CN105845936A - Preparation method of modified hard carbon negative electrode material for lithium ion battery - Google Patents
Preparation method of modified hard carbon negative electrode material for lithium ion battery Download PDFInfo
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- CN105845936A CN105845936A CN201610164343.0A CN201610164343A CN105845936A CN 105845936 A CN105845936 A CN 105845936A CN 201610164343 A CN201610164343 A CN 201610164343A CN 105845936 A CN105845936 A CN 105845936A
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- hard carbon
- lithium ion
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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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- 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 preparation method of a modified hard carbon negative electrode material for a lithium ion battery, wherein the preparation method comprises the following steps: 1) firstly, adding phenol and a strong alkali to a formaldehyde solution or an acetaldehyde solution, to obtain a water-soluble phenolic resin; 2) adding ammonium persulfate into the water-soluble phenolic resin prepared in the step 1), after being completely dissolved, adding an equal volume of vegetable oil, mixing evenly, then pouring the mixed solution into a hydrothermal reaction kettle, and carrying out a reaction to obtain a solid-state hard carbon precursor; 3) under the protection of nitrogen or inert gas, heating the solid-state hard carbon precursor obtained in the step 2) up to obtain hard carbon; 4) ball-milling or crushing the hard carbon; and 5) adding a carbon source in the hard carbon matrix, mixing evenly, carrying out heat preservation heating to obtain the modified hard carbon negative electrode material for the lithium ion battery. The modified hard carbon negative electrode material has excellent electrochemical performance, has excellent lithium intercalation and removal capacities; the first discharge specific capacity is 400 mAh/g or more, in the best embodiment, the first discharge specific capacity is up to 503 mAh/g, the first charge/discharge efficiency is up to 94.5%, and the modified hard carbon negative electrode material is applicable to power and energy storage lithium ion batteries.
Description
Technical field
The present invention relates to electrode field technology, particularly provide a kind of lithium ion battery to bear with modified hard charcoal
The preparation method of pole material.
Background technology
Along with the continuous intensification of global energy crisis, the increasingly exhausted and atmospheric pollution of petroleum resources,
The harm aggravation of global warning, development clean energy resource is imperative.In new forms of energy develop, tool
Have that running voltage is high, energy density big, discharging voltage balance, have extended cycle life and environmental friendliness etc.
The lithium ion battery of advantage finds broad application.Negative material is that evaluation lithium ion battery combination property is excellent
One of bad key factor.The lithium cell cathode material that commercialization at present uses is mainly graphite, graphite
Material is high due to degree of graphitization, and the layer structure with height causes embedding lithium under high current charge-discharge to hold
Measure relatively low.Along with development and the continuous progress of science and technology of social productive forces, hard carbon is negative material
Lithium ion battery, owing to the structure that its hard carbon cathode material is special is allowed to preferably at large current density
Electricity is lower to be used and receives much concern.With graphite-phase ratio, it is good with electrolyte compatibility (special that hard charcoal also has
PC system electrolyte) feature.But its electrode potential is high, current potential delayed and first efficiency low etc.
Problem is the most effectively solved.
Summary of the invention
In view of this, the present invention is directed to the disappearance of prior art existence, it is an object of the invention to provide
The preparation method of the modified hard carbon cathode material of a kind of lithium ion battery, the hard carbon cathode material obtained has
There are high power capacity, high charge-discharge efficiencies and high-rate charge-discharge capability.
For achieving the above object, the present invention uses such as purgation technical scheme: a kind of lithium ion battery is with changing
The preparation method of the hard carbon cathode material of property, comprises the following steps that
1) first, in formalin or acetaldehyde solution, phenol, highly basic are added, 50-80 DEG C of temperature
Degree lower stirring reaction 5-12h, obtains water soluble phenol resin；
2) Ammonium persulfate. is added above-mentioned steps 1) water soluble phenol resin prepared, wait to be completely dissolved
After complete, adding isopyknic vegetable oil, mix homogeneously is fallen back in thermal response still, is placed in power and is
In the microwave oven of 600～2000w, heat 10～600s, filter after having reacted, wash with water and ethanol
Wash 3-10 time, at a temperature of 40 DEG C, obtain the hard carbon precursor of solid-state after drying；
3) under the protection of nitrogen or noble gas, by step 2) the hard carbon precursor of gained solid-state is with 1-5
DEG C/programming rate of min is warming up to 400 DEG C, is incubated 1h, then with the intensification speed of 0.5-3 DEG C/min
Degree is warming up to 500-1200 DEG C, is incubated 3-20h, then naturally cools to room temperature, obtain hard carbon matrix；
4) hard carbon is carried out ball milling or pulverizing, obtain the hard carbon matrix that granularity is 1-60 μm；
5) adding carbon source, mix homogeneously in hard carbon matrix, rotating speed is 500-3500r/min, time
Between be 15-120min, then under the protection of nitrogen or noble gas, with the intensification of 2-5 DEG C/min
Speed is warming up to 400 DEG C, is incubated 1h, is then warming up to the programming rate of 0.5-3 DEG C/min
500-1200 DEG C, it is incubated 7-10h, is naturally cooling to room temperature, obtain the modified hard charcoal of lithium ion battery and bear
Pole material.
