CN107611405A - A kind of preparation method of lithium battery carbon coated ferriferrous oxide nano core-shell type microballoon - Google Patents
A kind of preparation method of lithium battery carbon coated ferriferrous oxide nano core-shell type microballoon Download PDFInfo
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- CN107611405A CN107611405A CN201710843894.4A CN201710843894A CN107611405A CN 107611405 A CN107611405 A CN 107611405A CN 201710843894 A CN201710843894 A CN 201710843894A CN 107611405 A CN107611405 A CN 107611405A
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Abstract
A kind of preparation method the invention discloses lithium battery with carbon coated ferriferrous oxide nano core-shell type microballoon.Employ simple solvent-thermal method and prepare the homogeneous nano ferriferrous oxide microballoon of particle diameter distribution, and in this, as core source, simultaneously using resin as carbon source, core source and carbon source are subjected to carbon coating by way of grinding, by the process such as solidify, be carbonized, carbon coated ferriferrous oxide nano core-shell type microballoon is prepared.Using such a microballoon as electrode material, applied to lithium cell cathode material.This process is simple, and raw material is cheap, is easy to get, it is easy to accomplish industrialized production.
Description
Technical field
The invention belongs to electrochemical material technical field, particularly relates to a kind of oxidation of lithium battery carbon coating four three
The preparation method of iron nano core-shell type microballoon negative material.
Background technology
Lithium ion battery has the energy density and power density higher than ni-mh, NI-G, lead-acid battery, itself also has and follows
Ring long lifespan, self-discharge rate are low, do not have the advantages that memory effect.Therefore, lithium battery turns into the emphasis of mechanism of new electrochemical power sources research
One of.Research finds that the structure and pattern of lithium ion battery negative material play a key effect to chemical property, so, bear
The research of pole material is always the focus and difficult point of lithium ion battery.
Transition metal oxide is a species of ion cathode material lithium, has higher storage lithium ion and release lithium
The ability of ion, there is higher theoretical specific capacity.Using transition metal oxide as lithium cell cathode material, in discharge and recharge
Excellent chemical property is shown in journey, but Volume Changes are more violent, destroy electrode structure, and capacity is decayed rapidly.Cause
How this, overcome because the shortcomings that volumetric expansion is brought is the important topic of a research and development, wherein with carbon material to Fe3O4Cladding,
It not only can effectively alleviate Fe3O4Volume Changes in charge and discharge process, and Fe can be avoided3O4The reunion of particle.
Carbon coating is a kind of its electrical conductivity of the simplest, raising of relative efficiency, so as to improve the side of its chemical property
Method, but the selection of cladding carbon matrix precursor and its method for coating are the difficult points of the process.Before the currently used carbon for being used to coat
Driving body has glucose, sucrose, starch, phthalein amine etc., but the carbon graphite that these carbon matrix precursors are formed at temperature needed for material sintering
Change degree is low, and the material electric conductivity thus prepared is not high, have impact on the electric conductivity of electrode material.
Resin is the presoma for preparing excellent carbon material, and it can not only improve the degree of graphitization of carbon, and with also
Originality, the unfavorable oxidation of transition metal can be prevented.In addition, resin also has, carbonization rate is high, and clad is fine and close, and intensity is high, no
It is easily rupturable to wait clear superiority.The present invention chooses phenolic resin, epoxy resin and has condensation polycyclic polynuclear aromatic structure
Copna resins are as carbon coated precursor.
The content of the invention
Draw it is an object of the invention to solve Volume Changes in charge and discharge process existing for lithium ion battery negative material
The chemical property attenuation problem risen, proposes a kind of preparation of carbon coating precursor coated ferriferrous oxide nano core-shell type microballoon
Method, as lithium ion battery negative material.
