CN105609774B - A kind of preparation method of Fluorin doped three-dimensional structure lithium sulfur battery anode material - Google Patents
A kind of preparation method of Fluorin doped three-dimensional structure lithium sulfur battery anode material Download PDFInfo
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- CN105609774B CN105609774B CN201610092809.0A CN201610092809A CN105609774B CN 105609774 B CN105609774 B CN 105609774B CN 201610092809 A CN201610092809 A CN 201610092809A CN 105609774 B CN105609774 B CN 105609774B
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H—ELECTRICITY
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Abstract
The present invention provides a kind of preparation method of Fluorin doped three-dimensional structure lithium sulfur battery anode material, including：（1）Graphite oxide is added to the water ultrasound, graphene oxide suspension is formed；（2）Tetrabutyl ammonium fluoride is added in graphene oxide suspension, is then transferred into water heating kettle and carries out hydro-thermal reaction, ethyl alcohol is washed, washed after the completion of reaction, is then freeze-dried, and three-dimensional Fluorin doped graphene is obtained；（3）The three-dimensional Fluorin doped graphene obtained is added to ultrasonic reaction in N methyl pyrrolidones with Ketjen black and forms suspension；（4）Elemental sulfur is added to ultrasound in N methyl pyrrolidones, suspension is formed until elemental sulfur is completely dissolved；（5）It will）Two kinds of obtained suspension mix, and stir evenly, and distilled water is then slowly added under stiring, the lithium sulfur battery anode material of three-dimensional structure is obtained after centrifugation, washing, drying.The method of the present invention improves the cycle life of lithium-sulfur cell.
Description
Technical field
The present invention relates to nano-carbon material synthesis more particularly to a kind of preparation methods of lithium sulfur battery anode material.
Background technology
Lithium-sulfur cell is using lithium metal as cathode, and elemental sulfur is the battery system of anode.There are two put the tool of lithium-sulfur cell
Level platform（About 2.4 V and 2.1 V）, but its electrochemical reaction mechanism is more complicated.Lithium-sulfur cell has higher than energy
（2600 Wh/kg）, specific capacity it is high（1675 mAh/g）, it is at low cost the advantages that, it is considered to be very promising a new generation's electricity
Pond.But there is the problems such as active material utilization is low, cycle life is low and safety is poor at present, this seriously restricts lithium
The development of sulphur battery.The main reason for causing the above problem has the following aspects：（1）Elemental sulfur is electronics and ion insulation
Body, room-temperature conductivity are low（5×10-30S·cm-1）, since the sulphur of not no ionic state exists, thus it is tired as positive electrode activation
It is difficult；（2）The poly- more lithium sulfide Li of state of height generated in electrode process2Sn（8 n >=4 ＞）It is soluble in electrolyte, positive and negative
Concentration difference is formed between pole, cathode is moved under the action of concentration gradient, and the high poly- more lithium sulfides of state are reduced into low by lithium metal
The poly- more lithium sulfides of state.With the progress reacted above, the oligomeric more lithium sulfides of state are assembled in cathode, are finally formed between electrodes
Concentration difference, and move to anode and be oxidized to the high poly- more lithium sulfides of state.This phenomenon is referred to as shuttle effect, reduces sulphur activity
The utilization rate of substance.Insoluble Li simultaneously2S and Li2S2It is deposited on cathode of lithium surface, is further degrading lithium-sulfur cell
Performance；（3）React final product Li2S is equally electronic body, can be deposited on sulfur electrode, and lithium ion vulcanizes in solid-state
Migration velocity is slow in lithium, keeps electrochemical reaction kinetic rate slack-off；（4）Sulphur and final product Li2The density of S is different, works as sulphur
It is lithiated rear volume expansion about 79%, easily leads to Li2The dusting of S causes the safety problem of lithium-sulfur cell.Above-mentioned insufficient restriction
The development of lithium-sulfur cell, this is also that current lithium-sulfur cell research needs the Important Problems solved.
Invention content
A kind of three-dimensional structure lithium sulfur battery anode material is provided in order to solve the above technical problem present invention, with party's legal system
For three-dimensional structure Fluorin doped graphene is gone out, nano-sulfur particles and Ketjen black are deposited on the three-D space structure of Fluorin doped graphene
In, which can improve the electric conductivity of sulphur motor, and can prevent the dissolving of discharging product polysulfide.
