CN110416545A - A method of Porous hollow carbon nano rod lithium ion battery negative material is prepared by template of Carapax Eriocheir sinensis - Google Patents
A method of Porous hollow carbon nano rod lithium ion battery negative material is prepared by template of Carapax Eriocheir sinensis Download PDFInfo
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- CN110416545A CN110416545A CN201910726705.4A CN201910726705A CN110416545A CN 110416545 A CN110416545 A CN 110416545A CN 201910726705 A CN201910726705 A CN 201910726705A CN 110416545 A CN110416545 A CN 110416545A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
A method of Porous hollow carbon nano rod lithium ion battery negative material being prepared by template of Carapax Eriocheir sinensis, it is related to a kind of preparation method of lithium ion battery negative material.The invention aims to solve existing template to prepare Porous hollow carbon nanomaterial there are templates to remove difficult, and the higher problem of material production cost.Method: one, Carapax Eriocheir sinensis template is prepared；Two, mixed carbon source；Three, it is carbonized；Four, diluted acid impregnates, and obtains Porous hollow carbon nano rod lithium ion battery negative material.Advantage: one, can slough template using dilute acid soln using Carapax Eriocheir sinensis as template, it is difficult to solve the problems, such as that existing template removes, and realize waste utilization, reduce cost.Two, the battery prepared has excellent long circulating stability energy and high rate performance, and capacity retention ratio can maintain 98% or more.Present invention is mainly used for prepare Porous hollow carbon nano rod lithium ion battery negative material by template of Carapax Eriocheir sinensis.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium ion battery negative material.
Background technique
With human society and economic further development, the limited resources such as traditional coal, petroleum, natural gas are by constantly
It excavates, exploit and utilizes, and face exhaustion.Meanwhile a large amount of burnings of fossil energy use, and lead to the rings such as haze, greenhouse effects
Border problem is increasingly serious.Therefore, the new energy for finding substitute fossil fuels is extremely urgent.Lithium ion battery is close due to having energy
Spend height, long service life, stable operating voltage, it is environmentally protective the advantages that, commercialized 30 years in the past, have become the energy and open
The important energy storage device of hair.
The design and preparation of negative electrode material are the key that obtain high performance lithium ion battery.Carbon-based material, due to material
Expect the features such as resource is extensive, stable structure, chemical stability are good, is widely used as the negative electrode material of lithium ion battery.Stone at present
Ink is most common carbon based negative electrodes material in lithium ion battery, but the theoretical capacity of graphite carbon material is only 372mAh/g, no
It is able to satisfy lithium ion battery high-energy and powerful demand.Therefore exploitation specific capacity is higher, cycle life is longer, price is lower
Honest and clean novel anode material, it has also become the focus of Study on Li-ion batteries.Porous hollow carbon nanomaterial is with higher to compare table
Area can make electrolyte sufficiently infiltrate electrode material, and its hollow structure, can be shortened transmission road of the lithium ion in bulk material
Diameter, while can also buffer the volume expansion of material during repeated charge, thus can be used as the lithium of high magnification long circulation life from
Sub- cell negative electrode material.The method for being typically prepared Porous hollow carbon material has chemical activation method, high temperature pyrolytic cracking (HTP) and template etc..
Chemical activation method is a kind of method that porous material is prepared by plus activating dose (such as KOH, alkalinity CaO), such method pair
Environmental pollution is larger；High temperature pyrolytic cracking (HTP) is usually that carbon source material is pyrolyzed to carbonization at high temperature, although such method process is simple,
But higher pyrolysis temperature needs high-power operation, causes energy loss excessive；Template is usually to use porous silica
Monomer and silicon dioxide colloid etc. are the method that template prepares porous carbon materials, and this class template removes difficult and higher cost.
Therefore, it in order to reduce cost, reduces environmental pollution and energy consumption is established a kind of inexpensive, high using waste biomass material
The preparation method of the Porous hollow carbon nanomaterial of performance is of great significance to the energy development strategy for realizing sustainability.
Summary of the invention
The invention aims to solve existing template prepare Porous hollow carbon nanomaterial there are template remove it is difficult,
And the higher problem of material preparation cost, and one kind is provided and prepares Porous hollow carbon nano rod lithium-ion electric by template of Carapax Eriocheir sinensis
The method of pond negative electrode material.
