CN109119625A - A kind of preparation method of ferroso-ferric oxide-carbon nanotube lithium cell cathode material - Google Patents
A kind of preparation method of ferroso-ferric oxide-carbon nanotube lithium cell cathode material Download PDFInfo
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- CN109119625A CN109119625A CN201811137012.3A CN201811137012A CN109119625A CN 109119625 A CN109119625 A CN 109119625A CN 201811137012 A CN201811137012 A CN 201811137012A CN 109119625 A CN109119625 A CN 109119625A
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Abstract
The invention discloses a kind of ferroso-ferric oxide-carbon nanotube lithium cell cathode material preparation methods, the following steps are included: step 1: the carbon nanotube of purchase being dispersed in concentrated nitric acid (mass fraction 65%-68%), be cleaned and dried after high-temperature acid is handled spare；Step 2: the processed carbon nanotube of acid is distributed in deionized water；Step 3: ferric chloride (FeCl36H2O), urea, polyvinylpyrrolidone are added in mixed liquor obtained by step 2, and the potassium sodium tartrate as reducing agent is then added, dissolution is sufficiently stirred；Step 4: and then pour into step 3 resulting mixed liquor in the stainless steel cauldron of polytetrafluoroethyllining lining, after heated sealed, washing is dried to obtain nanocomposite.Metal oxide nano-material is connected to the surface of bigger serface carbon material, carbon material structural stability can bearing object product variation bring stress, the shortcomings that overcoming the poorly conductive of nano-metal-oxide active material makes composite material obtain excellent lithium electrical property.
Description
Technical field
The present invention relates to cell nano Material Field, specifically a kind of magnetic nano ferroferric oxide-carbon nanotube lithium
The preparation method of cell negative electrode material.
Background technique
With being constantly progressive for today's society, electronic information technology, aerospace, sophisticated weapon equipment and mixing are dynamic
Power automobile, electric automobile technology are grown rapidly, the demand to the secondary cell of mechanism of new electrochemical power sources, especially high-energy density
It is very urgent.Development capacity is high, and charge-discharge electric power is big, has extended cycle life, environmental-friendly and inexpensive electrochmical power source just at
The project that whole world scientific worker studies jointly.Therefore select efficient green energy resource realize sustainable development be we must
So selection.Lithium ion battery is had outstanding performance in power supply, and open-circuit voltage is relatively high, energy density is big, good cycle, when use
Between long, small pollution of the environment, have bigger temperature use scope etc., in new energy become hot spot.Lithium ion battery
Advantageous in processing technology, it can do various forms, various sizes, be highly convenient for using meeting a variety of demands, and be energy
The rechargeable battery being enough recycled, very environmentally friendly in use, safety coefficient is high.In the numerous cathode of lithium ion battery
Among material, since carbon material has the spies such as manufacturing cost is cheap, electrode potential is low, cycle performance is excellent and safety coefficient is high
Point, is most widely used at present, mainly there is graphite-like, amorphous-type etc..
Wherein, carbon nanotube is hollow tubular structure, large specific surface area, draw ratio are big, light weight, tensile strength are high,
Have the advantages that Quantum Teleportation characteristic and the attention by researcher, the successful development of nearest large-size carbon nanotube, more
It is the enthusiasm for promoting people and the unique physicochemical properties of carbon nanotube being explored.Carbon nanotube also attracts as negative electrode material
Extensive concern.Carbon nanotube can be used as inert additwe, and due to its excellent electric conductivity, specific surface area is high, ultra-thin
The flexible and stability of tube wall and structure, carbon nanotube are very prominent as effect of the additive in building nanocomposite
Out.Its big specific surface area may insure effective contact area between electrolyte and electrode, ultra-thin tube wall and hollow structure
Shorten the distance of lithium ion diffusion.In addition, carbon nanotube, which winds mutually contact, forms unique conductive network, mentioned for electron transmission
For excellent continuous conductive path.Carbon nanotube acts not only as conductive material, can also make during fast charging and discharging
The pressure of adaptation volume change generation is buffered for outstanding inert component.
Metal oxide nano-material is the new direction of negative electrode material, and nano material has many new blocks that are different from
Advantage, the material of nano-scale have more stable structure and more superior storage lithium ability, nano-scale in charge and discharge process
Electrode material, large specific surface area, size is small, shortens the distance of the diffusion of lithium ion in the material, is conducive to high-power fill
The progress of exoelectrical reaction can preferably keep the integrality of structure in charge and discharge process.Due to its size characteristic metal oxygen
Tension existing for the surface of compound nano material is very big, can weaken lithium ion insertion to a certain extent and deviate to material
Caused by volume telescopic variation back and forth, be maintained at the complete of electrode during repeated charge, keep the performance of battery more excellent,
Increase application range.Metal oxide nano-material is capable of providing more due to unique size characteristic in active material surface
Effective contact point, surface texture featur provides more multipath again for the diffusion of lithium ion, can effectively weaken anti-
The electrode polarization that electrode is easy to appear in multiple charge and discharge process, keeps its lithium electrical property more excellent.
