparation method comprises the following steps of adding a certain amount of ferric salt and oxidized graphene into mixed solution of polyacrylonitrile/polymethyl methacrylate, obtaining electro-spinning solution after ultrasonic dispersion and high-speed stirring and dissolution, pre-oxidizing the nano-fibers obtained by electro-spinning at 200-300 DEG C, and obtaining the graphene-doped porous carbon/ferroferric oxide nano-fiber lithium battery anode material after carbonizing at 500-1000 DEG C. According to the graphene-doped porous carbon/ferroferric oxide nano-fiber lithium battery anode material prepared by the invention, the electrochemical performance can be effectively collaborative, and the specific capacity, the initial charge-discharge efficiency and the cycling performance of the battery are improved.
Description
Technical field
Porous carbon/ferriferrous oxide nano fiber lithium cell cathode material that the present invention relates to a kind of doped graphene and preparation method thereof, is applied to electrode material of lithium battery, is specifically related to chemical energy source technical field of energy storage.
Background technology
Energy problem is one of maximum challenge of facing of the mankind, and for addressing this problem, people constantly make great efforts the Development of Novel energy, meanwhile also it is also proposed more and more higher requirement to energy storage technology.And lithium ion battery is since the commercialization nineties in last century, occupied leading position at portable electronics market always.Meanwhile, along with numerous mobile electronic devices such as mobile phone, digital camera, notebook computer develop to miniaturization further, the demand of the novel power supply that people are little to volume, energy is high is also more and more urgent, and the new electrode materials of lithium ion battery that therefore exploitation has more high power capacity, more long-life and can realize fast charging and discharging becomes the study hotspot of material science.At present, the lithium cell cathode material that commercialization adopts is primarily of graphite-like material with carbon element, but the theoretical capacity of graphite only has 372mAh/g, therefore exploitation has higher charging and discharging capacity, stability and longer cycle life and the low electrode material of cost becomes current research emphasis.Compared with material with carbon element, metal oxide, as Sn, Si, SnO
2, Co
3o
4, Fe
2o
3and Fe
3o
4deng, there is higher theoretical capacity.Fe
3o
4be one of quite potential negative material, there are good (σ=2 × 10 of specific capacity high (926mAh/g) electron conduction
4s/m, is better than other transition metal oxides), cheap, aboundresources, the feature such as nontoxic and environmentally friendly, but huge change in volume and serious particle aggregation can be there is in doff lithium process, cause electric charge and Li
+transmission and diffusion poor, the cyclical stability as negative material is poor, high rate performance is not high.
Electrostatic spinning is a kind of cheapness and prepares the effective ways of carbon nano-fiber and carbon complex fiber material efficiently.In recent years, prepare the coated electrode material of carbon fiber by electrostatic spinning technique and be proved to be the chemical property that effectively can improve material, this is the conductivity that improve material because carbon is coated on the one hand, and the coated carbon-coating in outside also limit growing up of particle thus shortens the evolving path of lithium ion on the other hand.In addition, Graphene has good conductivity, mechanical property and larger specific area and is widely used in lithium battery positive and negative pole material.The layer structure of Graphene uniqueness makes it as the change that can cushion charge and discharge process volume during electrode material.
Summary of the invention
Porous carbon/ferriferrous oxide nano fiber lithium cell cathode material that the object of this invention is to provide a kind of doped graphene and preparation method thereof.Utilize electrostatic spinning technique preparation to contain the polyacrylonitrile of molysite and graphene oxide and poly-methyl esters methyl acrylate composite nano fiber, obtain doped ferroferric oxide/Graphene porous carbon nanofiber material through pre-oxidation, high temperature cabonization.This lithium cell cathode material contains Graphene and carbon nanofiber networks, can increase the conductivity of electrode material, improves the transmission speed of lithium ion and electronics.The network configuration of porous is conducive to the volumetric expansion of buffering ferriferrous oxide nano-particle in charge and discharge process, improves cycle performance and the high rate performance of battery significantly.
The technical scheme of the object of the invention is, provide a kind of porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of doped graphene, it is made up of carbon, tri-iron tetroxide and Graphene, and its mass ratio is 65:20-40:1-10, porosity 500-1000cm
3g
1.This lithium cell cathode material pore size is 2-10nm, and the diameter of described porous nano-fibre is 100-300nm, and described tri-iron tetroxide is with the formal distribution of nano particle in porous nano-fibre, and particle is of a size of 10-25nm.