The present invention is achieved by the following technical solutions, a kind of lithium battery carbon coated ferriferrous oxide nano core-shell type
The preparation method of microballoon, using following steps：
1.Fe3O4The preparation of nano particle
(1) ferric chloride (FeCl36H2O) is added in the ethylene glycol of certain volume, carries out ultrasonic disperse, obtain solution A；
(2) anhydrous sodium acetate and ferric chloride (FeCl36H2O) are added in solution A by certain mass ratio and carry out magnetic agitation,
Obtain solution B；
(3) solution B is poured into ptfe autoclave, carries out solvent thermal reaction under the high temperature conditions, obtain solution C；
(4) sediment gone solution C after supernatant carries out centrifuge washing, vacuum drying with distilled water, absolute ethyl alcohol, obtains
Black solid powder D, powder D are nanometer Fe3O4Particle；
2. the cladding of carbon
(1) by a certain amount of resin in a small amount of solvent ultrasonic dissolution, obtain solution E；
(2) by a certain amount of black powder D (nanometer Fes3O4) simultaneously ultrasonic disperse is added in solution E, obtain mixed solution F；
(3) mixed solution F is poured into agate mortar and is ground scattered until solvent volatilizees completely, obtain sticky solid G；
(4) sticky solid G is carried out to solidification at a certain temperature to dry and grind, obtains powder H；
(5) powder H is subjected to high temperature cabonization in a nitrogen atmosphere, then naturally cools to room temperature under atmosphere protection, obtain carbon
Coated ferriferrous oxide nano core-shell type microballoon.
The mass ratio of ferric chloride (FeCl36H2O) and sodium acetate is 1: 2-2: 1 in step 1, and ferric chloride (FeCl36H2O) quality is ethylene glycol
The 4%-8% of quality.Ultrasonic time is 10-30min, and the magnetic agitation time is 30-60min.Solvent thermal reaction temperature is 180-
220 DEG C, reaction time 12-24h.Vacuum drying temperature is 60 DEG C, time 12h.The oxygen of nanometer four prepared by solvent-thermal method
Change three-iron particle size uniformity, diameter range 200-300nm.
Raw material resin quality is Fe in step 23O4The 5%-30% of quality, resin used are phenolic resin, epoxy resin
Or any one in Copna resins.
Solidification temperature is 130 DEG C in step 2, time 12h.
Carburizing temperature is 500-700 DEG C in step 2, and heating rate is 1-3 DEG C/min, is incubated 60-120min.Shape after carbonization
Into with Fe3O4For core, agraphitic carbon is the carbon coated ferriferrous oxide nano core-shell type microballoon of shell, and its diameter range is 350nm-
500nm。
The present invention has advantages below：
1. carbon coated ferriferrous oxide nano core-shell type microballoon has, compound with regular structure, particle diameter distribution be homogeneous, shell thickness can
Control, the features such as pore-size distribution is narrow.
2. being used as carbon matrix precursor using resin, the degree of graphitization of carbon is improved, so that material conductivity is more effectively improved,
Resin has reproducibility simultaneously, can prevent the unfavorable oxidation of transition metal.
3. raw material is cheap, is easy to get, using the ground and mixed of resin and transition metal oxide, this process is simple, is easy to real
Existing industrialized production.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the typical nano ferriferrous oxide particle obtained in embodiment；
Fig. 2 is the carbon coated ferriferrous oxide nano core-shell type microballoon scanning electron microscope (SEM) photograph that embodiment 1 obtains；
Embodiment
The invention will be further described with reference to the accompanying drawings and examples.The scope of protection of present invention is not limited to
In the scope described in embodiment.
Embodiment 1：
Weigh ferric chloride (FeCl36H2O) (FeCl3·6H2O) 4.8g is added in 60mL ethylene glycol (EG), carried out as source of iron
Ultrasonic disperse 20min；Then, anhydrous sodium acetate 9.6g, wherein ferric chloride (FeCl36H2O) (FeCl are weighed3·6H2) and anhydrous acetic acid O
The ratio of sodium is 1: 2, is added to above-mentioned solution, magnetic agitation 30min；Above-mentioned solution is transferred to the anti-of polytetrafluoroethyllining lining
Answer in kettle, react 24h at 180 DEG C；Question response terminates, after naturally cooling to room temperature, by reaction product distilled water, anhydrous second
Alcohol carries out centrifuge washing successively；Nano ferriferrous oxide is obtained after 60 DEG C in vacuum dry 12h, its scanning electron microscope (SEM) photograph such as Fig. 1 institutes
Show.
