CN105355884B - Height ratio capacity lithium ion battery electrode material and preparation method thereof - Google Patents
Height ratio capacity lithium ion battery electrode material and preparation method thereof Download PDFInfo
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- CN105355884B CN105355884B CN201510829301.XA CN201510829301A CN105355884B CN 105355884 B CN105355884 B CN 105355884B CN 201510829301 A CN201510829301 A CN 201510829301A CN 105355884 B CN105355884 B CN 105355884B
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- 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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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/00—Electrodes
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- 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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
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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
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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Abstract
A kind of height ratio capacity lithium ion battery electrode material preparation method,Aoxidized including Hummers methods,Addition pyrroles prepares precursor solution,Prepare three dimensional gel,High temperature cabonization,Second of hydro-thermal reaction,Utilize graphene oxide,One-dimensional carbon material and pyrroles prepare three dimensional gel by hydro-thermal self-assembling reaction,Hydro-thermal reaction is total to transition metal salt after carbonization treatment again so as to which the doping of the transition metal oxide of generation finally to be prepared to the li-ion electrode materials of the three-dimensional self assembly of containing transition metal oxide in a three-dimensional structure,It is combined by transition metal oxide particle and three-dimensional carbon structure,So that the active material in electrode material reaches dispersed and has excellent electric conductivity and circulation specific capacity,The preparation method is simple simultaneously,It is low to prepare cost,Also provide a kind of height ratio capacity lithium ion battery electrode material simultaneously.
Description
Technical field
The invention belongs to chemical material field, more particularly, to a kind of lithium ion battery electrode material and preparation method thereof.
Background technology
The current energy, environmental problem generally turn into the most intractable two large problems in countries in the world, develop and utilize secondary energy sources
It will be the breach that solves the problems, such as.There is lithium ion battery high-energy-density, operating voltage height, memory-less effect etc. to be considered as two
Most there is the material of development potentiality in the secondary energy, it has in portable type electronic product, household electrical appliance, vehicles etc. widely should
With.But existing commercialization negative material is mainly graphite, its theoretical specific capacity only has 372mAh/g, it is difficult to meet lithium ion
Battery is applied in powerful device such as electric car, power network etc..It is, thus, sought for and exploitation efficiently, low consumption and cheap negative pole material
Expect to replace graphite be the key that solves the problems, such as, and study hotspot and difficult point.Transition metal oxide generally has than graphite
High 2~3 times of theoretical specific capacity, relatively low discharge platform, but have in charge and discharge process that volumetric expansion is big and poorly conductive this
Two big Important Problems, so as to cause, its capacity attenuation is rapid, cyclical stability is poor.
Recent study persons have carried out a series of research work to problem above, and some is by designing and preparing nanometer
The transition oxide of change, or by with mesoporous/micropore it is conductive it is carbon-based with transition metal it is compound wait it is tactful to its electrochemistry
It can make moderate progress but there is also following deficiency：1) nanosizing particle easily reunite, skewness；2) general porous, electrically conductive substrate
It is low for electrochemically inactive material, the overall volume specific capacity of material.Graphene as electrochemical active material, can realize lithium from
Son in its reversible storage there is bigger serface, good compliance and electric conductivity to be ground as transition metal Composite
The star's material studied carefully, but serious stacking phenomenon between layers be present in graphene.
In order to overcome, the graphene dispersion that graphene directly comes with transition metal composite band is uneven, transition metal reunion is tight
The phenomenon of weight, researcher use the transition metal for making to grow under high-temperature and high-pressure conditions to be dispersed in the system on graphene sheet layer
Standby method, or using the well-designed graphene such as template structure the methods of solve.These methods are relative complex, Gao Cheng
This, is unfavorable for industrialized preparation and production.