The preparation method of the porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of doped graphene, adopts following steps:
(1) graphene oxide is put in N-N dimethyl formamide, after ultrasonic disperse 5-10h, add polyacrylonitrile powder, polymethylmethacrylate powder and molysite, 3-6h is stirred under 80 DEG C of conditions, obtain electrostatic spinning solution, the mass fraction of polyacrylonitrile is 6%-10%, and the mass fraction of polymethyl methacrylate is 5%-10%, and the mass fraction of molysite is 20%-30%;
(2) be transferred in syringe by the electrostatic spinning liquid of gained in step (1) and carry out electrostatic spinning, spinning voltage is 10-30kv, and spinning flow is 0.1-2.0ml/h, and the distance between needle point and dash receiver is 10-30cm;
(3) nanofiber of gained in step (2) is carried out pre-oxidation in air atmosphere under 200-300 DEG C of condition, be transferred to subsequently in carbide furnace, under argon gas/nitrogen protection, 500-1000 DEG C is raised to the speed of 2-10 DEG C/min, process 5-10h, obtains the porous carbon/ferriferrous oxide nano fiber of doped graphene;
(4) by the porous nano-fibre of gained in step (3), utilize Kynoar/acetylene black binding agent to be pasted onto on Copper Foil, to be transferred in baking oven dry 2h under 100-200 DEG C of condition subsequently, to obtain electrode material of lithium battery.The mass ratio of described binding agent Kynoar/acetylene black is 1:1.
The molecular weight of the polyacrylonitrile powder described in step of the present invention (1) is 5-15 ten thousand, and the molecular weight of polymetylmetacrylate is 5-15 ten thousand, and described molysite is ferric acetyl acetonade, ferric nitrate, iron chloride.
Compared with existing lithium cell cathode material and preparation method thereof, the present invention has the following advantages:
(1) adopt electrostatic spinning technique to combine with carbonization the porous carbon/ferriferrous oxide nano fiber lithium cell cathode material preparing doped graphene, there is the advantages such as specific area is large, cost is low, the course of processing is simple;
(2) porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of doped graphene that prepared by the present invention has larger porosity, the change of ferriferrous oxide nano-particle volume in charge and discharge process can be alleviated fully, be conducive to diffusion and the infiltration of electrolyte, in addition, Graphene can also increase the conductivity of material, therefore considerably improves cyclical stability and the high rate performance of battery.
Accompanying drawing explanation
Fig. 1 to be the multiplication factor of the porous carbon/ferriferrous oxide nano fiber of doped graphene be SEM photo of 10,000 times;
Fig. 2 to be the multiplication factor of the porous carbon/ferriferrous oxide nano fiber of doped graphene be SEM photo of 100,000 times.
Embodiment
Below in conjunction with example, the present invention is further described.
Porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of doped graphene, it is made up of carbon, tri-iron tetroxide and Graphene, and its mass ratio is 65:20-40:1-10, porosity 500-1000cm
3g
1.This lithium cell cathode material pore size is 2-10nm, and the diameter of described porous nano-fibre is 100-300nm, and described tri-iron tetroxide is with the formal distribution of nano particle in porous nano-fibre, and particle is of a size of 10-25nm.
embodiment 1
The preparation method of the porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of doped graphene, adopts following steps:
(1) graphene oxide is put in N-N dimethyl formamide, after ultrasonic disperse 8h, add polyacrylonitrile powder, polymethylmethacrylate powder and molysite, under 80 DEG C of conditions, stir 4h, obtain electrostatic spinning solution.The mass fraction of polyacrylonitrile is 6-10%, and the mass fraction of polymethyl methacrylate is 5-10%, and the mass fraction of molysite is 20-30%;
(2) electrostatic spinning liquid of gained in step (1) is transferred in syringe carries out electrostatic spinning.Spinning voltage is 10-30kv, and spinning flow is 0.1-2.0ml/h, and the distance between needle point and dash receiver is 10-30cm;
(3) nanofiber of gained in step (2) is carried out pre-oxidation in air atmosphere under 200-300 DEG C of condition, be transferred to subsequently in carbide furnace, under argon gas/nitrogen protection, 600 DEG C are raised to the speed of 2-10 DEG C/min, process 5-10h, obtains the porous carbon/ferriferrous oxide nano fiber of doped graphene;
(4) by the porous nano-fibre of gained in step (3), utilize Kynoar/acetylene black binding agent to be pasted onto on Copper Foil, to be transferred in baking oven dry 2h under 100-200 DEG C of condition subsequently, to obtain electrode material of lithium battery.The mass ratio of described binding agent Kynoar/acetylene black is 1:1;
Table 1 shows the porous carbon/specific discharge capacity of ferriferrous oxide nano fiber lithium cell cathode material under different multiplying of doped graphene.The SEM photo of the porous carbon/ferriferrous oxide nano fiber of doped graphene is as shown in Fig. 1 (in figure, multiplication factor is 10,000 times and 100,000 times), as seen from Figure 1, the diameter of the porous carbon/ferriferrous oxide nano fiber of doped graphene that prepared by the present invention is distributed in 100-200nm.