Ferroso-ferric oxide is the oxide for the iron that the very big one kind of reserves is common in nature, mostly in the form of magnetic iron ore
It is present in ore, fusing point is 1597 DEG C, density 5.17g/cm3, the sub- magnet under room temperature is very strong, and conductivity is relatively high,
It is usually used in manufacturing audio tape and telecommunication apparatus in the past.As negative electrode material, ferroso-ferric oxide has specific capacity height, natural reserves
The advantages that abundant and environmental sound, but be also easy to that active material reunion and breaking and Dusting etc. occurs in charge and discharge process
Phenomenon makes the irreversible capacity height of battery, is difficult to ensure long circulating stationary performance.
Metal oxide nano-material is connected to the surface of bigger serface carbon material, carbon material structural stability can
The shortcomings that bearing volume change bring stress, overcoming the poorly conductive of nano-metal-oxide active material, makes composite material
Obtain excellent lithium electrical property.
In simple ferroso-ferric oxide electrode, the insertion and abjection of lithium ion can cause four oxygen during repeated charge
The expansion and contraction for changing three-iron nano particle volume, lead to poor contact between ferroferric oxide nano granules, electrode conductivuty
It is deteriorated, hinders discharge and recharge reaction, and carbon nanotubes, which is added, can play the role of connecting them, construct three-dimensional conductive network knot
Structure, effectively contact can be had by making to adhere between metallic particles on the carbon nanotubes, to improve cycle performance；Carbon is received
The huge surface area of mitron can also uniformly disperse ferroferric oxide nano granules to be fixed on surface, prevent charge and discharge
The reunion of particle in journey, enhances the stability of negative electrode material structure, material is made to be able to maintain stable performance.
The negative electrode material of function admirable in order to obtain needs a kind of method by ferroferric oxide nano granules and carbon nanotube
(MWNTs) it is combined with each other to obtain ferroferric oxide nano granules and carbon nano tube compound material (Fe3O4/MWNTs).
Summary of the invention
The present invention is exactly to provide a kind of ferroso-ferric oxide-carbon nanotube to solve deficiencies of the prior art
Metal oxide nano-material is connected to the surface of bigger serface carbon material, carbon by the preparation method of lithium cell cathode material
Material structure stability can bearing object product variation bring stress, overcome the poorly conductive of nano-metal-oxide active material
The shortcomings that, so that composite material is obtained excellent lithium electrical property.
The technical scheme adopted by the invention to solve the technical problem is that:
A kind of preparation method of ferroso-ferric oxide-carbon nanotube lithium cell cathode material, comprising the following steps:
Step 1: the carbon nanotube of purchase is dispersed in concentrated nitric acid (mass fraction 65%-68%), is carried out at high-temperature acid
It is cleaned and dried after reason spare；
Step 2: the processed carbon nanotube of acid is distributed in deionized water,；
Step 3: ferric chloride (FeCl36H2O), urea, polyvinylpyrrolidone are added in mixed liquor obtained by step 2, then
The potassium sodium tartrate as reducing agent is added, dissolution is sufficiently stirred, wherein ferric chloride (FeCl36H2O): urea: the matter of potassium sodium tartrate
Amount is than being 3.8~4.5:8~11:5~7；Raw material of the ferric chloride (FeCl36H2O) as magnetic ferroferric oxide, input amount decide
The thickness of the magnetic ferroferric oxide particle of attachment on the carbon nanotubes, urea provide alkaline ring for the conversion of ferric ion
Border, potassium sodium tartrate also want strict control as reducing agent, with the ratio of ferric ion, ensure that the ferric iron that is reduced from
The amount of son.
Step 4: and then pour into step 3 resulting mixed liquor in the stainless steel cauldron of polytetrafluoroethyllining lining, it is close
Envelope is heated to 180-210 DEG C, keeps the temperature 10-15h, and the nanocomposite can be obtained in washing drying.
The step 1 high temperature acid handles concrete operations are as follows: will be dispersed with the concentrated nitric acid of carbon nanotube in 140 DEG C of temperature
Lower heat preservation 6 hours.
