CN103594714A - Fluorinated graphene electrode material and preparation method thereof - Google Patents
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Abstract
The invention discloses a fluorinated graphene electrode material and a preparation method thereof. The preparation method comprises the steps: carrying out thermal intercalation of graphite fluoride by using an organic solvent with low boiling point; carrying out ultrasonic stripping of graphite fluoride; centrifuging to remove graphite fluoride which is not stripped, carrying out suction filtration of the centrifuged upper solution to obtain fluorinated graphene, and adding a conductive agent and an adhesive into fluorinated graphene to obtain the fluorinated graphene electrode material. According to the technical scheme of the invention, the prepared composite material has the advantages of high specific capacitance and voltage platform and the like, and is suitable for use in electrode materials of lithium batteries.
Description
Technical field
The present invention relates to a kind of fluorinated graphene electrode material of lithium battery and preparation method thereof, belong to energy storage material technical field.
Background technology
Fluoridizing of material with carbon element will be traced back to decades ago, and from fluorographite the earliest to fluorinated fullerene, carbon fluoride nano-tube to fluorinated graphene, fluorocarbons is the focus of research with the performance of its excellence always, and will cut a conspicuous figure in future technology application.
Fluorinated graphene can be regarded as Graphene to be fluoridized by some or all of, and the sp2 structure in graphite is by the some or all of sp3 that is transformed into, but still keeps laminated structure, is the thinnest insulator, can be called two-dimentional polytetrafluoroethylene.Become the two-dimentional newcomer in carbon family.Graphene is considered to the prototype structure unit of other dimension material: it can wrap into the C60 of 0D, is curled into the carbon nano-tube of 1D, is piled into the graphite of 3D, through fluoridizing and become the fluorinated graphene of 2D.Fluorinated graphene is rigid molecule, is different from the corrugated of Graphene, and fluorinated graphene is smooth sheet.Although fluorinated graphene is still two-dimensional structure, but carbon atom is not wherein in a plane, present chair form, fluorine atom is arranged in the both sides (O.Leenaerts of lamella according to certain rules, et al.First-principles investigation of graphene fluoride and graphene[J] .Physical Review B, 2010,82 (19), 195436).
The people such as R.R.Nair have successfully made fluorinated graphene by stoechiometric process, fluorine atom has been received on each independent carbon atom, this just can eliminate electron cloud, the normality that also can prevent electric current flows, but this can not affect graphite framework (R.R.Nair complete in microstructure, et al.Fluorographene:A Two-Dimensional Counterpart of Teflon[J] .Small, 2010,6 (24): 2877-2884).In former work, they mainly bias toward hydrogen atom rather than fluorine atom, but find that the hydrogenation graphite generating is at high temperature unstable, and fluorinated graphene is that a kind of mechanical strength is high, the compound of calorifics and stable chemical performance, in air, be heated to 400 ℃ still very stable.The birth of this novel substance will have an immense impact on to electronic application, and it will improve electron mass, and fluorinated graphene can be used as anode material of lithium battery, or is applied in organic electronic product as high-quality barrier material.The people such as Makotchenko use ClF3 to carry out fluorination reaction to graphite.The fluorographite preparing is put into Muffle furnace, be greater than thermal expansion at 800 ℃, fluorinated graphene prepared by this kind of method is said just a kind of (Makotchenko of expanded graphite in a sense, et al.The synthesis and properties of highly exfoliated graphites from fluorinated graphite intercalation compounds[J] .Carbon, 2011,49 (10), 3233-3241).The direct fluorinated graphenes of use XeF2 gas such as Jeon can obtain carbon fluorine than the fluorinated graphene of 1:1, but reaction condition is harsher and the extremely low (Jeon of productive rate, et al.Fluorographene:A Wide Bandgap Semiconductor with Ultraviolet Luminescence[J] .ACS Nano 2011,5,1042).The ultrasonic stripping methods of use such as Haixin Chang are directly peeled off fluorographite in ionic liquid, also can make the fluorinated graphene of few layer, but this kind of method ionic liquid cost of material used too expensive (Haixin Chang et al.Facile Synthesis of Wide-Bandgap Fluorinated Graphene Semiconductors[J] .Chem.Eur.J.2011,17 (32), 8896 – 8903).
