CN106920962A - A kind of nickel oxide/graphite composite nano materials for lithium ion battery and preparation method and application - Google Patents
A kind of nickel oxide/graphite composite nano materials for lithium ion battery and preparation method and application Download PDFInfo
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- CN106920962A CN106920962A CN201710279447.0A CN201710279447A CN106920962A CN 106920962 A CN106920962 A CN 106920962A CN 201710279447 A CN201710279447 A CN 201710279447A CN 106920962 A CN106920962 A CN 106920962A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of nickel oxide/graphite composite nano materials for lithium ion battery and preparation method and application, belong to lithium ion battery material technical field.The method is comprised the following steps：First by graphite, anhydrous nitric acid sodium and concentrated nitric acid are mixed, and washing is dried to obtain acidifying graphite.Again by acidifying graphite and nickel hydroxide ball milling, calcining obtains nickel oxide/graphite composite nano materials.When gained nickel oxide/graphite composite nano materials of the invention are used for lithium ion battery negative, with good chemical property, in 200mA g‑1Current density under circulation 50 times afterwards, remain to keep 861 mAh g‑1Reversible capacity, and in high current density（1200mA g‑1）Under conditions of, reversible capacity is maintained to 602mAh g‑1More than.
Description
Technical field
The invention belongs to lithium ion battery material technical field, and in particular to a kind of nickel oxide for lithium ion battery/
Graphite composite nano materials and preparation method and application.
Background technology
With the generation of energy crisis and increasingly serious environmental problem, in the urgent need to a kind of novel energy replaces coal, stone
The non-renewable energy resources such as oil.Rechargeable lithium ion batteries can cause people great as the energy storage carrier of green energy resource
Concern.Theoretical capacity (the 372mAh g of commercial Li-ion batteries negative material graphite-1) relatively low, it has been insufficient for increasingly increasing
Energy requirement long, therefore find with cheap, having extended cycle life, energy density high, reversible capacity high is excellent
The lithium ion battery negative material of the advantages of high rate performance and cyclical stability is particularly important.
Transition metal oxide (MxOy,M:Fe, Co, Ni, Mn) possess theoretical capacity and special storage lithium machine higher
Reason：MxOy+2yLi++2ye-→yLi2O+xM is thus the lithium ion battery negative material of new generation of most development and application potentiality
Material.
Wherein NiO is due to its extensive purposes, such as catalyst, and gas sensor, magnetic material and lithium ion battery are negative
Pole material etc., is widely studied and is paid close attention to.Used as very attractive lithium ion battery negative material NiO, it has
There is low potential, low cost, hypotoxicity, theoretical capacity (717mAh g safer compared to other transition metal oxides and high-1),
Numerous advantages such as volume energy density (about 5.8 times of graphite) high.But in cyclic process, ionic conductivity is poor, NiO hairs
Larger volumetric expansion of life etc. constrains the performance of the chemical property of NiO.
There are some researches show the nanometer particle size for reducing NiO can not only shorten Li+ diffusion lengths, can also increase electrode and electricity
The contact area of matter is solved, so as to improve cyclical stability.But the maximum problem of nano material is exactly easily to reunite so as to cause more
Many problems, and add carbon black or the conducting polymer can be improved these problems.Zhang et al. is obtained using hydro-thermal method
Nickel oxide (NiO-C) nano particle of carbon coating, and it is used as lithium ion battery negative material.In 100mAh g-1Electric current
Under density after the circle of circulation 50, reversible capacity remains at 706.9mAh g-1。
The present invention successfully synthesizes nano-nickel oxide NiO of the uniform load on graphite flake by simple ball-milling technology
Particle.When lithium ion battery negative material, nickel oxide/graphite composite nano materials have excellent cyclical stability,
In 200mAh g-1Current density under circulation 50 circle after, material can keep 861mAh g-1Reversible capacity, in 1200mAh g-1
High current density under, material also has 602mAh g-1Reversible capacity.The present invention has process is simple, and low in raw material price is easy
, low cost, efficiency high, advantages of environment protection can be with large-scale industrial application.