It is as follows that the present invention provides a kind of preparation process flow of the lithium sulfur battery anode material of three-dimensional structure：
（1）Graphite oxide is added to the water ultrasound, graphene oxide suspension is formed；
（2）Tetrabutyl ammonium fluoride is added in graphene oxide suspension, is then transferred into water heating kettle and carries out hydro-thermal
Reaction, ethyl alcohol is washed, is washed after the completion of reaction, is then freeze-dried, and three-dimensional Fluorin doped graphene is obtained；
（3）Take step（2）Obtained three-dimensional Fluorin doped graphene is added to Ketjen black in N-Methyl pyrrolidone ultrasonic
Reaction forms suspension；
（4）Elemental sulfur is added in N-Methyl pyrrolidone ultrasound at a certain temperature, until elemental sulfur is completely dissolved
Form suspension；
（5）It will（4）With（3）Obtained two kinds of suspension mixing, stirs evenly, distillation is then slowly added under stiring
Water obtains the lithium sulfur battery anode material of three-dimensional structure after centrifugation, washing, drying.
Step（1）The middle ultrasonic reaction time is 10 ~ 60 minutes, a concentration of 1 ~ 10g/L of graphene oxide suspension;
Step（2）The temperature of middle hydro-thermal reaction is 160 ~ 200 DEG C, and the reaction time is 1 ~ 6 hour, graphite oxide and the tetrabutyl
The mass ratio of ammonium fluoride is 1：0.1~1；
Step（3）The mass ratio of middle three-dimensional Fluorin doped graphene and Ketjen black is 1:0.05 ~ 0.5, a concentration of the 1 of suspension
~5g/L；
Step（4）Middle elemental sulfur and three-dimensional Fluorin doped graphene and Ketjen black gross mass and mass ratio be 10 ~ 20:1, surpass
40 ~ 50 DEG C of the reaction temperature of sound, ultrasonic time is is completely dissolved until sulphur, a concentration of 10 ~ 15g/L of sulphur suspension；
Step（5）The distilled water of middle addition：The volume ratio of N-Methyl pyrrolidone solution is 3 ~ 5 after mixing:1；
The present invention has the advantages that：（1）The preparation method restores graphite oxide, Fluorin doped is the same as hydro-thermal reaction one
Step is completed, and reaction efficiency is improved；（2）The Ketjen black and grapheme material of high conductivity can effectively improve the conductivity of electrode slice；
（3）In charge and discharge process, being configured with for three-dimensional structure is shuttled conducive to lithium ion and electronics in various dimensions conducting path, is improved
Ion and electron conductivity；（4）Ketjen black present in three-dimensional structure, further shortens between nano-sulfur particles and nanometer
The conduction distance of sulphur and graphene sheet layer, is conducive to the raising of conductivity；（5）Fluorine atom in Fluorin doped graphene has most strong
Electronegativity, shuttle effect is effectively reduced to the chemical adsorption of sulphur, improves the cycle life of lithium-sulfur cell.
Description of the drawings
Fig. 1 is the SEM figures of three-dimensional Fluorin doped graphene sulphur composite material prepared by the present invention.
Specific implementation mode
Below in conjunction with the accompanying drawings, the preferably embodiment of the present invention is described in further detail：
Embodiment 1
（1）10mg graphite oxides are added to ultrasound 10 minutes in 10mL water, form the graphene oxide suspension of 1g/L；
（2）1mg tetrabutyl ammonium fluorides are added in graphene oxide suspension, is then transferred into water heating kettle and reacts,
160 DEG C are reacted 6 hours, and ethyl alcohol is washed, washed after the completion of reaction, is then freeze-dried, and three-dimensional Fluorin doped graphene is obtained；
（3）It takes（2）Obtained 10mg three-dimensional Fluorin doped graphenes are added to the N- crassitudes of 15mL with 5mg Ketjen blacks
1g/L suspension is ultrasonically formed in ketone；
（4）150mg elemental sulfurs are added in 15mL N-Methyl pyrrolidones the ultrasound at certain 40 DEG C, until simple substance
Sulphur is completely dissolved the suspension to form 10g/L；
（5）It will（4）With（3）Obtained two kinds of suspension mixing, stirs evenly, 90mL is then slowly added under stiring
Distilled water obtains the lithium sulfur battery anode material of three-dimensional structure after centrifugation, washing, drying.