Carbon nanotube in step 2 and step 3: ferric chloride (FeCl36H2O): the mass ratio of polyvinylpyrrolidone is 1~1.2:
3.8~4.5:18~25, in step 1, the cleaning is that be washed with deionized water and ethyl alcohol alternate repetition to filtrate be neutral
(PH=6.8~7.2)；Polyvinylpyrrolidone does not need to be strict with as its content of surfactant.
In the step 4, mixed liquor is heated to seal to 200 DEG C in the stainless steel cauldron of polytetrafluoroethyllining lining,
Heat preservation 12 hours.After it is cooled to room temperature, it is no less than 5 times, will be obtained with deionized water and ethyl alcohol alternate repetition centrifuge washing
Magnetic 55-70 DEG C in a vacuum drying oven of black product, it is 24-36 hours dry.
The beneficial effects of the present invention are:
1, metal oxide nano-material is connected to the surface of bigger serface carbon material, and carbon material structural stability can
The shortcomings that bearing volume change bring stress, overcoming the poorly conductive of nano-metal-oxide active material, makes composite material
Obtain excellent lithium electrical property.
2, in simple ferroso-ferric oxide electrode, the insertion and abjection of lithium ion can cause four during repeated charge
The expansion and contraction of Fe 3 O nano particle volume, lead to poor contact between ferroferric oxide nano granules, electrodes conduct
Property be deteriorated, hinder discharge and recharge reaction, and be added carbon nanotubes can play the role of connect they, construct three-dimensional conductive network knot
Structure, effectively contact can be had by making to adhere between metallic particles on the carbon nanotubes, to improve cycle performance；Carbon is received
The huge surface area of mitron can also uniformly disperse ferroferric oxide nano granules to be fixed on surface, prevent charge and discharge
The reunion of particle in journey, enhances the stability of negative electrode material structure, material is made to be able to maintain stable performance.
It 3, is that carbon nano tube surface is made to adhere to hydroxyl, carboxyl isoreactivity group the purpose of step 1, so that surface is easy to carry out
Chemical reaction, provides growing point for ferriferrous oxide particles.
4, raw material of the ferric chloride (FeCl36H2O) as magnetic ferroferric oxide, input amount decide attachment on the carbon nanotubes
Magnetic ferroferric oxide particle thickness, urea provides alkaline environment, potassium sodium tartrate conduct for the conversion of ferric ion
Reducing agent also wants strict control with the ratio of ferric ion, ensure that the amount for the ferric ion being reduced.
Detailed description of the invention
Fig. 1 is the field emission scanning electron microscope figure of product obtained by the present invention；
Fig. 2 is the transmission electron microscope figure of product obtained by the present invention.
Specific embodiment
For a better understanding of the present invention, a specific embodiment of the invention is explained in detail with reference to the accompanying drawing.
A kind of preparation method of ferroso-ferric oxide-carbon nanotube lithium cell cathode material, comprising the following steps:
Step 1: the carbon nanotube of purchase is dispersed in concentrated nitric acid (mass fraction 65%-68%), is carried out at high-temperature acid
It is cleaned and dried after reason spare；
Step 2: the processed carbon nanotube of acid is distributed in deionized water,；
Step 3: ferric chloride (FeCl36H2O), urea, polyvinylpyrrolidone are added in mixed liquor obtained by step 2, then
The potassium sodium tartrate as reducing agent is added, dissolution is sufficiently stirred, wherein ferric chloride (FeCl36H2O): urea: the matter of potassium sodium tartrate
Amount is than being 3.8~4.5:8~11:5~7；Raw material of the ferric chloride (FeCl36H2O) as magnetic ferroferric oxide, input amount decide
The thickness of the magnetic ferroferric oxide particle of attachment on the carbon nanotubes, urea provide alkaline ring for the conversion of ferric ion
Border, potassium sodium tartrate also want strict control as reducing agent, with the ratio of ferric ion, ensure that the ferric iron that is reduced from
The amount of son.
Step 4: and then pour into step 3 resulting mixed liquor in the stainless steel cauldron of polytetrafluoroethyllining lining, it is close
Envelope is heated to 180-210 DEG C, keeps the temperature 10-15h, and the nanocomposite can be obtained in washing drying.
The step 1 high temperature acid handles concrete operations are as follows: will be dispersed with the concentrated nitric acid of carbon nanotube in 140 DEG C of temperature
Lower heat preservation 6 hours.
Carbon nanotube in step 2 and step 3: ferric chloride (FeCl36H2O): the mass ratio of polyvinylpyrrolidone is 1~1.2:
3.8~4.5:18~25, in step 1, the cleaning is that be washed with deionized water and ethyl alcohol alternate repetition to filtrate be neutral
(PH=6.8~7.2)；Polyvinylpyrrolidone does not need to be strict with as its content of surfactant.