The content of the invention
The present invention proposes to solve the above problems, there is provided a kind of height ratio capacity lithium ion battery electrode material and
Its preparation method, electrode material prepared by this method have three-dimensional stability structure, can make that active material is uniformly dispersed and system is led
The characteristics of good electrical property, high circulation specific capacity, be the height ratio capacity lithium ion battery based on the compound three-dimensional self assembly of graphene
Electrode material.
Height ratio capacity lithium ion battery electrode material provided by the invention, it is complex carbon material, it is characterised in that：Contained
Metal oxide mass fraction is crossed as 30~80%.
Height ratio capacity lithium ion battery electrode material provided by the invention, can also have the feature that：Wherein, transition
Metal oxide is any one in tin, cobalt, manganese, iron, copper, nickel, tungsten, molybdenum, titanium oxide
The present invention also provides a kind of height ratio capacity lithium ion battery electrode material preparation method, comprises the following steps：
Step 1, graphene oxide, the one-dimensional carbon material inorganic acid that graphite is obtained using Hummers method oxidation processes
Washed down with deionized water, and be made into the graphene oxide water solution of suitable concn and the one-dimensional carbon material aqueous solution respectively；
Step 2, after graphene oxide water solution, the one-dimensional carbon material aqueous solution carry out ultrasonic disperse respectively in step 1
By pyrroles of the certain mass than being mixed and added into certain mass fraction, precursor solution is made；
Step 3, first time hydro-thermal reaction is carried out to the precursor solution obtained by step 2 using hydro-thermal reaction, then
Freeze-drying, obtains three dimensional gel；
Step 4, three dimensional gel made from step 3 is subjected to high temperature cabonization；
Step 5, it is anti-that the product after step 4 high temperature is carbonized carries out second of hydro-thermal after being mixed with transition metal salt
Should, the solid product being filtrated to get is cleaned through multiple deionized water, alcoholic solvent, the three-dimensional of containing transition metal oxide is made
The li-ion electrode materials of self assembly.
Height ratio capacity lithium ion battery electrode material preparation method provided by the invention, can also have the feature that：
Wherein, wherein, inorganic acid is any one or its mixed acid in hydrochloric acid, sulfuric acid, nitric acid.
Height ratio capacity lithium ion battery electrode material preparation method provided by the invention, can also have the feature that：
Wherein, wherein, suitable concn is 7~15mg/ml in step 1.
Height ratio capacity lithium ion battery electrode material preparation method provided by the invention, can also have the feature that：
Wherein, certain mass ratio is graphene oxide water solution quality in step 2：One-dimensional carbon material aqueous solution quality is 1:3~3:1,
Certain mass fraction is 1~5%.
Height ratio capacity lithium ion battery electrode material preparation method provided by the invention, can also have the feature that：
Wherein, first time hydrothermal reaction condition is 10~16 hours at a temperature of 160~200 DEG C in step 3, the condition of freeze-drying for-
Kept for 24~72 hours at a temperature of 40 DEG C~-80 DEG C.
Height ratio capacity lithium ion battery electrode material preparation method provided by the invention, can also have the feature that：
Wherein, the condition of step 4 high temperature cabonization is kept for 1~4 hour at a temperature of 800~1200 DEG C.
Height ratio capacity lithium ion battery electrode material preparation method provided by the invention, can also have the feature that：
Wherein, one-dimensional carbon material refers to single-walled carbon nanotube, multi-walled carbon nanotube, carbon nano rod, carbon nanocoils, carbon nanometer in step 1
Any one in rod, carbon fiber, transition metal salt is the nitrate of tin, cobalt, manganese, iron, copper, nickel, tungsten, molybdenum, titanium in step 5
With any one in hydrochloride.
Height ratio capacity lithium ion battery electrode material preparation method provided by the invention, can also have the feature that：
Wherein, the condition of second of hydro-thermal reaction is 12~20 hours at a temperature of 180~220 DEG C in step 5.