A method of Porous hollow carbon nano rod lithium ion battery negative material being prepared by template of Carapax Eriocheir sinensis, specifically
It completes according to the following steps:
One, it prepares Carapax Eriocheir sinensis template: 1., using tap water by discarded Carapax Eriocheir sinensis cleaning, then adopt and be washed with deionized 2~
4 times, drying is cooled to room temperature, obtains clean Carapax Eriocheir sinensis；2., clean Carapax Eriocheir sinensis smashed to pieces, be subsequently placed in tube furnace into
Row calcining, obtains gray powdery product, i.e. Carapax Eriocheir sinensis template；
Two, mixed carbon source: carbon source is dissolved in deionized water, and magnetic agitation 1h~10h, obtains carbon source solution, by crab
Crab shell template is added in carbon source solution, and magnetic agitation 2h~8h, obtains mixture；The mass ratio of the carbon source and deionized water
For 1:(3~7)；The mass ratio of the crab shell template and carbon source is 1:(1~5)；
Three, it is carbonized: heating being stirred to mixture at being 80 DEG C~110 DEG C in temperature, is heated with stirring in mixture
Moisture distilled-to-dryness obtains fixed mixture；Fixed mixture is transferred in tube furnace, is warming up under inert gas protection
600 DEG C~1000 DEG C, and under inert gas protection, be carbonized 1h~5h at being 600 DEG C~1000 DEG C in temperature, is cooled to room temperature
After take out, the material after being carbonized；
Four, diluted acid impregnates: the material after carbonization is put into dilute acid soln and impregnates 12h~for 24 hours, then be washed with deionized to
Neutrality, drying, obtains Porous hollow carbon nano rod lithium ion battery negative material.
The principle of the invention and advantage: one, Carapax Eriocheir sinensis is a kind of natural composite material, mainly by calcium carbonate (CaCO3), carbonic acid
Magnesium (MgCO3), protein and chitin composition show well-arranged porous structure, therefore the present invention in micromorphology
Using Carapax Eriocheir sinensis as the template for preparing porous structure material, the business templates such as silica monomer and silicon dioxide colloid are compared,
Crab shell template is not necessarily to be removed with the hydrofluoric acid (HF) with strong corrosive, and common dilute acid soln can slough template, solves existing
There is template to remove difficult problem, and using discarded Carapax Eriocheir sinensis as template raw material, realizes waste utilization, reduce cost.Two, of the invention
The Porous hollow carbon nano rod lithium ion battery negative material of preparation has Porous hollow club shaped structure, which has biggish
Specific surface area, it is possible to increase contact area between electrode and electrolyte provides more storage lithium active sites, in addition, can also significantly contract
The transmission path of short lithium ion and electronics improves migration rate, improves electrode high rate performance, while hollow structure is also material
Volume expansion provides cushion space, enhances the stable circulation performance of electrode.Three, with Porous hollow carbon nano rod prepared by the present invention
Material is active material, and acetylene black is conductive agent, and Kynoar (PVDF) is binder, prepares Porous hollow carbon nano rod electricity
Pole；It is to electrode, with the LiPF containing 1mol/L with metal lithium sheet again using Porous hollow carbon nano rod electrode as Electrode6
EC (ethylene carbonate)-DEC (diethyl carbonate)-DMC (dimethyl carbonate) solution be electrolyte, polypropylene porous film be every
Film is assembled into CR2025 type battery, and CR2025 type battery has excellent chemical property, and initial charge capacity is
508.6mAh/g, after being recycled 100 times with the current density of 100mA/g, reversible capacity is still able to maintain 502.2mAh/g or so,
Capacity retention ratio can maintain 98% or more, and when with the current density charge and discharge of 1A/g, electrode shows about 400.0mAh/g
Specific capacity, there is the battery prepared using Porous hollow carbon nano rod material prepared by the present invention as active material excellent length to follow
Ring stability and high rate performance.
Detailed description of the invention
Fig. 1 is the XRD spectrum of Porous hollow carbon nano rod lithium ion battery negative material prepared by embodiment 1；
Fig. 2 is the SEM figure of Porous hollow carbon nano rod lithium ion battery negative material prepared by embodiment 1；
Fig. 3 is the TEM figure of Porous hollow carbon nano rod lithium ion battery negative material prepared by embodiment 1；
Fig. 4 is CR2025 type cycle performance of battery figure prepared by embodiment 2, in figure ▲ indicating electric discharge, △ indicates charging；
Fig. 5 is CR2025 type battery high rate performance figure prepared by embodiment 2, in figure ● indicates electric discharge, zero indicates charging.