Embodiment 2
（1）10mg graphite oxides are added to ultrasound 60 minutes in 1mL water, form the graphene oxide suspension of 10g/L；
（2）10mg tetrabutyl ammonium fluorides are added in graphene oxide suspension, is then transferred into water heating kettle and reacts,
200 DEG C are reacted 1 hour, and ethyl alcohol is washed, washed after the completion of reaction, is then freeze-dried, and three-dimensional Fluorin doped graphene is obtained；
（3）It takes（2）Obtained 10mg three-dimensional Fluorin doped graphenes are added to the N- methyl pyrroles of 2.1mL with 0.5mg Ketjen blacks
5g/L suspension is ultrasonically formed in pyrrolidone；
（4）210mg elemental sulfurs are added in 14mL N-Methyl pyrrolidones the ultrasound at 50 DEG C, until elemental sulfur is complete
Fully dissolved forms the suspension of 15g/L；
（5）It will（4）With（3）Obtained two kinds of suspension mixing, stirs evenly, is then slowly added under stiring
80.5mL distilled water obtains the lithium sulfur battery anode material of three-dimensional structure after centrifugation, washing, drying.
Embodiment 3
（1）10mg graphite oxides are added to ultrasound 30 minutes in 5mL water, form the graphene oxide suspension of 2g/L；
（2）5mg tetrabutyl ammonium fluorides are added in graphene oxide suspension, is then transferred into water heating kettle and reacts,
180 DEG C are reacted 3 hours, and ethyl alcohol is washed, washed after the completion of reaction, is then freeze-dried, and three-dimensional Fluorin doped graphene is obtained；
（3）It takes（2）Obtained 10mg three-dimensional Fluorin doped graphenes are added to the N- methylpyrroles of 5.5mL with 1mg Ketjen blacks
2g/L suspension is ultrasonically formed in alkanone；
（4）132mg elemental sulfurs are added in 11mL N-Methyl pyrrolidones the ultrasound at 45 DEG C, until elemental sulfur is complete
Fully dissolved forms the suspension of 12g/L；
（5）It will（4）With（3）Obtained two kinds of suspension mixing, stirs evenly, 66mL is then slowly added under stiring
Distilled water obtains the lithium sulfur battery anode material of three-dimensional structure after centrifugation, washing, drying.
Embodiment 4
（1）10mg graphite oxides are added to ultrasound 20 minutes in 2mL water, form the graphene oxide suspension of 5g/L；
（2）3mg tetrabutyl ammonium fluorides are added in graphene oxide suspension, is then transferred into water heating kettle and reacts,
170 DEG C are reacted 5 hours, and ethyl alcohol is washed, washed after the completion of reaction, is then freeze-dried, and three-dimensional Fluorin doped graphene is obtained；
（3）It takes（2）Obtained 10mg three-dimensional Fluorin doped graphenes are added to the N- crassitudes of 4mL with 2mg Ketjen blacks
3g/L suspension is ultrasonically formed in ketone；
（4）156mg elemental sulfurs are added in 12mL N-Methyl pyrrolidones the ultrasound at 42 DEG C, until elemental sulfur is complete
Fully dissolved forms the suspension of 13g/L；
（5）It will（4）With（3）Obtained two kinds of suspension mixing, stirs evenly, 72mL is then slowly added under stiring
Distilled water obtains the lithium sulfur battery anode material of three-dimensional structure after centrifugation, washing, drying.
Embodiment 5
（1）10mg graphite oxides are added to ultrasound 40 minutes in 4mL water, the graphene oxide for forming 2.5g/L suspends
Liquid；
（2）8mg tetrabutyl ammonium fluorides are added in graphene oxide suspension, is then transferred into water heating kettle and reacts,
190 DEG C are reacted 2 hours, and ethyl alcohol is washed, washed after the completion of reaction, is then freeze-dried, and three-dimensional Fluorin doped graphene is obtained；
（3）It takes（2）Obtained 10mg three-dimensional Fluorin doped graphenes are added to the N- methylpyrroles of 3.25mL with 3mg Ketjen blacks
4g/L suspension is ultrasonically formed in alkanone；
（4）182mg elemental sulfurs are added in 13mL N-Methyl pyrrolidones the ultrasound at 48 DEG C, until elemental sulfur is complete
Fully dissolved forms the suspension of 14g/L；
（5）It will（4）With（3）Obtained two kinds of suspension mixing, stirs evenly, is then slowly added under stiring
56.875mL distilled water obtains the lithium sulfur battery anode material of three-dimensional structure after centrifugation, washing, drying.