The content of the invention
Primary and foremost purpose of the invention is to provide a kind of nickel oxide/graphite composite nano materials.
Low cost, high efficiency it is a further object of the present invention to provide above-mentioned nickel oxide/graphite composite nano materials, can be big
Method prepared by scale.
Another object of the present invention is to provide above-mentioned nickel oxide/graphite composite nano materials as high performance lithium ion battery
The application process of negative material.
Mesh of the present invention is achieved through the following technical solutions.
A kind of preparation method of nickel oxide/graphite composite nano materials for lithium ion battery, comprises the following steps：
(1) graphite and anhydrous nitric acid sodium are put into reactor, stirring is lower to add concentrated nitric acid, in being washed with water to after reaction
Property, dry, obtain acidifying graphite；
(2) nickel hydroxide/graphite composite Nanos by acidifying graphite, nickel hydroxide and ball mixing and ball milling then isolated
Material；
(3) in a nitrogen atmosphere, nickel hydroxide/graphite composite nano materials are positioned in tube furnace and are calcined, obtain oxygen
Change nickel/graphite composite nano materials.
Preferably, step (1) described graphite is the one kind or many in natural flake graphite, native graphite and Delanium
Kind.
Preferably, the time of step (1) described reaction is 12 hours 12 hours.
Preferably, step (2) ball and the mass ratio of raw material are 20:1-20:10, the raw material include acidifying graphite and
Nickel hydroxide.
Preferably, rotating speed during step (2) described ball milling is 300~500rpm；Ball-milling Time is 24-48h.
Preferably, the temperature of step (3) described calcining is 250-450 DEG C；Time is 2-4h.
Preferably, a kind of preparation method of nickel oxide/graphite composite nano materials is as follows：
30g natural flake graphites are weighed, 15g anhydrous nitric acid sodium is put into 100ml beakers, under magnetic agitation, is slowly added to
60ml concentrated nitric acids, stirring is washed with distilled water to pH in neutrality after 12 hours, be dried to obtain acidifying graphite standby.By different proportion
The graphite and nickel hydroxide of acidifying are weighed, the mass ratio of zirconium ball, zirconium ball and raw material (including acidifying graphite and nickel hydroxide) is added
It is 20:1, under 300~500rpm rotating speeds, ball milling 48h, isolated nickel hydroxide/graphite composite nano materials, in nitrogen
Under atmosphere, in 2h is calcined at 350 DEG C in placement tube furnace, nickel oxide/graphite composite nano materials are obtained.
Ball milling mainly has following two effects in the present invention；(1) number of plies of graphite is efficiently reduced；(2) hydroxide is caused
Nickel is evenly dispersed on the graphite flake peeled off.
A kind of nickel oxide/graphite composite nano materials as obtained in the process described above, it is preferred that the nickel oxide/stone
The mass fraction of graphite is 1~30% in black composite nano materials；It is further preferred that the mass fraction of graphite is 10%.
A kind of above-described nickel oxide/application of the graphite composite nano materials in lithium ion battery negative is prepared.
Preferably, the application is comprised the following steps：Nickel oxide/graphite composite nano materials, carbon black and PVDF are mixed and is made
Slurry, is then coated on Copper Foil, obtains lithium ion battery negative.
Preferably, the application specifically includes following steps：Weigh 0.2g nickel oxide/graphite composite powder, 0.025g carbon blacks,
0.025g PVDF, in being transferred to vial after being fully ground in mortar, add 1ml NMP, by material after magnetic agitation 30min
Material is uniformly coated on electrode is made on Copper Foil, using lithium metal as to electrode, being assembled into CR2016 type buttons in glove box
Battery.In full battery applications, then lithium metal is changed into electrode that lithium cell positive material is made to electrode.
Compared with prior art, the invention has the advantages that and beneficial effect：
(1) present invention uses nitric acid dousing graphite, between oxygen-containing functional group successfully is inserted in into graphite flake, so that graphite passes through
The number of plies can be reduced after ball milling.