The table 1 doped ferroferric oxide/specific discharge capacity of Graphene porous carbon nanofiber material under different multiplying (mAh/g)
| Sample | 0.05C | 1.0 C | 2 C | 5 C | 10 C | 20 C | 50 C |
| Example 1 | 900 | 720 | 511 | 485 | 431 | 411 | 401 |
| Example 2 | 930 | 850 | 708 | 651 | 598 | 553 | 539 |
| Example 3 | 850 | 760 | 553 | 493 | 420 | 407 | 398 |
| Example 4 | 860 | 754 | 523 | 489 | 436 | 403 | 382 |
embodiment 2
The preparation method of the porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of doped graphene, adopts following steps:
(1) graphene oxide is put in N-N dimethyl formamide, after ultrasonic disperse 8h, add polyacrylonitrile powder, polymethylmethacrylate powder and molysite, 5h is stirred under 80 DEG C of conditions, obtain electrostatic spinning solution, the mass fraction of polyacrylonitrile is 6-10%, and the mass fraction of polymethyl methacrylate is 5-10%, and the mass fraction of molysite is 20-30%;
(2) be transferred in syringe by the electrostatic spinning liquid of gained in step (1) and carry out electrostatic spinning, spinning voltage is 10-30kv, and spinning flow is 0.1-2.0ml/h, and the distance between needle point and dash receiver is 10-30cm;
(3) nanofiber of gained in step (2) is carried out pre-oxidation in air atmosphere under 200-300 DEG C of condition, be transferred to subsequently in carbide furnace, under argon gas/nitrogen protection, 650 DEG C are raised to the speed of 2-10 DEG C/min, process 5-10h, obtains the porous carbon/ferriferrous oxide nano fiber of doped graphene;
(4) by the porous nano-fibre of gained in step (3), utilize Kynoar/acetylene black binding agent to be pasted onto on Copper Foil, to be transferred in baking oven dry 2h under 100-200 DEG C of condition subsequently, to obtain electrode material of lithium battery.The mass ratio of described binding agent Kynoar/acetylene black is 1:1, and the porous carbon/specific discharge capacity of ferriferrous oxide nano fiber lithium cell cathode material under different multiplying of the doped graphene of preparation is as shown in table 1.
embodiment 3
The preparation method of the porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of doped graphene, adopts following steps:
(1) graphene oxide is put in N-N dimethyl formamide, after ultrasonic disperse 8h, add polyacrylonitrile powder, polymethylmethacrylate powder and molysite, under 80 DEG C of conditions, stir 5h, obtain electrostatic spinning solution.The mass fraction of polyacrylonitrile is 6-10%, and the mass fraction of polymethyl methacrylate is 5-10%, and the mass fraction of molysite is 20-30%;
(2) electrostatic spinning liquid of gained in step (1) is transferred in syringe carries out electrostatic spinning.Spinning voltage is 10-30kv, and spinning flow is 0.1-2.0ml/h, and the distance between needle point and dash receiver is 10-30cm;
(3) nanofiber of gained in step (2) is carried out pre-oxidation in air atmosphere under 200-300 DEG C of condition, be transferred to subsequently in carbide furnace, under argon gas/nitrogen protection, 700 DEG C are raised to the speed of 2-10 DEG C/min, process 5-10h, obtains the porous carbon/ferriferrous oxide nano fiber of doped graphene;
(4) by the porous nano-fibre of gained in step (3), Kynoar/acetylene black binding agent is utilized to be pasted onto on Copper Foil, to be transferred in baking oven dry 2h under 100-200 DEG C of condition subsequently, obtain electrode material of lithium battery, the mass ratio of described binding agent Kynoar/acetylene black is 1:1.Porous carbon/the specific discharge capacity of ferriferrous oxide nano fiber lithium cell cathode material under different multiplying preparing doped graphene is as shown in table 1.