At present in primary cell theoretical specific energy maximum be exactly lithium fluorocarbon battery (about 2180Wh/kg), it is also first as the positive electrode of the anodal lithium battery lithium fluorocarbon of a kind of solid battery of commodity.Fluorinated graphene specific energy is high, voltage is high, self discharge is low, its Theoretical Mass specific energy is higher, be easy to accomplish miniaturization and lightness, and its discharge platform is (2.5-2.7V) steadily, operating temperature range is wide, self discharge is low, and storage life long (> 10 years), therefore has been a great concern.At present, the technology of preparing of fluorinated graphene is still immature, real few for the research of fluorinated graphene.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of fluorinated graphene material is provided, this fluorinated graphene material has the advantages such as regularity is high, the number of plies is few, product is pure.Its preparation method technique is simple, raw material is cheap, cost is low, and output is high, is applicable to large-scale production.
The technology of the present invention object is realized by following technical proposals.
Fluorinated graphene electrode material and preparation method thereof, described fluorinated graphene material is to be prepared from through the then ultrasonic dispersion of the hot intercalation of organic solvent by fluorographite, according to following step, is prepared:
Described organic solvent is selected chloroform, oxolane, acetone, isopropyl alcohol, acetonitrile or ethanol; Specifically, select organic solvent 100mL, in stainless steel cauldron, at the uniform velocity stir half an hour, make Graphite fluoride Composite Deposition in organic solvent; At 60 ℃-150 ℃, heat 6h-12h, then by the ultrasonic 2h – of gained solution 12h, by solution centrifugal 5min – 30min under the rotating speed of 500r/min – 4000r/min, remove lower floor's solid, by gained solution suction filtration, obtain filter cake, filter cake is dried at 60 ℃, obtain fluorinated graphene material.
In step 2 is implemented, at fluorinated graphene, acetylene black, Kynoar solution, mix in process, select to add NMP, with the slurry that obtains mixing; Ground slurry is evenly coated on aluminium foil, described aluminium foil prior in baking oven 50 ℃ standing 20 minutes, be positioned in convection oven and under uniform temperature, dry 1～2 hour, the material having dried is placed in to vacuum drying chamber dry 24 hours.
The positive electrode preparing is assembled into lithium battery, the electrochemical property test of being then correlated with, lithium battery assembly technology wherein, just very prepared fluorinated graphene electrode material, negative pole is lithium metal, electrolyte is LB335C; Battery test system is the Land CT2001A of Wuhan Jin Nuo Electronics Co., Ltd., and adopts transmission electron microscope to carry out morphology analysis, as shown in Figure 1.As shown in Figures 2 and 3, by solvent heat graft process, can effectively prepare fluorinated graphene, and can there is not other chemical reactions with fluorographite in solvent for use, because the fluorinated graphene sheet number of plies reduces, increased electrochemical reaction specific area, improve the transmission rate of lithium ion, thereby improved discharge voltage and the specific capacity of battery.
Technical solution of the present invention is because being used the hot graft process of low boiling point organic solvent to prepare fluorinated graphene material, do not need high temperature, high vacuum condition and special reaction kit, simple with other preparation methods' comparison preparation process of fluorinated graphene material, preparation cost is cheap.Can control easily by the temperature-time of simple regulation and control reaction solution concentration, hot intercalation and centrifugal rotating speed time etc. the thickness of fluorinated graphene; In addition, resulting product is pure, is easy to realize large-scale production, compares with fluorographite raw material, and the fluorinated graphene material making has higher voltage platform and specific capacity.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo (the Dutch Tecnai G2 F20 of FEI Co.) of the electrode material prepared of the present invention.