As a kind of preferred version, described step 1) in, to count in mass ratio, formalin or acetaldehyde are molten
Liquid: phenol: highly basic=1:2:0.05～0.2.
As a kind of preferred version, described step 2) in Ammonium persulfate. quality (g): water soluble phenolic resin
Fat volume (mL)=1:10-50.
As a kind of preferred version, described formalin concentration is 37%, and acetaldehyde solution concentration is 40%.
As a kind of preferred version, described highly basic is at least one in NaOH, KOH, and purity is
More than 99.9%.
As a kind of preferred version, described Ammonium persulfate. purity is more than 99.9%.
As a kind of preferred version, described vegetable oil is Oleum sesami, Oleum Brassicae campestris or at least the one of olive oil
Kind.
As a kind of preferred version, step 5) described in carbon source be asphalt, coal tar pitch, coal tar
In at least one.
The present invention compared with prior art has clear advantage and beneficial effect, particularly as follows: the present invention
Modified hard carbon cathode material there is the chemical property of excellence, there is excellent embedding lithium, de-lithium ability,
First discharge specific capacity is all in more than 400mAh/g, optimal embodiment, and discharge specific volume first
Amount up to 497mAh/g, first charge-discharge efficiency is up to 92%, it is adaptable to power and energy storage lithium from
Sub-battery；The preparation method of the present invention is simple and easy to do, and low cost can be applicable to industrialized production.
Detailed description of the invention
Embodiment 1
The preparation method of the modified hard carbon cathode material of a kind of lithium ion battery, comprises the following steps that
1) first, in formalin, phenol, highly basic are added, stirring reaction 5h at a temperature of 80 DEG C,
Obtain water soluble phenol resin；Count in mass ratio, formalin: phenol: highly basic=1:2:0.2；
This formalin concentration is 37%；This highly basic is NaOH, and purity is more than 99.9%.
2) Ammonium persulfate. is added above-mentioned steps 1) water soluble phenol resin prepared, Ammonium persulfate. matter
Amount (g): water soluble phenol resin volume (mL)=1:10, after being completely dissolved, adds equal-volume
Vegetable oil, mix homogeneously is fallen back in thermal response still, is placed in the microwave oven that power is 2000w,
Heating 10s, filters after react, by water and washing with alcohol 10 times, at a temperature of 40 DEG C after drying
Obtain the hard carbon precursor of solid-state；This Ammonium persulfate. purity is more than 99.9%；This vegetable oil is Oleum sesami.
3) under the protection of nitrogen or noble gas, by step 2) the hard carbon precursor of gained solid-state is with 5
DEG C/programming rate of min is warming up to 400 DEG C, is incubated 1h, then with the programming rate liter of 3 DEG C/min
Temperature, to 500 DEG C, is incubated 20h, then naturally cools to room temperature, obtain hard carbon matrix；
4) hard carbon is carried out ball milling or pulverizing, obtain the hard carbon matrix that granularity is 1-60 μm；
5) adding carbon source, mix homogeneously in hard carbon matrix, rotating speed is 3500r/min, and the time is
15min, then under the protection of nitrogen or noble gas, is warming up to the programming rate of 5 DEG C/min
400 DEG C, it is incubated 1h, is then warming up to 1200 DEG C with the programming rate of 3 DEG C/min, be incubated 7h,
It is naturally cooling to room temperature, obtains the modified hard carbon cathode material of lithium ion battery；The carbon source being somebody's turn to do is oil
Colophonium.
Embodiment 2
The preparation method of the modified hard carbon cathode material of a kind of lithium ion battery, comprises the following steps that
1) first, in acetaldehyde solution, phenol, highly basic are added, stirring reaction 12h at a temperature of 50 DEG C,
Obtain water soluble phenol resin；Count in mass ratio, formalin or acetaldehyde solution: phenol: highly basic=1:
2:0.05；This acetaldehyde solution concentration is 40%；This highly basic is KOH, and purity is more than 99.9%.