Specific embodiment
Specific embodiment 1: present embodiment be it is a kind of using Carapax Eriocheir sinensis as template prepare Porous hollow carbon nano rod lithium from
The method of sub- cell negative electrode material, is specifically realized by the following steps:
One, it prepares Carapax Eriocheir sinensis template: 1., using tap water by discarded Carapax Eriocheir sinensis cleaning, then adopt and be washed with deionized 2~
4 times, drying is cooled to room temperature, obtains clean Carapax Eriocheir sinensis；2., clean Carapax Eriocheir sinensis smashed to pieces, be subsequently placed in tube furnace into
Row calcining, obtains gray powdery product, i.e. Carapax Eriocheir sinensis template；
Two, mixed carbon source: carbon source is dissolved in deionized water, and magnetic agitation 1h~10h, obtains carbon source solution, by crab
Crab shell template is added in carbon source solution, and magnetic agitation 2h~8h, obtains mixture；The mass ratio of the carbon source and deionized water
For 1:(3~7)；The mass ratio of the crab shell template and carbon source is 1:(1~5)；
Three, it is carbonized: heating being stirred to mixture at being 80 DEG C~110 DEG C in temperature, is heated with stirring in mixture
Moisture distilled-to-dryness obtains fixed mixture；Fixed mixture is transferred in tube furnace, is warming up under inert gas protection
600 DEG C~1000 DEG C, and under inert gas protection, be carbonized 1h~5h at being 600 DEG C~1000 DEG C in temperature, is cooled to room temperature
After take out, the material after being carbonized；
Four, diluted acid impregnates: the material after carbonization is put into dilute acid soln and impregnates 12h~for 24 hours, then be washed with deionized to
Neutrality, drying, obtains Porous hollow carbon nano rod lithium ion battery negative material.
China's crab class product resource is abundant, and the Carapax Eriocheir sinensis after eating is generally regarded as rubbish and throws away, and it is negative to increase environment
Load.Carapax Eriocheir sinensis is a kind of natural composite material, mainly by calcium carbonate (CaCO3), magnesium carbonate (MgCO3), protein and chitin group
At showing well-arranged porous structure in micromorphology, therefore present embodiment is using Carapax Eriocheir sinensis as preparing porous knot
The template of structure material, compared to business templates such as silica monomer and silicon dioxide colloids, crab shell template is not necessarily to strong rotten with having
The hydrofluoric acid (HF) of corrosion removes, and common dilute acid soln can slough template, and it is difficult to solve the problems, such as that existing template removes, and
Using discarded Carapax Eriocheir sinensis as template raw material, realizes waste utilization, reduce cost.
Specific embodiment 2: the difference of present embodiment and specific embodiment one is: carbon source described in step 2
For expired honey, expired white granulated sugar or expired egg.Other are same as the specific embodiment one.
Expired honey, expired white granulated sugar or expired egg are directly processed, and cause the wasting of resources.Present embodiment with
Expired honey, expired white granulated sugar or expired egg are used as carbon source, and reaching reduces cost, solves the problems, such as the wasting of resources.
Specific embodiment 3: one of present embodiment and specific embodiment one or two difference are: step 1 1. in
The drying concrete operations are as follows: in convection oven, dry 4h~12h at being 80 DEG C in temperature.Other and specific embodiment party
Formula one or two is identical.
Specific embodiment 4: one of present embodiment and specific embodiment one to three difference are: step 1 2. in
The calcining design parameter is as follows: calcination temperature is 300 DEG C~400 DEG C, and calcination time is 2h~6h.Other and specific embodiment party
Formula one to three is identical.
Specific embodiment 5: one of present embodiment and specific embodiment one to four difference are: in step 3
600 DEG C~1000 DEG C are warming up to for 5 DEG C/min~10 DEG C/min under inert gas shielding with heating rate.Other and specific implementation
Mode one to four is identical.
Specific embodiment 6: one of present embodiment and specific embodiment one to five difference are: institute in step 4
State dilute acid soln be concentration be 2mol/L~6mol/L hydrochloric acid, concentration be 1mol/L~3mol/L nitric acid or concentration be
The acetic acid of 2mol/L~4mol/L.Other are identical as specific embodiment one to five.
Specific embodiment 7: one of present embodiment and specific embodiment one to six difference are: institute in step 4
It is as follows to state drying concrete operations: in a vacuum drying oven, dry 6h~12h at being 80 DEG C in temperature.Other and specific embodiment party
Formula one to six is identical.
The content of present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several specific embodiments
The purpose of invention also may be implemented in contract sample.