Phenolic resin 0.025g is weighed as carbon source, a little absolute ethyl alcohol is added dropwise, carries out ultrasound or stirring and dissolving；Then,
0.5g nano ferriferrous oxides are added, wherein phenolic resin quality is Fe3O4The 5% of quality, continue ultrasonic disperse 20min；
Afterwards, pour the mixture into agate mortar, using absolute ethyl alcohol as solvent, add a little be ground until solvent is evaporated completely
Entirely.
Sticky solid after grinding is solidified into 12h at 130 DEG C；Cured product is placed in tubular type retort, in N2Protect
Under shield, 650 DEG C are warming up to 3 DEG C/min heating rate, carbonization 120min is carried out, finally in N2Room is naturally cooled under protection
Temperature, obtains carbon coated ferriferrous oxide nano core-shell type microballoon, and its scanning electron microscope (SEM) photograph is as shown in Figure 2.Electro-chemical test display is passed through
It is stable in 637mAh/g as lithium cell cathode material specific capacity after 100 circulations.
Embodiment 2：
Weigh ferric chloride (FeCl36H2O) (FeCl3·6H2O) 4.8g is added in 80mL ethylene glycol (EG), carried out as source of iron
Ultrasonic disperse 20min；Then, anhydrous sodium acetate 4.8g, wherein ferric chloride (FeCl36H2O) (FeCl are weighed3·6H2) and anhydrous acetic acid O
The ratio of sodium is 1: 1, is added to above-mentioned solution, magnetic agitation 30min；Above-mentioned solution is transferred to the anti-of polytetrafluoroethyllining lining
Answer in kettle, react 16h at 200 DEG C；Question response terminates, after naturally cooling to room temperature, by reaction solution distilled water, absolute ethyl alcohol
Centrifuge washing is carried out successively；Nano ferriferrous oxide is obtained after 60 DEG C in vacuum dry 12h.
Epoxy resin 0.05g is weighed as carbon source, a little toluene is added dropwise, carries out ultrasound or stirring and dissolving；Then, add
0.5g nano ferriferrous oxides, its epoxy resin quality is Fe3O4The 10% of quality, continue ultrasonic disperse 20min；It
Afterwards, pour the mixture into agate mortar, using toluene as solvent, add a little be ground until solvent volatilization is complete.
Sticky solid after grinding is solidified into 12h at 130 DEG C；Cured product is placed in tubular type retort, in N2Protect
Under shield, 500 DEG C are warming up to 1 DEG C/min heating rate, carbonization 100min is carried out, finally in N2Room is naturally cooled under protection
Temperature, carbon coated ferriferrous oxide nano core-shell type microballoon is obtained, electro-chemical test is shown after 100 circulations, as lithium battery
Negative material specific capacity is stable in 601mAh/g.
Embodiment 3：
Weigh ferric chloride (FeCl36H2O) (FeCl3·6H2O) 4.8g is added in 100mL ethylene glycol (EG), carried out as source of iron
Ultrasonic disperse 20min；Then, anhydrous sodium acetate 2.4g, wherein ferric chloride (FeCl36H2O) (FeCl are weighed3·6H2) and anhydrous acetic acid O
The ratio of sodium is 2: 1, is added to above-mentioned solution, magnetic agitation 30min；Above-mentioned solution is transferred to the anti-of polytetrafluoroethyllining lining
Answer in kettle, react 12h at 220 DEG C；Question response terminates, after naturally cooling to room temperature, by reaction solution distilled water, absolute ethyl alcohol
Centrifuge washing is carried out successively, and nano ferriferrous oxide is obtained after 60 DEG C in vacuum dry 12h.
Copna resins 0.1g is weighed as carbon source, a little tetrahydrofuran is added dropwise, carries out ultrasound or stirring and dissolving；Then, add
Enter 0.5g nano ferriferrous oxides, wherein Copna resin qualities are Fe3O4The 20% of quality, continue ultrasonic disperse 20min；
Afterwards, pour the mixture into agate mortar, using tetrahydrofuran as solvent, add a little be ground until solvent is evaporated completely
Entirely.