(2) present invention uses simple ball-milling method, has synthesized nickel oxide/graphite composite nano materials and has successfully been applied
In lithium ion battery negative material.Nickel oxide nanoparticle is dispersed in the graphite surface of stripping, effectively alleviates circulating battery mistake
The influence that nickel oxide volumetric expansion brings in journey, the addition of graphite inhibits the reunion of nickel oxide, and reaction contact area increases,
Ionic conductivity is also improved, so as to improve the chemical property of material.
(3) present invention uses simple ball-milling method, using mechanical shear stress, native graphite successfully is peeled off into few number of plies
Graphite.
(4) nickel hydroxide used by the present invention is commercially available general reagent, and graphite used is cheap, and the present invention
Method used is ball-milling method, so being adapted to fairly large synthesis.At the same time, the present invention also has preparation process is simple, environment
Friendly the advantages of.Thus, potential of the present invention with large-scale industrial production.
(5) with good circulation when nickel oxide of the invention/graphite composite nano materials are for lithium ion battery negative
Performance：Described composite nano materials, when mass content of graphite is 10%, are 200mA g in current density-1Lower discharge and recharge 50
After secondary, reversible capacity is 861mAh g-1, in 1200mAh g-1High current density under, material also has 602mAh g-1It is reversible
Capacity.It can be seen that ion cathode material lithium cycle performance prepared by the present invention is preferably, reversible capacity is higher.
Brief description of the drawings
Fig. 1 is the XRD of embodiment 1-4 gained nickel hydroxide/graphite composite nano materials.
Fig. 2 is the XRD of embodiment 1-4 gained nickel oxide/graphite composite nano materials.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1
30g natural flake graphites are weighed successively, and 15g anhydrous nitric acid sodium is put into 100ml beakers, under magnetic agitation, dropwise
60ml concentrated nitric acids are added, stirring is washed with distilled water to pH in neutrality, is dried to obtain acidifying graphite after 12 hours.Weigh successively
0.3596g acidifying graphites, 8.9904g nickel hydroxides, 187g zirconiums ball (mill is situated between) is added in ball grinder, adds sealing ring,
Ball milling 48h under 400rpm, the sample that will be obtained leaches zirconium ball through screen cloth, obtains nickel hydroxide/graphite composite nano materials.By institute
Obtain material to be positioned in tube furnace, in a nitrogen atmosphere, 350 DEG C are warming up to the speed for heating up 5 DEG C per minute, insulation 2h is obtained
Nickel oxide/graphite composite nano materials.
0.2g nickel oxide/graphite composite nano materials, 0.025g carbon blacks, 0.025g PVDF are weighed, is fully ground in mortar
It is transferred in vial after mill, adds 1ml NMP, material is uniformly coated on after magnetic agitation 30min electrode is made on Copper Foil,
Using lithium metal as to electrode, being assembled into CR2016 type button cells in glove box, then to the CR2016 type button cells
Carry out electrochemical property test.
Embodiment 2
30g natural flake graphites are weighed successively, and 15g anhydrous nitric acid sodium is put into 100ml beakers, under magnetic agitation, dropwise
60ml concentrated nitric acids are added, stirring is washed with distilled water to pH in neutrality, is dried to obtain acidifying graphite after 12 hours.Weigh successively
0.7670g acidifying graphites, 8.5826g nickel hydroxides, 187g zirconiums ball (mill is situated between) is added in ball grinder, adds sealing ring,
Ball milling 48h under 400rpm, the sample that will be obtained leaches zirconium ball through screen cloth, obtains nickel hydroxide/graphite composite nano materials.By institute
Obtain material to be positioned in tube furnace, in a nitrogen atmosphere, 350 DEG C are warming up to the speed for heating up 5 DEG C per minute, insulation 2h is obtained
Nickel oxide/graphite composite nano materials.
0.2g nickel oxide/graphite composite nano materials, 0.025g carbon blacks, 0.025g PVDF are weighed, is fully ground in mortar
It is transferred in vial after mill, adds 1ml NMP, material is uniformly coated on after magnetic agitation 30min electrode is made on Copper Foil,
Using lithium metal as to electrode, being assembled into CR2016 type button cells in glove box, then to the CR2016 type button cells
Carry out electrochemical property test.