Using following verification experimental verifications effect of the present invention
A kind of embodiment 1: side preparing Porous hollow carbon nano rod lithium ion battery negative material using Carapax Eriocheir sinensis as template
Method is specifically realized by the following steps:
One, it prepares Carapax Eriocheir sinensis template: 1., by discarded Carapax Eriocheir sinensis using originally water washing 3 times, then adopt and be washed with deionized
3 times, drying is cooled to room temperature, obtains clean Carapax Eriocheir sinensis；2., clean Carapax Eriocheir sinensis smashed to pieces, be subsequently placed in tube furnace into
Row calcining, obtains gray powdery product, i.e. Carapax Eriocheir sinensis template；
Two, mixed carbon source: carbon source is dissolved in deionized water, and magnetic agitation 5h, obtains carbon source solution, by crab shell mold
Plate is added in carbon source solution, and magnetic agitation 4h, obtains mixture；The mass ratio of the carbon source and deionized water is 1:5；It is described
The mass ratio of crab shell template and carbon source is 1:2；The carbon source is expired honey；
Three, it is carbonized: heating being stirred to mixture at being 80 DEG C in temperature, moisture in mixture is heated with stirring to and is evaporated
Until, obtain fixed mixture；Fixed mixture is transferred in tube furnace, under inert gas protection with heating rate for 5
DEG C/min is warming up to 800 DEG C, and under inert gas protection, be carbonized 2h at being 800 DEG C in temperature, takes out after being cooled to room temperature,
Material after being carbonized；
Four, diluted acid impregnates: the material after carbonization is put into dilute acid soln and is impregnated for 24 hours, then is washed with deionized to neutrality,
Drying, obtains Porous hollow carbon nano rod lithium ion battery negative material.
1 step 1 of embodiment 1. described in drying concrete operations it is as follows: in convection oven, temperature be at 80 DEG C it is dry
8h。
1 step 1 of embodiment 2. described in calcining design parameter it is as follows: calcination temperature be 350 DEG C, calcination time 6h.
Dilute acid soln described in 1 step 4 of embodiment is the hydrochloric acid that concentration is 2mol/L.
The Porous hollow carbon nano rod lithium ion battery negative material prepared to embodiment 1 detects, and testing result is such as
Shown in Fig. 1, Fig. 1 is the XRD spectrum of Porous hollow carbon nano rod lithium ion battery negative material prepared by embodiment 1, passes through Fig. 1
Know that the Porous hollow carbon nano rod lithium ion battery negative material of the preparation of embodiment 1 at 26.2 °, 42.2 ° and 44.3 °, is deposited
In three broad peaks, (002) diffraction maximum of disordered carbon is corresponded respectively to, the diffraction maximum of graphitized carbon (100) and (101) corresponds to
JCPDS card number 25-0284 shows the carbon material of preparation amorphization degree with higher.
The Porous hollow carbon nano rod lithium ion battery negative material prepared to embodiment 1 is observed, and observation result is such as
Shown in Fig. 2 and 3, Fig. 2 is the SEM figure of Porous hollow carbon nano rod lithium ion battery negative material prepared by embodiment 1, and Fig. 3 is
The TEM of Porous hollow carbon nano rod lithium ion battery negative material prepared by embodiment 1 schemes, as can be seen from Figure 2 embodiment 1
Uniform bar array is presented in the Porous hollow carbon nano rod lithium ion battery negative material of preparation, and the average diameter of stick is about 70nm
Left and right, and there are many holes on carbon nano rod surface.As seen from Figure 3, Porous hollow carbon nano rod lithium ion prepared by embodiment 1
Cell negative electrode material has hollow structure.
Embodiment 2: the method for preparing electrode, assembled battery as active material using Porous hollow carbon nano rod is specifically pressed
What following steps were completed:
One, it prepares Porous hollow carbon nano rod electrode: being to live with Porous hollow carbon nano rod lithium ion battery negative material
Property substance, acetylene black is conductive agent, Kynoar (PVDF) be binder, prepare Porous hollow carbon nano rod electrode；
Two, it assembles: being to electrode, to contain 1mol/L with metal lithium sheet using Porous hollow carbon nano rod electrode as cathode
LiPF6EC (ethylene carbonate)-DEC (diethyl carbonate)-DMC (dimethyl carbonate) solution be electrolyte, polypropylene is more
Pore membrane is diaphragm, is assembled into CR2025 type battery；The LiPF containing 1mol/L6EC (ethylene carbonate)-DEC (carbonic acid two
Ethyl ester) volume ratio of EC:DEC:DMC is 1:1:1 in-DMC (dimethyl carbonate) solution.
CR2025 type battery prepared by embodiment 2 obtains cycle performance figure such as Fig. 4 with current cycle 100 times of 100mA/g
It is shown, in figure ▲ indicating electric discharge, △ indicates charging, and as shown in Figure 4, CR2025 type battery prepared by embodiment 2 fills for the first time
Capacitance is 508.6mAh/g, after circulation 100 times, is still able to maintain the reversible capacity of 502.2mAh/g, reversible capacity is kept
Rate is 98.7%, illustrates that CR2025 type battery prepared by embodiment 2 has excellent cyclical stability.