In the step 4, mixed liquor is heated to seal to 200 DEG C in the stainless steel cauldron of polytetrafluoroethyllining lining,
Heat preservation 12 hours.After it is cooled to room temperature, it is no less than 5 times, will be obtained with deionized water and ethyl alcohol alternate repetition centrifuge washing
Magnetic 55-70 DEG C in a vacuum drying oven of black product, it is 24-36 hours dry.
Specific experiment step
The acid processing carbon nanotube that 0.1-0.12g acid is handled is weighed, is dispersed in 38-45ml deionized water,
The dissolution of 0.38-0.45g ferric chloride (FeCl36H2O) is added, 0.8-1.1g urea is added, 1.8-2.5g polyvinylpyrrolidone is added, and
It persistently stirs under magnetic stirring 1-1.5 hours, then 0.5-0.7g potassium sodium tartrate is added and is dissolved.Then mixed liquor is fallen
Enter in the stainless steel cauldron of polytetrafluoroethyllining lining, be heated to seal to 180-200 DEG C, keeps the temperature 10-15h.Room is cooled to it
Wen Hou is centrifuged repeatedly with deionized water and ethyl alcohol and is washed each 4-6 times, in a vacuum drying oven by obtained magnetic black product
55-70 DEG C dry 24-36 hours to get arrive target product.
Concrete operations are as follows: the carbon nanotube of purchase is dispersed in concentrated nitric acid (mass fraction 65%-68%) first, is put into
In the stainless steel cauldron of polytetrafluoroethyllining lining, it is heated to 140 DEG C and keeps the temperature 6 hours, then carbon nanotube is centrifuged
And cleaning, being washed repeatedly with deionized water and ethyl alcohol to filtrate is neutral (PH=7), is dried in a vacuum 24 hours to get arriving
Acid processing carbon nanotube.Purpose is that carbon nano tube surface is made to adhere to hydroxyl, carboxyl isoreactivity group, so that being easy of surface
Reaction is learned, provides growing point for ferriferrous oxide particles.
Embodiment one:
The acid processing carbon nanotube that 0.11g acid is handled is weighed, is dispersed in 40ml deionized water, 0.4g is added
Ferric chloride (FeCl36H2O) dissolution, is added 0.9g urea and 2g polyvinylpyrrolidone, and persistently stirring 1.3 is small under magnetic stirring
When, then 0.6g potassium sodium tartrate is added and is dissolved.Then mixed liquor is poured into the stainless steel cauldron of polytetrafluoroethyllining lining
In, 190 DEG C are heated to seal to, 12h is kept the temperature.After it is cooled to room temperature, with deionized water and ethyl alcohol be centrifuged repeatedly washing 5 times with
On, by obtained magnetic black product in a vacuum drying oven 60 DEG C of drying 30 hours to get arriving target product.
Embodiment two:
The acid processing carbon nanotube that 0.1g acid is handled is weighed, is dispersed in 40ml deionized water, 0.38g is added
Ferric chloride (FeCl36H2O) dissolution, is added 0.8g urea, 1.8g polyvinylpyrrolidone is added, and persistently stir 1 under magnetic stirring
Hour, then 0.5g potassium sodium tartrate is added and is dissolved.Then mixed liquor is poured into the stainless steel reaction of polytetrafluoroethyllining lining
In kettle, 180 DEG C are heated to seal to, keeps the temperature 10 hours.After it is cooled to room temperature, washing is centrifuged repeatedly with deionized water and ethyl alcohol
Each 5 times, by obtained magnetic black product in a vacuum drying oven 55 DEG C of drying 24 hours to get arriving target product.
Embodiment three:
The acid processing carbon nanotube that 0.12g acid is handled is weighed, is dispersed in 45ml deionized water, is added
The dissolution of 0.45g ferric chloride (FeCl36H2O), is added 1.1g urea, and 2.5g polyvinylpyrrolidone is added, and continues under magnetic stirring
0.7g potassium sodium tartrate is then added and dissolves by stirring 1.5 hours.Then mixed liquor is poured into the stainless of polytetrafluoroethyllining lining
In steel reaction kettle, 200 DEG C are heated to seal to, keeps the temperature 15 hours.After it is cooled to room temperature, with deionized water and ethyl alcohol repeatedly from
Heart washing each 5 times, obtained magnetic black product is produced for 70 DEG C for drying 36 hours to get to target in a vacuum drying oven
Object.
The main distinction of above-mentioned product is the particle thickness degree of the magnetic ferroferric oxide adhered in carbon nanotube not
Together, but respective objects product can be obtained.