Fig. 2 is the infrared spectrum contrast of the fluorinated graphene prepared of the present invention and fluorographite raw material, and wherein 1 is fluorographite, and 2 is fluorinated graphene.
Fig. 3 is the discharge curve contrast of the electrode material prepared of the present invention and fluorographite raw material, and wherein current density is 10mA/g, and 1 is fluorographite, and 2 is fluorinated graphene electrode material.
Embodiment
Below in conjunction with specific embodiment, further illustrate technical scheme of the present invention, fluorographite manufacturer is that Hubei Zhuo Xi fluoridizes Science and Technology Ltd..
Take 20mg fluorographite and add in 100mL oxolane, at the uniform velocity stir half an hour, make Graphite fluoride Composite Deposition in acetone, then add in stainless steel cauldron, reactor is put into Muffle furnace, heat 12h at 60 ℃, after finishing heating time, by the ultrasonic 6h of gained suspension, then by the centrifugal 30min under the rotating speed of 500r/min of the suspension after ultrasonic, remove lower floor's solid, by gained solution suction filtration, obtain filter cake, filter cake is dried at 60 ℃, obtain fluorinated graphene material.Weigh the fluorinated graphene of certain proportioning, acetylene black, PVDF solution (being dissolved in NMP, mass fraction 10%), fluorinated graphene, acetylene black, Kynoar mass ratio is 80:10:10, is then placed in mortar and grinds, then splash into 2ml NMP.Ground slurry is evenly coated on aluminium foil, be positioned in convection oven and dry 1-2 hour under uniform temperature.The material having dried is placed in to vacuum drying chamber dry 24 hours.Obtain fluorinated graphene electrode material.The positive electrode preparing is assembled into lithium battery, and under the discharge rate of 10mA/g, the fluorinated graphene material making has than the high voltage platform of fluorographite and specific capacity.
Take 50mg fluorographite and add in 100mL acetone, at the uniform velocity stir half an hour, make Graphite fluoride Composite Deposition in acetone, then add in stainless steel cauldron, at 80 ℃, heat 10h, after finishing heating time, by the ultrasonic 8h of gained suspension, then by the centrifugal 30min under the rotating speed of 1000r/min of the suspension after ultrasonic, remove lower floor's solid, by gained solution suction filtration, obtain filter cake, filter cake is dried at 60 ℃, obtain fluorinated graphene material.Weigh the fluorinated graphene of certain proportioning, acetylene black, PVDF solution (being dissolved in NMP, mass fraction 10%), fluorinated graphene, acetylene black, Kynoar mass ratio is 75:15:10, is then placed in mortar and grinds, then splash into 2ml NMP.Ground slurry is evenly coated on aluminium foil, be positioned in convection oven and dry 1-2 hour under uniform temperature.The material having dried is placed in to vacuum drying chamber dry 24 hours.Obtain fluorinated graphene electrode material.The positive electrode preparing is assembled into lithium battery, and under the discharge rate of 10mA/g, the fluorinated graphene material making has than the high voltage platform of fluorographite and specific capacity.