Sticky solid after grinding is solidified into 12h at 130 DEG C；Cured product is placed in tubular type retort, in N2Protect
Under shield, 600 DEG C are warming up to 2 DEG C/min heating rate, carbonization 80min is carried out, finally in N2Room is naturally cooled under protection
Temperature, carbon coated ferriferrous oxide nano core-shell type microballoon is obtained, electro-chemical test is shown after 100 circulations, as lithium battery
Negative material specific capacity is stable in 539mAh/g.
Embodiment 4：
Weigh ferric chloride (FeCl36H2O) (FeCl3·6H2O) 4.8g is added in 120mL ethylene glycol (EG), carried out as source of iron
Ultrasonic disperse 20min；Then, anhydrous sodium acetate 9.6g, wherein ferric chloride (FeCl36H2O) (FeCl are weighed3·6H2) and anhydrous acetic acid O
The ratio of sodium is 1: 2, is added to above-mentioned solution, magnetic agitation 30min；Above-mentioned solution is transferred to the anti-of polytetrafluoroethyllining lining
Answer in kettle, react 20h at 180 DEG C；Question response terminates, after naturally cooling to room temperature, by reaction solution distilled water, absolute ethyl alcohol
Centrifuge washing is carried out successively；Nano ferriferrous oxide is obtained after 60 DEG C in vacuum dry 12h.
Phenolic resin 0.15g is weighed as carbon source, a little absolute ethyl alcohol is added dropwise, carries out ultrasound or stirring and dissolving；Then, add
Enter 0.5g nano ferriferrous oxides, wherein phenolic resin quality is Fe3O4The 30% of quality, continue ultrasonic disperse 20min；
Afterwards, pour the mixture into agate mortar, using absolute ethyl alcohol as solvent, add a little be ground until solvent is evaporated completely
Entirely.
Sticky solid after grinding is solidified into 12h at 130 DEG C；Cured product is placed in tubular type retort, in N2Protect
Under shield, 700 DEG C are warming up to 3 DEG C/min heating rate, carbonization 60min is carried out, finally in N2Room is naturally cooled under protection
Temperature, carbon coated ferriferrous oxide nano core-shell type microballoon is obtained, electro-chemical test is shown after 100 circulations, as lithium battery
Negative material specific capacity is stable in 497mAh/g.
Claims (3)
1. a kind of lithium battery preparation method of carbon coated ferriferrous oxide nano core-shell type microballoon, it is characterised in that including as follows
Step：
First, Fe3O4The preparation of nano particle
(1) during ferric chloride (FeCl36H2O) is added to, wherein ferric chloride (FeCl36H2O) quality is the 4%-8% of quality of glycol, is carried out
Ultrasonic disperse 10-30min, obtains solution A；
(2) ratio of anhydrous sodium acetate and ferric chloride (FeCl36H2O) in mass ratio 1: 2-2: 1 is added in solution A, magnetic agitation
30-60min, obtain solution B；
(3) solution B is poured into ptfe autoclave, 12-24h solvent thermal reaction is carried out under 180-220 DEG C of high temperature,
Obtain solution C；
(4) sediment gone solution C after supernatant carries out centrifuge washing with distilled water, absolute ethyl alcohol, is dried in vacuo at 60 DEG C
12h, it is nanometer Fe to obtain black solid powder D, powder D3O4Particle；
2nd, the cladding of carbon
(1) by a certain amount of resin in a small amount of solvent ultrasonic dissolution, obtain solution E；
(2) by a certain amount of black powder D (nanometer Fes3O4) simultaneously ultrasonic disperse 10-30min is added in solution E, obtain mixed solution
F；
(3) mixed solution F is poured into agate mortar and is ground scattered until solvent volatilizees completely, obtain sticky solid G；
(4) sticky solid G is solidified at 130 DEG C and dries 12h and grind, obtain powder H；
(5) powder H being subjected to high temperature cabonization in a nitrogen atmosphere, carburizing temperature is 500-700 DEG C, 1-3 DEG C of heating rate/min,
60-120min is incubated, room temperature is naturally cooled under last atmosphere protection, obtains carbon coated ferriferrous oxide nano core-shell type microballoon.