2) Ammonium persulfate. is added above-mentioned steps 1) water soluble phenol resin prepared, Ammonium persulfate. matter
Amount (g): water soluble phenol resin volume (mL)=1:50, after being completely dissolved, the body such as addition
Long-pending vegetable oil, mix homogeneously is fallen back in thermal response still, is placed in the microwave oven that power is 600w,
Heating 600s, filters after react, by water and washing with alcohol 3 times, at a temperature of 40 DEG C after drying
Obtain the hard carbon precursor of solid-state；This Ammonium persulfate. purity is more than 99.9%；This vegetable oil is Oleum Brassicae campestris.
3) under the protection of nitrogen or noble gas, by step 2) the hard carbon precursor of gained solid-state is with 1
DEG C/programming rate of min is warming up to 400 DEG C, is incubated 1h, then with the programming rate of 0.5 DEG C/min
It is warming up to 500 DEG C, is incubated 20h, then naturally cools to room temperature, obtain hard carbon matrix；
4) hard carbon is carried out ball milling or pulverizing, obtain the hard carbon matrix that granularity is 1-60 μm；
5) adding carbon source, mix homogeneously in hard carbon matrix, rotating speed is 500r/min, and the time is
120min, then under the protection of nitrogen or noble gas, is warming up to the programming rate of 2 DEG C/min
400 DEG C, it is incubated 1h, is then warming up to 500 DEG C with the programming rate of 0.5 DEG C/min, be incubated 10h,
It is naturally cooling to room temperature, obtains the modified hard carbon cathode material of lithium ion battery；The carbon source being somebody's turn to do is coal tar
Oil.
Embodiment 3
The preparation method of the modified hard carbon cathode material of a kind of lithium ion battery, comprises the following steps that
1) first, in formalin, phenol, highly basic are added, stirring reaction 8h at a temperature of 60 DEG C,
Obtain water soluble phenol resin；Count in mass ratio, formalin or acetaldehyde solution: phenol: highly basic=1:
2:0.1；This formalin concentration is 37%；This highly basic is NaOH, and purity is more than 99.9%.
2) Ammonium persulfate. is added above-mentioned steps 1) water soluble phenol resin prepared, Ammonium persulfate. matter
Amount (g): water soluble phenol resin volume (mL)=1:30, after being completely dissolved, adds equal-volume
Vegetable oil, mix homogeneously is fallen back in thermal response still, is placed in the microwave oven that power is 1200w,
Heating 400s, filters after react, by water and washing with alcohol 7 times, at a temperature of 40 DEG C after drying
Obtain the hard carbon precursor of solid-state；This Ammonium persulfate. purity is more than 99.9%；This vegetable oil is olive oil.
3) under the protection of nitrogen or noble gas, by step 2) the hard carbon precursor of gained solid-state is with 3
DEG C/programming rate of min is warming up to 400 DEG C, is incubated 1h, then with the programming rate liter of 2 DEG C/min
Temperature, to 900 DEG C, is incubated 10h, then naturally cools to room temperature, obtain hard carbon matrix；
4) hard carbon is carried out ball milling or pulverizing, obtain the hard carbon matrix that granularity is 1-60 μm；
5) adding carbon source, mix homogeneously in hard carbon matrix, rotating speed is 2500r/min, and the time is
100min, then under the protection of nitrogen or noble gas, is warming up to the programming rate of 3 DEG C/min
400 DEG C, it is incubated 1h, is then warming up to 700 DEG C with the programming rate of 2 DEG C/min, be incubated 9h,
It is naturally cooling to room temperature, obtains the modified hard carbon cathode material of lithium ion battery；The carbon source being somebody's turn to do is oil
Colophonium.
Embodiment 4
The preparation method of the modified hard carbon cathode material of a kind of lithium ion battery, comprises the following steps that
1) first, in formalin, phenol, highly basic are added, stirring reaction 7h at a temperature of 59 DEG C,
Obtain water soluble phenol resin；Count in mass ratio, formalin or acetaldehyde solution: phenol: highly basic=1:
2:0.15；This formalin concentration is 37%；This highly basic is NaOH, and purity is more than 99.9%.
2) Ammonium persulfate. is added above-mentioned steps 1) water soluble phenol resin prepared, Ammonium persulfate. matter
Amount (g): water soluble phenol resin volume (mL)=1:25, after being completely dissolved, adds equal-volume
Vegetable oil, mix homogeneously is fallen back in thermal response still, is placed in the microwave oven that power is 1000w,
Heating 190s, filters after react, by water and washing with alcohol 7 times, at a temperature of 40 DEG C after drying
Obtain the hard carbon precursor of solid-state；This Ammonium persulfate. purity is more than 99.9%；This vegetable oil is Oleum sesami.