Embodiment 3
30g natural flake graphites are weighed successively, and 15g anhydrous nitric acid sodium is put into 100ml beakers, under magnetic agitation, dropwise
60ml concentrated nitric acids are added, stirring is washed with distilled water to pH in neutrality, is dried to obtain acidifying graphite after 12 hours.Weigh successively
1.5677g acidifying graphites, 7.7819g nickel hydroxides, 187g zirconiums ball (mill is situated between) is added in ball grinder, adds sealing ring,
Ball milling 48h under 400rpm, the sample that will be obtained leaches zirconium ball through screen cloth, obtains nickel hydroxide/graphite composite nano materials.By institute
Obtain material to be positioned in tube furnace, in a nitrogen atmosphere, 350 DEG C are warming up to the speed for heating up 5 DEG C per minute, insulation 2h is obtained
Nickel oxide/graphite composite nano materials.
0.2g nickel oxide/graphite composite nano materials, 0.025g carbon blacks, 0.025g PVDF are weighed, is fully ground in mortar
It is transferred in vial after mill, adds 1ml NMP, material is uniformly coated on after magnetic agitation 30min electrode is made on Copper Foil,
Using lithium metal as to electrode, being assembled into CR2016 type button cells in glove box, then to the CR2016 type button cells
Carry out electrochemical property test.
Embodiment 4
30g natural flake graphites are weighed successively, and 15g anhydrous nitric acid sodium is put into 100ml beakers, under magnetic agitation, dropwise
60ml concentrated nitric acids are added, stirring is washed with distilled water to pH in neutrality, is dried to obtain acidifying graphite after 12 hours.Weigh successively
2.4g acidifying graphites, 6.9496g nickel hydroxides, 187g zirconiums ball (mill is situated between) is added in ball grinder, sealing ring is added, in 400rpm
Lower ball milling 48h, the sample that will be obtained leaches zirconium ball through screen cloth, obtains nickel hydroxide/graphite composite nano materials.By resulting materials
It is positioned in tube furnace, in a nitrogen atmosphere, 350 DEG C is warming up to the speed for heating up 5 DEG C per minute, insulation 2h is aoxidized
Nickel/graphite composite nano materials.
0.2g nickel oxide/graphite composite nano materials, 0.025g carbon blacks, 0.025g PVDF are weighed, is fully ground in mortar
It is transferred in vial after mill, adds 1ml NMP, material is uniformly coated on after magnetic agitation 30min electrode is made on Copper Foil,
Using lithium metal as to electrode, being assembled into CR2016 type button cells in glove box, then to the CR2016 type button cells
Carry out electrochemical property test.
Embodiment 5
30g natural flake graphites are weighed successively, and 15g anhydrous nitric acid sodium is put into 100ml beakers, under magnetic agitation, dropwise
60ml concentrated nitric acids are added, stirring is washed with distilled water to pH in neutrality, is dried to obtain acidifying graphite after 4 hours.Weigh successively
2.4g acidifying graphites, 6.9496g nickel hydroxides, 34g zirconiums ball (mill is situated between) is added in ball grinder, adds sealing ring, at 300 rpm
Ball milling 48h, the sample that will be obtained leaches zirconium ball through screen cloth, obtains nickel hydroxide/graphite composite nano materials.Resulting materials are put
Be placed in tube furnace, in a nitrogen atmosphere, 350 DEG C be warming up to 5 DEG C of the speed of heating up per minute, insulation 2h obtain nickel oxide/
Graphite composite nano materials.
0.2g nickel oxide/graphite composite nano materials, 0.025g carbon blacks, 0.025g PVDF are weighed, is fully ground in mortar
It is transferred in vial after mill, adds 1ml NMP, material is uniformly coated on after magnetic agitation 30min electrode is made on Copper Foil,
Using lithium metal as to electrode, being assembled into CR2016 type button cells in glove box, then to the CR2016 type button cells
Carry out electrochemical property test.