Ferroferric oxide nano granules are uniformly adhered to the surface of carbon nanotube in the composite material, the nano combined material
Material has shown excellent long circulating performance as ion cathode material lithium, is 100mA g in current density-1Under conditions of,
Fe3O4The cyclic discharge capacity for the first time of/MWNTs is 782mAh g-1, charging capacity is 450mAh g-1, discharge after 70 circulations
Capacity stills remain in 661mAh g-1, charging capacity is 634mAh g-1.Illustrate the Fe obtained with this3O4/ MWNTs composite material
Constant current long circulating performance it is very excellent.In addition, product of the present invention can also be applied since nano ferriferrous oxide has magnetism
In electro-magnetic wave absorption field.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (4)
1. a kind of ferroso-ferric oxide-carbon nanotube lithium cell cathode material preparation method, characterized in that the method includes with
Lower step:
Step 1: by carbon nanotube be dispersed in mass fraction be 65%-68% concentrated nitric acid in, carry out high-temperature acid processing after
It is cleaned and dried spare；
Step 2: the processed carbon nanotube of acid is distributed in deionized water；
Step 3: ferric chloride (FeCl36H2O), urea, polyvinylpyrrolidone are added in mixed liquor obtained by step 2, are then added
As the potassium sodium tartrate of reducing agent, dissolution is sufficiently stirred, wherein ferric chloride (FeCl36H2O): urea: the mass ratio of potassium sodium tartrate
For 3.8~4.5:8~11:5~7；
Step 4: and then pour into step 3 resulting mixed liquor in the stainless steel cauldron of polytetrafluoroethyllining lining, sealing adds
Heat arrives 180-210 DEG C, keeps the temperature 10-15h, and washing is dried to obtain the nanocomposite.
2. a kind of preparation method of ferroso-ferric oxide-carbon nanotube lithium cell cathode material according to claim 1, special
Sign is that the step 1 high temperature acid handles concrete operations are as follows: protects the concentrated nitric acid for being dispersed with carbon nanotube at a temperature of 140 DEG C
Temperature 6 hours.
3. a kind of preparation method of ferroso-ferric oxide-carbon nanotube lithium cell cathode material according to claim 1, special
Sign is carbon nanotube in step 2 and step 3: ferric chloride (FeCl36H2O): the mass ratio of polyvinylpyrrolidone is 1~1.2:3.8
~4.5:18~25, in step 1, the cleaning is that be washed with deionized water and ethyl alcohol alternate repetition to filtrate pH value be 6.8
~7.2.
4. a kind of preparation method of ferroso-ferric oxide-carbon nanotube lithium cell cathode material according to claim 1, special
Sign is, in the step 4, mixed liquor is heated to seal to 200 DEG C in the stainless steel cauldron of polytetrafluoroethyllining lining, is protected
It is no less than 5 times with deionized water and ethyl alcohol alternate repetition centrifuge washing, the magnetic that will be obtained after it is cooled to room temperature within temperature 12 hours
Property 55-70 DEG C in a vacuum drying oven of black product, dry 24-36 hours.
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| CN111599604A (en) * | 2020-06-03 | 2020-08-28 | 邓新峰 | C-MnFe with shell-core structure2O4-CNT (carbon nanotube) supercapacitor electrode material and preparation method thereof |
| CN111599604B (en) * | 2020-06-03 | 2021-12-24 | 国网黑龙江省电力有限公司电力科学研究院 | C-MnFe with shell-core structure2O4-CNT (carbon nanotube) supercapacitor electrode material and preparation method thereof |
| CN112537797A (en) * | 2020-12-07 | 2021-03-23 | 安徽师范大学 | Ferroferric oxide/carbon nano tube/sulfur-loaded composite material with one-dimensional chain-like core-shell structure, preparation method and application |
| CN112537797B (en) * | 2020-12-07 | 2023-04-18 | 安徽师范大学 | Ferroferric oxide/carbon nano tube/sulfur-loaded composite material with one-dimensional chain-like core-shell structure, preparation method and application |
| CN112736235A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Biomass/carbon nanotube induced Fe3O4Nano composite material and application thereof as negative electrode material of lithium ion battery |
| CN112736235B (en) * | 2021-01-15 | 2024-02-20 | 辽宁大学 | Biomass/carbon nanotube induced Fe 3 O 4 Nanocomposite and application thereof as lithium ion battery anode material |
| CN113945477A (en) * | 2021-10-18 | 2022-01-18 | 安徽安瓦新能源科技有限公司 | Method for detecting carbon content in battery electrode material |
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Application publication date: 20190101 |