Embodiment 3
Take 60mg fluorographite and add in 100mL isopropyl alcohol, at the uniform velocity stir half an hour, make Graphite fluoride Composite Deposition in acetone, then add in stainless steel cauldron, reactor is put into Muffle furnace, heat 12h at 100 ℃, after finishing heating time, by the ultrasonic 10h of gained suspension, then by the centrifugal 20min under the rotating speed of 1500r/min of the suspension after ultrasonic, remove lower floor's solid, by gained solution suction filtration, obtain filter cake, filter cake is dried at 60 ℃, obtain fluorinated graphene material.Weigh the fluorinated graphene of certain proportioning, acetylene black, PVDF solution (being dissolved in NMP, mass fraction 10%), fluorinated graphene, acetylene black, Kynoar mass ratio is 82:8:10, is then placed in mortar and grinds, then splash into 2ml NMP.Ground slurry is evenly coated on aluminium foil, be positioned in convection oven and dry 1-2 hour under uniform temperature.The material having dried is placed in to vacuum drying chamber dry 24 hours.Obtain fluorinated graphene electrode material.The positive electrode preparing is assembled into lithium battery, and under the discharge rate of 10mA/g, the fluorinated graphene material making has than the high voltage platform of fluorographite and specific capacity.Embodiment 4
Take 100mg fluorographite and add in 100mL chloroform, at the uniform velocity stir half an hour, make Graphite fluoride Composite Deposition in acetone, then add in stainless steel cauldron, reactor is put into Muffle furnace, heat 8h at 120 ℃, after finishing heating time, by the ultrasonic 9h of gained suspension, then by the centrifugal 15min under the rotating speed of 2500r/min of the suspension after ultrasonic, remove lower floor's solid, by gained solution suction filtration, obtain filter cake, filter cake is dried at 60 ℃, obtain fluorinated graphene material.Weigh the fluorinated graphene of certain proportioning, acetylene black, PVDF solution (being dissolved in NMP, mass fraction 10%), fluorinated graphene, acetylene black, Kynoar mass ratio is 85:5:10, is then placed in mortar and grinds, then splash into 2ml NMP.Ground slurry is evenly coated on aluminium foil, be positioned in convection oven and dry 1-2 hour under uniform temperature.The material having dried is placed in to vacuum drying chamber dry 24 hours.Obtain fluorinated graphene electrode material.The positive electrode preparing is assembled into lithium battery, and under the discharge rate of 10mA/g, the fluorinated graphene material making has than the high voltage platform of fluorographite and specific capacity.
Embodiment 5
Take 100mg fluorographite and add in 100mL chloroform, at the uniform velocity stir half an hour, make Graphite fluoride Composite Deposition in acetone, then add in stainless steel cauldron, reactor is put into Muffle furnace, heat 8h at 120 ℃, after finishing heating time, by the ultrasonic 9h of gained suspension, then by the centrifugal 15min under the rotating speed of 2500r/min of the suspension after ultrasonic, remove lower floor's solid, by gained solution suction filtration, obtain filter cake, filter cake is dried at 60 ℃, obtain fluorinated graphene material.Weigh the fluorinated graphene of certain proportioning, acetylene black, PVDF solution (being dissolved in NMP, mass fraction 10%), fluorinated graphene, acetylene black, Kynoar mass ratio is 75:15:10, is then placed in mortar and grinds, then splash into 2ml NMP.Ground slurry is evenly coated on aluminium foil, be positioned in convection oven and dry 1-2 hour under uniform temperature.The material having dried is placed in to vacuum drying chamber dry 24 hours.Obtain fluorinated graphene electrode material.The positive electrode preparing is assembled into lithium battery, and under the discharge rate of 10mA/g, the fluorinated graphene material making has than the high voltage platform of fluorographite and specific capacity.
Above the present invention has been done to exemplary description; should be noted that; in the situation that not departing from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (8)
1. fluorinated graphene electrode material, is characterized in that, described fluorinated graphene material is to be prepared from through the then ultrasonic dispersion of the hot intercalation of organic solvent by fluorographite, according to following step, is prepared:
Step 1, is dispersed in fluorographite in organic solvent, adds stainless steel cauldron to make it airtight, at 60 ℃-150 ℃, heat 6h-12h, then by after the ultrasonic centrifugal removal of gained solution lower floor solid, the filter cake that gained solution suction filtration is obtained is dried, and obtains fluorinated graphene material;
Step 2, taking fluorinated graphene, acetylene black, Kynoar solution mixes, the slurry mixing is evenly coated to bake drying on aluminium foil, obtain fluorinated graphene electrode material, fluorinated graphene wherein, acetylene black, Kynoar mass ratio is (75-85): (15-5): 10, preferably (80-85): (10-15): 10, described Kynoar solution is that Kynoar is dissolved in 1-METHYLPYRROLIDONE (NMP), mass fraction 10%.