3) under the protection of nitrogen or noble gas, by step 2) the hard carbon precursor of gained solid-state is with 4
DEG C/programming rate of min is warming up to 400 DEG C, is incubated 1h, then with the programming rate liter of 3 DEG C/min
Temperature, to 700 DEG C, is incubated 10h, then naturally cools to room temperature, obtain hard carbon matrix；
4) hard carbon is carried out ball milling or pulverizing, obtain the hard carbon matrix that granularity is 1-60 μm；
5) adding carbon source, mix homogeneously in hard carbon matrix, rotating speed is 1500r/min, and the time is
62min, then under the protection of nitrogen or noble gas, is warming up to the programming rate of 4 DEG C/min
400 DEG C, it is incubated 1h, is then warming up to 800 DEG C with the programming rate of 2 DEG C/min, be incubated 9h,
It is naturally cooling to room temperature, obtains the modified hard carbon cathode material of lithium ion battery；The carbon source being somebody's turn to do is oil
Colophonium.
Comparative example
Use the modified natural graphite material that Colophonium obtains as covering material.
Below foregoing individual embodiments and comparative example are carried out electrochemical property test:
For detecting the performance of the lithium ion battery negative material of negative material of the present invention, test with half-cell
Method is tested, with above example and the negative material of comparative example: SBR (solid content 50%):
CMC: Super-p=95.5: 2: 1.5: 1 (weight ratio), adds appropriate amount of deionized water and reconciles into pulpous state,
Coating on Copper Foil and be dried in vacuum drying oven and make negative plate in 12 hours, electrolyte is 1M
LiPF6/EC+DEC+DMC=1: 1: 1, microporous polypropylene membrane is barrier film, to electrode is
Lithium sheet, is assembled into battery.Constant current charge-discharge experiment, discharge and recharge is carried out at LAND battery test system
Voltage is limited in 0.01～3.0V, and the discharge and recharge cabinet computerizedd control carries out collection and the control of data
System, test temperature: 25 DEG C and 60 DEG C.The data obtained are as shown in table 1 below.
Table 1 lists different embodiment and the negative material Performance comparision of comparative example.
As it can be seen from table 1 the first charge-discharge efficiency of the modified hard carbon cathode material of the present invention is universal
Higher, the embedding lithium of modified hard carbon cathode material, de-lithium performance are good, and high rate during charging-discharging and
Cycle performance is the most excellent.
The above, be only presently preferred embodiments of the present invention, the not technical scope to the present invention
Impose any restrictions, therefore every technical spirit according to the present invention is to made for any of the above embodiments any trickle
Amendment, equivalent variations and modification, all still fall within the range of technical solution of the present invention.
Claims (8)
1. the lithium ion battery preparation method of modified hard carbon cathode material, it is characterised in that: bag
Include and have the following steps:
1) first, in formalin or acetaldehyde solution, phenol, highly basic are added, 50-80 DEG C of temperature
Degree lower stirring reaction 5-12h, obtains water soluble phenol resin；
2) Ammonium persulfate. is added above-mentioned steps 1) water soluble phenol resin prepared, wait to be completely dissolved
After complete, adding isopyknic vegetable oil, mix homogeneously is fallen back in thermal response still, is placed in power and is
In the microwave oven of 600～2000w, heat 10～600s, filter after having reacted, wash with water and ethanol
Wash 3-10 time, at a temperature of 40 DEG C, obtain the hard carbon precursor of solid-state after drying；
3) under the protection of nitrogen or noble gas, by step 2) the hard carbon precursor of gained solid-state is with 1-5
DEG C/programming rate of min is warming up to 400 DEG C, is incubated 1h, then with the intensification speed of 0.5-3 DEG C/min
Degree is warming up to 500-1200 DEG C, is incubated 3-20h, then naturally cools to room temperature, obtain hard carbon matrix；
4) hard carbon is carried out ball milling or pulverizing, obtain the hard carbon matrix that granularity is 1-60 μm；
5) adding carbon source, mix homogeneously in hard carbon matrix, rotating speed is 500-3500r/min, time
Between be 15-120min, then under the protection of nitrogen or noble gas, with the intensification of 2-5 DEG C/min
Speed is warming up to 400 DEG C, is incubated 1h, is then warming up to the programming rate of 0.5-3 DEG C/min
500-1200 DEG C, it is incubated 7-10h, is naturally cooling to room temperature, obtain the modified hard charcoal of lithium ion battery and bear
Pole material.