Invention effect and effect
Height ratio capacity lithium ion battery electrode material provided by the invention and preparation method thereof, utilizes graphene oxide, one
Dimension carbon material and pyrroles prepare three dimensional gel by hydro-thermal self-assembling reaction, then are total to hydro-thermal with transition metal salt after carbonization treatment
Reaction finally prepares containing transition metal oxide in a three-dimensional structure so as to which the transition metal oxide of generation be adulterated
The li-ion electrode materials of three-dimensional self assembly, it is combined by transition metal oxide particle and three-dimensional carbon structure so that electrode
Active material in material reaches dispersed and has excellent electric conductivity and circulation specific capacity, while preparation method letter
It is single, it is low to prepare cost.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the height ratio capacity lithium ion battery electrode material preparation method of the present invention；
Fig. 2 be the present invention height ratio capacity lithium ion battery electrode material be fabricated to the negative pole of lithium battery after, the battery
The curve map of capacity and efficiency for charge-discharge；
Fig. 3 be the present invention height ratio capacity lithium ion battery electrode material be fabricated to the negative pole of lithium battery after, the battery
Discharge capacity curve map under 0.5mA/g~10A/g charging and discharging currents density.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, it is real below
Example combination accompanying drawing is applied to be specifically addressed the height ratio capacity lithium ion battery electrode material preparation method of the present invention.
Embodiment 1
Fig. 1 is the schematic flow sheet of the height ratio capacity lithium ion battery electrode material preparation method of the present embodiment
Step 1 S1, oxidation.By graphite using Hummers methods (W.S.Hummers, R.E.Hoffeman,
J.Am.Chem.Soc.1958,80,1339 graphene oxide, one-dimensional carbon material hydrochloric acid and the deionization that) oxidation processes obtain
Water is washed down, and is made into the 10mg/ml aqueous solution respectively；
Step 2 S2, prepares precursor solution.Graphene oxide, one-dimensional carbon material obtained by step 1 are subjected to ultrasound respectively
In mass ratio 1 after scattered 30min:1 to be mixed and added into mass fraction be 2% pyrroles, so as to which precursor solution be made；
Step 3 S3, prepares three dimensional gel.180 DEG C are carried out to the precursor solution obtained by step 2 using hydro-thermal reaction
Lower 12h hydro-thermal reaction, 48h then is freeze-dried at -50 DEG C, obtains three dimensional gel；
Step 4 S4, high temperature cabonization.After three dimensional gel made from step 3 is placed in into 1050 DEG C of high temperature cabonization 2h,
Step 5 S5, second of hydro-thermal reaction.Product and transition metal salt after step 4 high temperature is carbonized, this implementation
Example is cleaned using the hydro-thermal reaction that second 16h at 200 DEG C is carried out after copper nitrate mixing, then through multiple deionized water, ethanol, from
And the li-ion electrode materials of the three-dimensional self assembly of containing transition metal oxide are made.
Embodiment 2
Step 1 S1, oxidation.By graphite using Hummers methods (W.S.Hummers, R.E.Hoffeman,
J.Am.Chem.Soc.1958,80,1339 graphene oxide, one-dimensional carbon material hydrochloric acid and the deionization that) oxidation processes obtain
Water is washed down, and is made into the 7mg/ml aqueous solution respectively；
Step 2 S2, prepares precursor solution.Graphene oxide, one-dimensional carbon material obtained by step 1 are subjected to ultrasound respectively
In mass ratio 1 after scattered 30min:3 to be mixed and added into mass fraction be 1% pyrroles, so as to which precursor solution be made；
Step 3 S3, prepares three dimensional gel.160 DEG C are carried out to the precursor solution obtained by step 2 using hydro-thermal reaction
Lower 16h hydro-thermal reaction, 72h then is freeze-dried at -40 DEG C, obtains three dimensional gel；
Step 4 S4, high temperature cabonization.After three dimensional gel made from step 3 is placed in into 800 DEG C of high temperature cabonization 4h,
Step 5 S5, second of hydro-thermal reaction.Product and transition metal salt after step 4 high temperature is carbonized, this implementation
Example is cleaned using the hydro-thermal reaction that second 20h at 180 DEG C is carried out after ferric nitrate mixing, then through multiple deionized water, ethanol, from
And the li-ion electrode materials of the three-dimensional self assembly of containing transition metal oxide are made.