Embodiment 6
30g natural flake graphites are weighed successively, and 15g anhydrous nitric acid sodium is put into 100ml beakers, under magnetic agitation, dropwise
60ml concentrated nitric acids are added, stirring is washed with distilled water to pH in neutrality, is dried to obtain acidifying graphite after 8 hours.Weigh successively
2.4g acidifying graphites, 6.9496g nickel hydroxides, 18.7g zirconiums ball (mill is situated between) is added in ball grinder, sealing ring is added, in 500rpm
Lower ball milling 48h, the sample that will be obtained leaches zirconium ball through screen cloth, obtains nickel hydroxide/graphite composite nano materials.By resulting materials
It is positioned in tube furnace, in a nitrogen atmosphere, 350 DEG C is warming up to the speed for heating up 5 DEG C per minute, insulation 2h is aoxidized
Nickel/graphite composite nano materials.
0.2g nickel oxide/graphite composite nano materials, 0.025g carbon blacks, 0.025g PVDF are weighed, is fully ground in mortar
It is transferred in vial after mill, adds 1ml NMP, material is uniformly coated on after magnetic agitation 30min electrode is made on Copper Foil,
Using lithium metal as to electrode, being assembled into CR2016 type button cells in glove box, then to the CR2016 type button cells
Carry out electrochemical property test.
Embodiment 7
30g natural flake graphites are weighed successively, and 15g anhydrous nitric acid sodium is put into 100ml beakers, under magnetic agitation, dropwise
60ml concentrated nitric acids are added, stirring is washed with distilled water to pH in neutrality, is dried to obtain acidifying graphite after 4 hours.Weigh successively
2.4g acidifying graphites, 6.9496g nickel hydroxides, 187g zirconiums ball (mill is situated between) is added in ball grinder, sealing ring is added, in 400rpm
Lower ball milling 36h, the sample that will be obtained leaches zirconium ball through screen cloth, obtains nickel hydroxide/graphite composite nano materials.By resulting materials
It is positioned in tube furnace, in a nitrogen atmosphere, 425 DEG C is warming up to the speed for heating up 5 DEG C per minute, insulation 4h is aoxidized
Nickel/graphite composite nano materials.
0.2g nickel oxide/graphite composite nano materials, 0.025g carbon blacks, 0.025g PVDF are weighed, is fully ground in mortar
It is transferred in vial after mill, adds 1ml NMP, material is uniformly coated on after magnetic agitation 30min electrode is made on Copper Foil,
Using lithium metal as to electrode, being assembled into CR2016 type button cells in glove box, then to the CR2016 type button cells
Carry out electrochemical property test.
Embodiment 8
30g natural flake graphites are weighed successively, and 15g anhydrous nitric acid sodium is put into 100ml beakers, under magnetic agitation, dropwise
60ml concentrated nitric acids are added, stirring is washed with distilled water to pH in neutrality, is dried to obtain acidifying graphite after 4 hours.Weigh successively
2.4g acidifying graphites, 6.9496g nickel hydroxides, 187g zirconiums ball (mill is situated between) is added in ball grinder, sealing ring is added, in 400rpm
Lower ball milling 24h, the sample that will be obtained leaches zirconium ball through screen cloth, obtains nickel hydroxide/graphite composite nano materials.By resulting materials
It is positioned in tube furnace, in a nitrogen atmosphere, 500 DEG C is warming up to the speed for heating up 5 DEG C per minute, insulation 3h is aoxidized
Nickel/graphite composite nano materials.
0.2g nickel oxide/graphite composite nano materials, 0.025g carbon blacks, 0.025g PVDF are weighed, is fully ground in mortar
It is transferred in vial after mill, adds 1ml NMP, material is uniformly coated on after magnetic agitation 30min electrode is made on Copper Foil,
Using lithium metal as to electrode, being assembled into CR2016 type button cells in glove box, then to the CR2016 type button cells
Carry out electrochemical property test.
Performance test
Nickel hydroxide/graphite composite nano materials prepared by above-described embodiment 1-4 and nickel oxide/graphite composite nano materials
It is analyzed using X-ray diffraction technology (XRD), as a result as shown in Fig. 1 and Fig. 2.