A kind of preparation side of the modified hard carbon cathode material of lithium ion battery
Method, it is characterised in that: described step 1) in, count in mass ratio, formalin or acetaldehyde solution: benzene
Phenol: highly basic=1:2:0.05～0.2.
A kind of preparation side of the modified hard carbon cathode material of lithium ion battery
Method, it is characterised in that: described step 2) in Ammonium persulfate. quality (g): water soluble phenol resin volume
(mL)=1:10-50.
A kind of preparation side of the modified hard carbon cathode material of lithium ion battery
Method, it is characterised in that: described formalin concentration is 37%, and acetaldehyde solution concentration is 40%.
A kind of preparation side of the modified hard carbon cathode material of lithium ion battery
Method, it is characterised in that: described highly basic is at least one in NaOH, KOH, and purity is 99.9%
Above.
A kind of preparation side of the modified hard carbon cathode material of lithium ion battery
Method, it is characterised in that: described Ammonium persulfate. purity is more than 99.9%.
A kind of preparation side of the modified hard carbon cathode material of lithium ion battery
Method, it is characterised in that: described vegetable oil is at least one of Oleum sesami, Oleum Brassicae campestris or olive oil.
A kind of preparation side of the modified hard carbon cathode material of lithium ion battery
Method, it is characterised in that: step 5) described in carbon source be in asphalt, coal tar pitch, coal tar extremely
Few one.
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| CN106450320A (en) * | 2016-12-12 | 2017-02-22 | 华中科技大学 | Novel method for preparing hard carbon and application of novel method |
| CN106450313A (en) * | 2016-11-15 | 2017-02-22 | 安徽安达新能源材料有限公司 | Porous hard-carbon lithium ion battery anode material, preparation method thereof and lithium ion battery |
| CN106744798A (en) * | 2016-12-12 | 2017-05-31 | 华中科技大学 | A kind of method and its application that hard carbon is prepared using carbon containing biological mass shell |
| CN109786694A (en) * | 2018-12-28 | 2019-05-21 | 徐州赛欧电子科技有限公司 | A kind of preparation method of lithium battery hard charcoal negative electrode material |
| CN109921020A (en) * | 2017-12-13 | 2019-06-21 | 宁波杉杉新材料科技有限公司 | A kind of preparation method of high-capacity lithium ion cell hard charcoal negative electrode material |
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| CN109786694A (en) * | 2018-12-28 | 2019-05-21 | 徐州赛欧电子科技有限公司 | A kind of preparation method of lithium battery hard charcoal negative electrode material |
| CN115279690A (en) * | 2020-04-10 | 2022-11-01 | 株式会社吴羽 | Method for producing carbonaceous material for negative electrode of nonaqueous electrolyte secondary battery, method for producing electrode of nonaqueous electrolyte secondary battery, and method for producing nonaqueous electrolyte secondary battery |
| CN114373924A (en) * | 2020-10-14 | 2022-04-19 | 天津工业大学 | Green phenolic resin-based hard carbon negative electrode material for lithium/sodium ion battery and preparation method thereof |
| CN115449041A (en) * | 2021-06-09 | 2022-12-09 | 济南精智方正新材料有限公司 | Preparation method of micro-spherical phenolic resin |
| CN113437295A (en) * | 2021-06-18 | 2021-09-24 | 青海凯金新能源材料有限公司 | Hard carbon negative electrode material and preparation method thereof |
| CN115849331A (en) * | 2021-09-24 | 2023-03-28 | 胡启章 | Hard carbon microbead, its preparation method and energy storage device containing same |
| CN114975869A (en) * | 2022-06-06 | 2022-08-30 | 榆林学院 | Button type sodium ion battery and preparation method thereof |
| CN114975869B (en) * | 2022-06-06 | 2024-03-08 | 榆林学院 | Button sodium ion battery and preparation method thereof |
| CN115036479A (en) * | 2022-06-13 | 2022-09-09 | 成都佰思格科技有限公司 | Composite negative electrode material, preparation method thereof and sodium ion battery |
| CN115036479B (en) * | 2022-06-13 | 2023-04-25 | 成都佰思格科技有限公司 | Composite negative electrode material, preparation method thereof and sodium ion battery |
| CN117466278A (en) * | 2023-11-01 | 2024-01-30 | 东北大学 | Method for ball milling modification of hard carbon material and application of ball milling modification of hard carbon material in negative electrode of sodium ion battery |
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