Embodiment 3
Step 1 S1, oxidation.By graphite using Hummers methods (W.S.Hummers, R.E.Hoffeman,
J.Am.Chem.Soc.1958,80,1339 graphene oxide, one-dimensional carbon material hydrochloric acid and the deionization that) oxidation processes obtain
Water is washed down, and is made into the 15mg/ml aqueous solution respectively；
Step 2 S2, prepares precursor solution.Graphene oxide, one-dimensional carbon material obtained by step 1 are subjected to ultrasound respectively
In mass ratio 3 after scattered 60min:1 to be mixed and added into mass fraction be 5% pyrroles, so as to which precursor solution be made；
Step 3 S3, prepares three dimensional gel.200 DEG C are carried out to the precursor solution obtained by step 2 using hydro-thermal reaction
Lower 10h hydro-thermal reaction, 24h then is freeze-dried at -80 DEG C, obtains three dimensional gel；
Step 4 S4, high temperature cabonization.After three dimensional gel made from step 3 is placed in into 1200 DEG C of high temperature cabonization 1h,
Step 5 S5, second of hydro-thermal reaction.Product and transition metal salt after step 4 high temperature is carbonized, this implementation
Example is cleaned using the hydro-thermal reaction that second 12h at 220 DEG C is carried out after titanium tetrachloride mixing, then through multiple deionized water, ethanol,
So as to which the li-ion electrode materials of the three-dimensional self assembly of containing transition metal oxide be made.
By test, measure respectively in embodiment 1,2,3 transition metal oxide mass fraction (with normal condition most
Stable oxide conversion)
Tested through analysis, electrode material prepared by the above method is carbon composite, including above-mentioned transiting metal oxidation
Thing and complex carbon material.
In order to illustrate the high power capacity of li-ion electrode materials in the present embodiment through a step, the electricity examination of material is carried out below
Test.
Fig. 2 is the battery after the height ratio capacity lithium ion battery electrode material in this implementation is fabricated to the negative pole of lithium battery
Capacity and efficiency for charge-discharge curve map
The electrode material of the embodiment of the present invention 1 is fabricated to the negative pole of lithium battery, and test pair is used as using this lithium battery
As the model CT2001A manufactured using Wuhan Land Electronic Co., Ltd. multi-channel battery test instrument is to the survey
Try object and carry out electrochemical property test；The charging/discharging voltage window of test is 0.001~3V, charging and discharging currents 100mA/g,
Measured capacity and the curve map of efficiency for charge-discharge are as shown in figure 1, Fig. 1 transverse axis is cycle-index number axis, the right side in Fig. 1
Vertical pivot is coulombic efficiency number axis, and the lefthand vertical axis in Fig. 1 is capacity number axis, and the curve 1 in Fig. 1 is coulombic efficiency curve, in Fig. 1
Curve 2 be capacity curve, from figure 1 it appears that the discharge capacity first of test object in 1700mAh/g or so, is passed through
After 100 charge and discharge cycles, the capacity of test object is stable in 600mAh/g, and in addition to preceding circulation several times, coulombic efficiency is all the time
Maintain more than 95%, it can be seen that test object has high power capacity and excellent cycling stability.