Battery prepared by above-described embodiment is soft using cell tester (the new prestige in Shenzhen) and BTS7.5.5 after 12h is shelved
Part, test temperature is room temperature, and current density is 200mA g-1~1200mA g-1In the case of, constant current charge-discharge is carried out to it
(discharge cut-off voltage is 0.01V, and charging voltage is 3V), tests the cycle performance and high rate performance of battery.Each implementation of the invention
The cycle performance of the battery prepared by example is shown in Table 1, table 2 with high rate performance test result.
Table 1
Note：" content of graphite " refers to the mass fraction of graphite in nickel oxide/graphite composite nano materials in table.
Table 2
The present invention is prepared for nickel oxide/graphite composite nano materials using ball-milling method, by changing the ratio that graphite is added
Carry out the optimal proportion of the synthesis condition and graphite input amount of research material in the range of 1-30%, and analyze following for respective material
Ring performance and high rate performance etc..By comparing 8 embodiments, the sample that the original input amount of graphite (with respect to nickel oxide) is 10% is found
Product, with good cycle performance, can be in 200mA g-1Under current density 860mA h g are kept after the circle of circulation 50-1With
On reversible capacity, in 1200mA h g-1High current density under, material also has 602mA h g-1Reversible capacity.
Embodiment is not limited for the present invention preferably implementation method, but embodiments of the present invention by above-described embodiment
System, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. the preparation method of a kind of nickel oxide/graphite composite nano materials for lithium ion battery, it is characterised in that including with
Lower step：
（1）Graphite, anhydrous nitric acid sodium and concentrated nitric acid are mixed, then is washed, dried, obtain acidifying graphite；
（2）By acidifying graphite and nickel hydroxide ball milling, then isolated nickel hydroxide/graphite composite nano materials；
（3）In a nitrogen atmosphere, nickel hydroxide/graphite composite nano materials are positioned in tube furnace and calcined, obtain nickel oxide/
Graphite composite nano materials.
2. preparation method according to claim 1, it is characterised in that step（1）The graphite is natural flake graphite, day
One or more in right graphite and Delanium.
3. preparation method according to claim 1, it is characterised in that step（1）The time of the stirring is 4-12 hours.
4. preparation method according to claim 1, it is characterised in that step（2）The quality of ball and raw material in the ball milling
Than being 20:1-20:10, the raw material includes acidifying graphite and nickel hydroxide.
5. preparation method according to claim 1, it is characterised in that step（2）The rotating speed during ball milling for 300 ~
500rpm；Ball-milling Time is 24-48h.
6. preparation method according to claim 1, it is characterised in that step（3）The temperature of the calcining is 250-450
℃；Time is 2-4h.
7. a kind of nickel oxide/graphite composite nano materials obtained in the method as described in claim any one of 1-6.
8. a kind of nickel oxide/graphite composite nano materials according to claim 7, it is characterised in that the nickel oxide/graphite
The mass fraction of graphite is 1 ~ 30% in composite nano materials.
9. a kind of nickel oxide described in claim 7/application of the graphite composite nano materials in lithium ion battery negative is prepared.
10. application according to claim 9, it is characterised in that the application is comprised the following steps：Nickel oxide/graphite is multiple
Nano material, carbon black and PVDF mixed pulps are closed, is then coated on Copper Foil, obtain lithium ion battery negative.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110137471A (en) * | 2019-05-16 | 2019-08-16 | 常熟理工学院 | A kind of nickel oxide and micro crystal graphite compound and its preparation method and application |
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| CN104599863A (en) * | 2015-01-15 | 2015-05-06 | 华东理工大学 | Method for preparation of composite material, composite material and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104599863A (en) * | 2015-01-15 | 2015-05-06 | 华东理工大学 | Method for preparation of composite material, composite material and application thereof |
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| 陈智栋等: "氧化镍/膨胀石墨复合物的合成及其电容性能", 《电子元件与材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110137471A (en) * | 2019-05-16 | 2019-08-16 | 常熟理工学院 | A kind of nickel oxide and micro crystal graphite compound and its preparation method and application |
| CN110137471B (en) * | 2019-05-16 | 2020-08-11 | 常熟理工学院 | Nickel oxide and microcrystalline graphite compound and preparation method and application thereof |
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Application publication date: 20170704 |