Fig. 5 is the high rate performance figure that CR2025 type battery prepared by embodiment 2 carries out charge and discharge with different current densities,
In figure ● indicate electric discharge, zero indicates charging.When current density increases to 1A/g, embodiment 2 prepare CR2025 type battery according to
So with the reversible capacity of about 400.0mAh/g, the CR2025 type battery high current with higher for showing prepared by embodiment 2 is filled
Discharge performance.
Claims (7)
1. a kind of method for preparing Porous hollow carbon nano rod lithium ion battery negative material as template using Carapax Eriocheir sinensis, feature exist
It is completed by the following steps in it:
One, it prepares Carapax Eriocheir sinensis template: 1., using tap water by discarded Carapax Eriocheir sinensis cleaning, then adopt and be washed with deionized 2~4 times,
Drying, is cooled to room temperature, obtains clean Carapax Eriocheir sinensis；2., clean Carapax Eriocheir sinensis smashed to pieces, be subsequently placed in tube furnace and forged
It burns, obtains gray powdery product, i.e. Carapax Eriocheir sinensis template；
Two, mixed carbon source: carbon source is dissolved in deionized water, and magnetic agitation 1h~10h, obtains carbon source solution, by Carapax Eriocheir sinensis
Template is added in carbon source solution, and magnetic agitation 2h~8h, obtains mixture；The mass ratio of the carbon source and deionized water is 1:
(3~7)；The mass ratio of the crab shell template and carbon source is 1:(1~5)；
Three, it is carbonized: heating being stirred to mixture at being 80 DEG C~110 DEG C in temperature, is heated with stirring to moisture in mixture
Distilled-to-dryness obtains fixed mixture；Fixed mixture is transferred in tube furnace, is warming up to 600 under inert gas protection
DEG C~1000 DEG C, and under inert gas protection, be carbonized 1h~5h at being 600 DEG C~1000 DEG C in temperature, after being cooled to room temperature
It takes out, the material after being carbonized；
Four, diluted acid impregnates: the material after carbonization being put into dilute acid soln and impregnates 12h~for 24 hours, then is washed with deionized into
Property, drying obtains Porous hollow carbon nano rod lithium ion battery negative material.
2. one kind according to claim 1 prepares Porous hollow carbon nano rod negative electrode of lithium ion battery by template of Carapax Eriocheir sinensis
The method of material, it is characterised in that carbon source described in step 2 is expired honey, expired white granulated sugar or expired egg.
3. one kind according to claim 2 prepares Porous hollow carbon nano rod negative electrode of lithium ion battery by template of Carapax Eriocheir sinensis
The method of material, it is characterised in that step 1 1. described in drying concrete operations it is as follows: in convection oven, temperature be 80 DEG C
Lower dry 4h~12h.
4. one kind according to claim 3 prepares Porous hollow carbon nano rod negative electrode of lithium ion battery by template of Carapax Eriocheir sinensis
The method of material, it is characterised in that step 1 2. described in calcining design parameter it is as follows: calcination temperature be 300 DEG C~400 DEG C, forge
The burning time is 2h~6h.
5. one kind according to claim 2 prepares Porous hollow carbon nano rod negative electrode of lithium ion battery by template of Carapax Eriocheir sinensis
The method of material, it is characterised in that under inert gas protection with heating rate for 5 DEG C/min~10 DEG C/min liter in step 3
Temperature is to 600 DEG C~1000 DEG C.
6. one kind according to claim 2 prepares Porous hollow carbon nano rod negative electrode of lithium ion battery by template of Carapax Eriocheir sinensis
The method of material, it is characterised in that dilute acid soln described in step 4 be concentration be 2mol/L~6mol/L hydrochloric acid, concentration be
The nitric acid or concentration of 1mol/L~3mol/L is the acetic acid of 2mol/L~4mol/L.
7. one kind according to claim 2 prepares Porous hollow carbon nano rod negative electrode of lithium ion battery by template of Carapax Eriocheir sinensis
The method of material, it is characterised in that drying concrete operations described in step 4 is as follows: being 80 DEG C in temperature in a vacuum drying oven
Lower dry 6h~12h.
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| CN116666585A (en) * | 2023-06-08 | 2023-08-29 | 江苏久泰电池科技有限公司 | Negative electrode material of sodium ion battery, negative electrode plate and sodium ion battery |
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