2. according to the method for claim 1, it is characterised in that：Material resin quality is Fe3O4The 5%-30% of quality, institute
Resin can be any one in phenolic resin, epoxy resin or Copna resins.
3. according to the method for claim 1, it is characterised in that：Ferroso-ferric oxide diameter range is 200-300nm, carbon coating
Ferriferrous oxide nano core-shell microspheres diameter range is 350nm-500nm.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108258196A (en) * | 2018-01-27 | 2018-07-06 | 景德镇陶瓷大学 | A kind of preparation method and applications of micro-nano structure iron oxide/carbon composite |
| CN109485101A (en) * | 2018-12-05 | 2019-03-19 | 北京工业大学 | A method of nano-scale carbon coated magnetic ferroso-ferric oxide is prepared as raw material to backwash iron cement |
| CN110649237A (en) * | 2019-09-27 | 2020-01-03 | 厦门理工学院 | Iron oxide @ carbon nanocomposite and preparation method and application thereof |
| CN110756132A (en) * | 2019-10-31 | 2020-02-07 | 大连理工大学 | Preparation method of core-shell magnetic microspheres |
| CN113184915A (en) * | 2021-04-23 | 2021-07-30 | 扬州工业职业技术学院 | Double-shell coated ferroferric oxide nano-particles, preparation method and application thereof |
| CN113351209A (en) * | 2021-06-07 | 2021-09-07 | 浙江工业大学 | Carbon-coated ferroferric oxide composite material and preparation method and application thereof |
| CN114275824A (en) * | 2022-01-18 | 2022-04-05 | 杭州幄肯新材料科技有限公司 | Porous carbon-coated ferroferric oxide nano-particles and solid-phase preparation method thereof |
-
2017
- 2017-09-13 CN CN201710843894.4A patent/CN107611405A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 刘文文: ""Fe3O4@C 复合微球的制备及其在电磁波吸收和电化学领域中的应用"", 《万方数据库》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108258196A (en) * | 2018-01-27 | 2018-07-06 | 景德镇陶瓷大学 | A kind of preparation method and applications of micro-nano structure iron oxide/carbon composite |
| CN108258196B (en) * | 2018-01-27 | 2020-04-21 | 景德镇陶瓷大学 | Preparation method and application of micro-nano structure iron oxide/carbon composite material |
| CN109485101A (en) * | 2018-12-05 | 2019-03-19 | 北京工业大学 | A method of nano-scale carbon coated magnetic ferroso-ferric oxide is prepared as raw material to backwash iron cement |
| CN109485101B (en) * | 2018-12-05 | 2021-03-16 | 北京工业大学 | Method for preparing nanoscale carbon-coated magnetic ferroferric oxide by taking backwashing iron mud as raw material |
| CN110649237A (en) * | 2019-09-27 | 2020-01-03 | 厦门理工学院 | Iron oxide @ carbon nanocomposite and preparation method and application thereof |
| CN110649237B (en) * | 2019-09-27 | 2021-05-14 | 厦门理工学院 | Iron oxide @ carbon nanocomposite and preparation method and application thereof |
| CN110756132A (en) * | 2019-10-31 | 2020-02-07 | 大连理工大学 | Preparation method of core-shell magnetic microspheres |
| CN113184915A (en) * | 2021-04-23 | 2021-07-30 | 扬州工业职业技术学院 | Double-shell coated ferroferric oxide nano-particles, preparation method and application thereof |
| CN113351209A (en) * | 2021-06-07 | 2021-09-07 | 浙江工业大学 | Carbon-coated ferroferric oxide composite material and preparation method and application thereof |
| CN114275824A (en) * | 2022-01-18 | 2022-04-05 | 杭州幄肯新材料科技有限公司 | Porous carbon-coated ferroferric oxide nano-particles and solid-phase preparation method thereof |
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Application publication date: 20180119 |