embodiment 4
The preparation method of the porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of doped graphene, adopts following steps:
(1) graphene oxide is put in N-N dimethyl formamide, after ultrasonic disperse 8h, add polyacrylonitrile powder, polymethylmethacrylate powder and molysite, under 80 DEG C of conditions, stir 5h, obtain electrostatic spinning solution.The mass fraction of polyacrylonitrile is 6-10%, and the mass fraction of polymethyl methacrylate is 5-10%, and the mass fraction of molysite is 20-30%;
(2) electrostatic spinning liquid of gained in step (1) is transferred in syringe carries out electrostatic spinning.Spinning voltage is 10-30kv, and spinning flow is 0.1-2.0ml/h, and the distance between needle point and dash receiver is 10-30cm;
(3) nanofiber of gained in step (2) is carried out pre-oxidation in air atmosphere under 200-300 DEG C of condition, be transferred to subsequently in carbide furnace, under argon gas/nitrogen protection, 750 DEG C are raised to the speed of 2-10 DEG C/min, process 5-10h, obtains the porous carbon/ferriferrous oxide nano fiber of doped graphene;
(4) by the porous nano-fibre of gained in step (3), utilize Kynoar/acetylene black binding agent to be pasted onto on Copper Foil, to be transferred in baking oven dry 2h under 100-200 DEG C of condition subsequently, to obtain electrode material of lithium battery.The mass ratio of described binding agent Kynoar/acetylene black is 1:1.Porous carbon/the specific discharge capacity of ferriferrous oxide nano fiber lithium cell cathode material under different multiplying preparing doped graphene is as shown in table 1.
Claims (4)
1. porous carbon/ferriferrous oxide nano fiber the lithium cell cathode material of a doped graphene, it is characterized in that: the porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of described doped graphene is made up of carbon, tri-iron tetroxide and Graphene, the mass ratio of carbon, tri-iron tetroxide and Graphene is 65:20-40:1-10, and porosity is 500-1000cm
3g
1.
2. porous carbon/ferriferrous oxide nano fiber the lithium cell cathode material of doped graphene according to claim 1, it is characterized in that: the diameter of described nanofiber is 100-300nm, pore-size above nanofiber is 2-10nm, tri-iron tetroxide is scattered in porous nano-fibre with the form of nano particle, and tri-iron tetroxide is of a size of 10-25nm.
3. the preparation method of the porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of doped graphene as claimed in claim 1, is characterized in that: carry out according to the following steps:
(1) graphene oxide is put in N-N dimethyl formamide, after ultrasonic disperse 5-10h, add polyacrylonitrile powder, polymethylmethacrylate powder and molysite, 3-6h is stirred under 80 DEG C of conditions, obtain electrostatic spinning solution, the mass fraction of polyacrylonitrile is 6%-10%, and the mass fraction of polymethyl methacrylate is 5%-10%, and the mass fraction of molysite is 20%-30%;
(2) be transferred in syringe by the electrostatic spinning liquid of gained in step (1) and carry out electrostatic spinning, spinning voltage is 10-30kv, and spinning flow is 0.1-2.0ml/h, and the distance between needle point and dash receiver is 10-30cm;
(3) nanofiber of gained in step (2) is carried out pre-oxidation in air atmosphere under 200-300 DEG C of condition, be transferred to subsequently in carbide furnace, under argon gas/nitrogen protection, 500-1000 DEG C is raised to the speed of 2-10 DEG C/min, process 5-10h, obtains the porous carbon/ferriferrous oxide nano fiber of doped graphene;
(4) by the porous nano-fibre of gained in step (3), Kynoar/acetylene black binding agent is utilized to be pasted onto on Copper Foil, to be transferred in baking oven dry 2h under 100-200 DEG C of condition subsequently, obtain electrode material of lithium battery, the mass ratio of described binding agent Kynoar/acetylene black is 1:1.
4. the preparation method of the porous carbon/ferriferrous oxide nano fiber lithium cell cathode material of doped graphene according to claim 3, it is characterized in that: in described step (1), the molecular weight of polyacrylonitrile is 5-15 ten thousand, the molecular weight of polymethyl methacrylate is 5-15 ten thousand, and molysite is ferric acetyl acetonade, ferric nitrate, iron chloride.
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| CN106159228A (en) * | 2016-07-26 | 2016-11-23 | 广东工业大学 | A kind of nitrogen-doped graphene metal oxide nano composite material and its preparation method and application |
| CN106158426A (en) * | 2016-08-19 | 2016-11-23 | 南京林业大学 | A kind of method preparing flexible super capacitor wire electrode |
| CN106207126A (en) * | 2016-08-25 | 2016-12-07 | 陕西科技大学 | A kind of Fe3o4the preparation method of the lithium ion battery negative material of/rGO sandwich structure |
| WO2018006557A1 (en) * | 2016-07-06 | 2018-01-11 | The Hong Kong University Of Science And Technology | Tunable and scalable synthesis of hierarchical porous nanocarbon/sulfur composite cathodes |
| CN107768645A (en) * | 2017-11-28 | 2018-03-06 | 吉林大学 | A kind of porous nitrogen-doped carbon nanometer sheet composite negative pole material and preparation method thereof |
| CN107845787A (en) * | 2017-09-28 | 2018-03-27 | 东北师范大学 | Pomegranate shape Fe3O4@N C lithium cell cathode material preparation methods |
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