2. fluorinated graphene electrode material according to claim 1, is characterized in that, in step 2 is implemented, at fluorinated graphene, acetylene black, Kynoar solution, mixes in process, selects to add NMP, with the slurry that obtains mixing; Ground slurry is evenly coated on aluminium foil, described aluminium foil prior in baking oven 50 ℃ standing 20 minutes, be positioned in convection oven and under uniform temperature, dry 1～2 hour, the material having dried is placed in to vacuum drying chamber dry 24 hours.
3. fluorinated graphene electrode material according to claim 1, is characterized in that, in step 1, described organic solvent is selected chloroform, oxolane, acetone, isopropyl alcohol, acetonitrile or ethanol.
4. fluorinated graphene electrode material according to claim 1, is characterized in that, in step 1, selects organic solvent 100mL, in stainless steel cauldron, at the uniform velocity stirs half an hour, makes Graphite fluoride Composite Deposition in organic solvent; At 60 ℃-150 ℃, heat 6h-12h, then by the ultrasonic 2h – of gained solution 12h, by solution centrifugal 5min – 30min under the rotating speed of 500r/min – 4000r/min, remove lower floor's solid, by gained solution suction filtration, obtain filter cake, filter cake is dried at 60 ℃, obtain fluorinated graphene material.
5. the preparation method of fluorinated graphene electrode material, is characterized in that, described fluorinated graphene material is to be prepared from through the then ultrasonic dispersion of the hot intercalation of organic solvent by fluorographite, according to following step, is prepared:
Step 1, is dispersed in fluorographite in organic solvent, adds stainless steel cauldron to make it airtight, at 60 ℃-150 ℃, heat 6h-12h, then by after the ultrasonic centrifugal removal of gained solution lower floor solid, the filter cake that gained solution suction filtration is obtained is dried, and obtains fluorinated graphene material;
Step 2, taking fluorinated graphene, acetylene black, Kynoar solution mixes, the slurry mixing is evenly coated to bake drying on aluminium foil, obtain fluorinated graphene electrode material, fluorinated graphene wherein, acetylene black, Kynoar mass ratio is (75-85): (15-5): 10, preferably (80-85): (10-15): 10, described Kynoar solution is that Kynoar is dissolved in 1-METHYLPYRROLIDONE (NMP), mass fraction 10%.
6. the preparation method of fluorinated graphene electrode material according to claim 5, it is characterized in that, in step 2 is implemented, at fluorinated graphene, acetylene black, Kynoar solution, mix in process, select to add NMP, with the slurry that obtains mixing; Ground slurry is evenly coated on aluminium foil, described aluminium foil prior in baking oven 50 ℃ standing 20 minutes, be positioned in convection oven and under uniform temperature, dry 1～2 hour, the material having dried is placed in to vacuum drying chamber dry 24 hours.
7. the preparation method of fluorinated graphene electrode material according to claim 5, is characterized in that, in step 1, described organic solvent is selected chloroform, oxolane, acetone, isopropyl alcohol, acetonitrile or ethanol.
8. the preparation method of fluorinated graphene electrode material according to claim 5, is characterized in that, in step 1, selects organic solvent 100mL, in stainless steel cauldron, at the uniform velocity stirs half an hour, makes Graphite fluoride Composite Deposition in organic solvent; At 60 ℃-150 ℃, heat 6h-12h, then by the ultrasonic 2h – of gained solution 12h, by solution centrifugal 5min – 30min under the rotating speed of 500r/min – 4000r/min, remove lower floor's solid, by gained solution suction filtration, obtain filter cake, filter cake is dried at 60 ℃, obtain fluorinated graphene material.
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