Fig. 3 is the battery after the height ratio capacity lithium ion battery electrode material of the present embodiment is fabricated to the negative pole of lithium battery
The discharge capacity curve map under 0.5mA/g~10A/g charging and discharging currents density
The electrode material of the embodiment of the present invention 1 is fabricated to the negative pole of lithium battery, and test pair is used as using this lithium battery
As the model CT2001A manufactured using Wuhan Land Electronic Co., Ltd. multi-channel battery test instrument is to the survey
Try object and carry out electrochemical property test, the measured discharge capacity under 0.5mA/g~10A/g charging and discharging currents density is bent
Line as shown in Fig. 2 figure it is seen that the test object under different current density conditions, still has higher capacity,
Especially under the so high current densities of 10A/g, battery still has certain capacity, and therewith in 0.1A/g electric currents
600mAh/g or so capacity can be completely recovered under density again.
The effect of embodiment and beneficial effect
This series implements height ratio capacity lithium ion battery electrode material provided and preparation method thereof, utilizes graphite oxide
Alkene, one-dimensional carbon material and pyrroles prepare three dimensional gel by hydro-thermal self-assembling reaction, then after carbonization treatment with transition metal salt
Hydro-thermal reaction finally prepares containing transition metal oxygen in a three-dimensional structure so as to which the transition metal oxide of generation be adulterated altogether
The li-ion electrode materials of the three-dimensional self assembly of compound, it is combined by transition metal oxide particle and three-dimensional carbon structure, make
The active material in electrode material is obtained to reach dispersed and there is excellent electric conductivity and circulation specific capacity, while the preparation
Method is simple, and it is low to prepare cost.
Claims (8)
1. a kind of height ratio capacity lithium ion battery electrode material preparation method, it is characterised in that comprise the following steps：
Step 1, the graphene oxide that graphite is obtained using Hummers method oxidation processes, one-dimensional carbon material inorganic acid and goes
Ionized water is washed down, and is made into the graphene oxide water solution of suitable concn and the one-dimensional carbon material aqueous solution respectively；
Step 2, graphene oxide water solution described in step 1, the one-dimensional carbon material aqueous solution are subjected to ultrasound point respectively
By pyrroles of the certain mass than being mixed and added into certain mass fraction after dissipating, precursor solution is made；
Step 3, first time hydro-thermal reaction is carried out to the precursor solution obtained by step 2 using hydro-thermal reaction, then
Freeze-drying, obtains three dimensional gel；
Step 4, the three dimensional gel made from step 3 is subjected to high temperature cabonization；
Step 5, the product after step 4 high temperature is carbonized carry out second of hydro-thermal reaction after being mixed with transition metal salt, will
The solid product being filtrated to get cleans through multiple deionized water, alcoholic solvent, and the three-dimensional from group of containing transition metal oxide is made
The li-ion electrode materials of dress,
Wherein, mass fraction of the li-ion electrode materials containing the transition metal oxide is 30~80%.
2. height ratio capacity lithium ion battery electrode material preparation method according to claim 1, it is characterised in that:
Wherein, inorganic acid is any one in hydrochloric acid, sulfuric acid, nitric acid or its mixed acid.
3. height ratio capacity lithium ion battery electrode material preparation method according to claim 1, it is characterised in that：
Wherein, suitable concn described in step 1 is 7~15mg/ml.
4. height ratio capacity lithium ion battery electrode material preparation method according to claim 1, it is characterised in that：
Wherein, the ratio of certain mass described in step 2 is that the graphene oxide water solution quality and the one-dimensional carbon material are water-soluble
The ratio of liquid quality, the ratio are 1:3~3:1,
The certain mass fraction is 1~5%.
5. height ratio capacity lithium ion battery electrode material preparation method according to claim 1, it is characterised in that：
Wherein, first time hydrothermal reaction condition described in step 3 is the freezing 10~16 hours at a temperature of 160~200 DEG C
Dry condition is kept for 24~72 hours at a temperature of being -40 DEG C~-80 DEG C.
6. height ratio capacity lithium ion battery electrode material preparation method according to claim 1, it is characterised in that：
Wherein, the condition of high temperature cabonization described in step 4 is kept for 1~4 hour at a temperature of 800~1200 DEG C.