The preparation and performance test of electrode；By electrode material, acetylene black and PVDF in mass ratio 80：10：10 in NMP
Mixing, it is electrode film to be coated on aluminium foil, and metal lithium sheet is to electrode, and CELGARD 2400 is diaphragm, the LiTFSI/ of 1mol/L
DOL-DME (volume ratios 1:1) it is electrolyte, the LiNO of 1mol/L3For additive, button electricity is assembled into full of Ar glove boxes
Pond carries out constant current charge-discharge test using Land battery test systems.Charging/discharging voltage ranging from 1-3V, current density are
0.01C, performance are as shown in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Specific discharge capacity after recycling for the first time | 1280mAh/g | 1230mAh/g | 1240mAh/g | 1220mAh/g | 1260mAh/g |
| Specific discharge capacity after 100 cycles | 790mAh/g | 780mAh/g | 710mAh/g | 720mAh/g | 760mAh/g |
Fig. 1 is the SEM figures that the present invention prepares positive electrode, and as can be seen from the figure the positive electrode has a large amount of openings
Three-dimensional cavernous structure, can be good at provide ion transmission channel, improve the chemical property of material.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
The specific implementation of the present invention is confined to these explanations.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to the present invention's
Protection domain.
Claims (4)
1. a kind of preparation method of Fluorin doped three-dimensional structure lithium sulfur battery anode material, which is characterized in that including：
（1）Graphite oxide is added to the water ultrasound, graphene oxide suspension is formed；
（2）Tetrabutyl ammonium fluoride is added in graphene oxide suspension, is then transferred into water heating kettle and carries out hydro-thermal reaction,
Ethyl alcohol is washed, is washed after the completion of reaction, is then freeze-dried, and three-dimensional Fluorin doped graphene is obtained；
（3）Take step（2）Obtained three-dimensional Fluorin doped graphene is added to ultrasonic reaction in N-Methyl pyrrolidone with Ketjen black
Form suspension；
（4）Elemental sulfur is added in N-Methyl pyrrolidone ultrasound at a certain temperature, to be formed until elemental sulfur is completely dissolved
Suspension；
（5）It will（4）With（3）Obtained two kinds of suspension mixing, stirs evenly, distilled water is then slowly added under stiring,
The lithium sulfur battery anode material of three-dimensional structure is obtained after centrifugation, washing, drying；
Step（2）The temperature of middle hydro-thermal reaction is 160-200 DEG C, and the reaction time is 1-6 hours, and graphite oxide is fluorinated with the tetrabutyl
The mass ratio of ammonium is 1：0 .1-1；Step（3）The mass ratio of middle three-dimensional Fluorin doped graphene and Ketjen black is 1:0 .05-0 .5,
A concentration of 1-5g/L of suspension.
2. the method as described in claim 1, which is characterized in that the step（1）The middle ultrasonic reaction time is 10-60 minutes,
A concentration of 1-10g/L of graphene oxide suspension.
3. the method as described in claim 1, which is characterized in that step（4）Middle elemental sulfur and three-dimensional Fluorin doped graphene and section
The mass ratio of the black gross mass sum of qin is 10-20:1,40-50 DEG C of ultrasonic reaction temperature, ultrasonic time is to be completely dissolved until sulphur,
A concentration of 10-15g/L of sulphur suspension.
4. the method as described in claim 1, which is characterized in that step（5）The distilled water of middle addition：N- methylpyrroles after mixing
The volume ratio of alkanone solution is 3-5:1.
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| WO2017139985A1 (en) * | 2016-02-19 | 2017-08-24 | 肖丽芳 | Preparation method for fluorine-doped lithium-sulfur battery anode material having three-dimensional structure |
| CN106602064A (en) * | 2016-12-27 | 2017-04-26 | 深圳市川马电子股份有限公司 | Preparation method and application of iodine-doped graphene |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530911A (en) * | 2010-12-22 | 2012-07-04 | 海洋王照明科技股份有限公司 | Graphene fluoride preparation method |
| CN103682280A (en) * | 2012-09-07 | 2014-03-26 | 中国科学院宁波材料技术与工程研究所 | Lithium-sulfur battery, positive electrode material of battery, and preparation method of material |
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| US8366970B2 (en) * | 2010-07-08 | 2013-02-05 | Xerox Corporation | Method for treating a carbon allotrope |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530911A (en) * | 2010-12-22 | 2012-07-04 | 海洋王照明科技股份有限公司 | Graphene fluoride preparation method |
| CN103682280A (en) * | 2012-09-07 | 2014-03-26 | 中国科学院宁波材料技术与工程研究所 | Lithium-sulfur battery, positive electrode material of battery, and preparation method of material |
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