7. height ratio capacity lithium ion battery electrode material preparation method according to claim 1, it is characterised in that:
Wherein, one-dimensional carbon material described in step 1 refers to single-walled carbon nanotube, multi-walled carbon nanotube, carbon nano rod, carbon nanometer
Any one in line, carbon nanometer rod, carbon fiber,
Transition metal salt described in step 5 is appointing in the nitrate and hydrochloride of tin, cobalt, manganese, iron, copper, nickel, tungsten, molybdenum, titanium
Meaning is a kind of.
8. height ratio capacity lithium ion battery electrode material preparation method according to claim 1, it is characterised in that：
Wherein, the condition of second of hydro-thermal reaction described in step 5 is 12~20 hours at a temperature of 180~220 DEG C.
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| CN105810917A (en) * | 2016-05-24 | 2016-07-27 | 刘高志 | Preparation of SnO2-Cr2O3-graphene composite and application thereof in negative electrode of lithium ion cell |
| CN107808779B (en) * | 2016-09-08 | 2019-10-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon nanotube/three-dimensional graphene composite material, preparation method and application |
| CN106848229B (en) * | 2017-02-03 | 2020-07-03 | 南京邮电大学 | Preparation method of metal organic compound cathode material |
| CN107316999B (en) * | 2017-06-06 | 2020-03-20 | 上海理工大学 | Partially-amorphized tin dioxide three-dimensional self-assembled lithium ion electrode material based on graphene compounding and preparation method thereof |
| CN108258210B (en) * | 2017-12-29 | 2020-08-04 | 山西大学 | Preparation method of 3D porous graphene/carbon nanotube-nano silicon aerogel lithium ion battery cathode material |
| CN108550824B (en) * | 2018-04-28 | 2020-08-04 | 上海理工大学 | Preparation method of high-capacity battery negative electrode material |
| CN110635127B (en) * | 2019-10-31 | 2021-05-14 | 扬州工业职业技术学院 | Lithium ion battery electrode material based on metal molybdate compound nano material |
| CN111628176B (en) * | 2020-06-17 | 2022-01-28 | 苏州盟维动力科技有限公司 | Multi-component three-dimensional conductive carbon network, self-supporting composite electrode, and preparation methods and applications thereof |
| CN113130862B (en) * | 2021-03-10 | 2022-04-26 | 东南大学 | Three-dimensional graphene composite material and preparation method and application thereof |
| CN114068195B (en) * | 2021-11-18 | 2023-06-06 | 四川金汇能新材料股份有限公司 | Carbon negative electrode material compounded with metal and preparation method thereof |
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| CN1601786A (en) * | 2003-09-26 | 2005-03-30 | 中国科学院物理研究所 | Oxygen-contg composite carbon material for secondary lithium cell, its prepn process and usage |
| US9697931B2 (en) * | 2011-12-22 | 2017-07-04 | Korea Institute Of Industrial Technology | Method of preparing large-area, three-dimensional graphene transparent electrode using electrospray process and large-area, three-dimensional graphene transparent electrode prepared therefrom |
| CN103311541B (en) * | 2012-03-08 | 2015-11-18 | 中国科学院金属研究所 | A kind of lithium ion battery composite cathode material and preparation method thereof |
| CN102826543B (en) * | 2012-09-19 | 2014-05-28 | 北京理工大学 | Preparation method of foamable three-dimensional graphene |
| CN102931408B (en) * | 2012-11-21 | 2015-09-23 | 大连海洋大学 | Graphene composite transition metal oxide nanofiber lithium ion battery electrode and preparation method thereof |
| CN104617274B (en) * | 2015-02-10 | 2016-08-24 | 哈尔滨理工大学 | A kind of preparation method of flexible Tin monoxide nanometer sheet/CNT-grapheme foam three-dimensional composite material |
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