CN108163852A - A kind of ganoderma lucidum base two-dimensional sheet carbon material and preparation method thereof and the application as secondary cell negative pole material - Google Patents
A kind of ganoderma lucidum base two-dimensional sheet carbon material and preparation method thereof and the application as secondary cell negative pole material Download PDFInfo
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- CN108163852A CN108163852A CN201810005167.5A CN201810005167A CN108163852A CN 108163852 A CN108163852 A CN 108163852A CN 201810005167 A CN201810005167 A CN 201810005167A CN 108163852 A CN108163852 A CN 108163852A
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- ganoderma lucidum
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
Application the invention discloses a kind of ganoderma lucidum base two-dimensional sheet carbon material and preparation method thereof and as secondary battery cathode material.The preparation of carbon material is that dry glossy ganoderma crushing is placed in activator solution to impregnate; drying; under protective atmosphere; high temperature cabonization obtains the carbon material of flourishing, defect prosperity the two-dimensional sheet of specific surface area height, pore structure; the two-dimensional sheet carbon material is used as lithium ion battery, sodium ion battery electrode material, shows excellent chemical property.Ganoderma Lucidum is short with growth cycle, the advantages such as of low cost, and the preparation method technological process of two-dimensional sheet carbon material is simple, with short production cycle, environmental-friendly, is conducive to industrialized production.
Description
Technical field
The present invention relates to a kind of fungi base carbon material, more particularly to one kind prepares high-specific surface area based on Ganoderma Lucidum
The method of porous two-dimensional sheet carbon material as well as lithium ion battery, the application of anode material of lithium-ion battery, belong to
Carbon material preparation field.
Background technology
Carbon material gives up because having the characteristics that excellent adsorptivity, good thermal stability, higher mechanical strength in waste water
Gas disposal, electrode material, bio-carrier etc. have a good application prospect, and cause the extensive concern of domestic and foreign scholars.
The raw material for being traditionally used for preparing carbon material is mainly the fossil resources such as oil, coal, with the development of human society, resource profit
Structure is changing, and fossil resource consumption speedup slows down, and renewable resource becomes the hot spot of scholars' research.
In recent years, biomass carbon, because its is cheap, reserves are huge, environmentally friendly, starts as a kind of emerging renewable resource
By extensive concern.
Carbon material currently on the market is mainly wooden carbon material, and raw material mainly has bamboo, coconut husk etc..But these former materials
The shortcomings of material generally existing growth cycle is long, growth takes up a large area, as raw material during carbon material is prepared activity yied
Relatively low, manufacturing cost is higher.
In recent years with the exacerbation of energy crisis, people also increasingly promote the concern of electrochemical energy storing device.Carbon material
Also it is increasingly used in electrochemical energy storing device (such as lithium ion battery, sodium-ion battery) etc..For lithium ion battery
For, graphite is using the carbon material for being most also extensively earliest commercial applications.However sodium-ion battery is due to its ionic radius
More than lithium ion so that graphite can not show good performance as its electrode material.
Invention content
It is lacked for biomass carbon material in the prior art as battery electrode material there are specific surface is low, pore volume is low etc.
It falls into, first purpose of the invention is to be to provide that a kind of specific surface area is high, pore volume is high, defect prosperity ganoderma lucidum base two-dimensional slice
Shape carbon material.
For the raw material for being used to prepare biomass carbon material in the prior art, such as there are growth cycles for bamboo, cocoanut shell
It is long, floor space is wide, low yield, it is of high cost the shortcomings of, second object of the present invention is to be to provide one kind with artificial culture
Ganoderma lucidum is raw material, the method that quick, efficient, low cost, high yield prepare carbon material；Ganoderma Lucidum growth cycle is short, into
This is low, and carbon yield is high, is conducive to industrialized production.
Third object of the present invention is to be to provide a kind of carbon material as lithium ion battery or sodium-ion battery
With the lithium ion battery or sodium-ion battery of its preparation, it is excellent to show capacity height, good cycle etc. for the application of negative material
Point.
In order to realize above-mentioned technical purpose, the present invention provides a kind of preparation method of ganoderma lucidum base carbon material, this method is
Ganoderma lucidum is dried and is ground into powder, ganoderma powder is placed in activator solution impregnate after, drying, under an inert atmosphere, with 5~
The rate of 15 DEG C/min be warming up to 600~1100 DEG C carbonization 0.5~10h to get；
Activator and the mass ratio of ganoderma powder are 2~8 in the activator solution:1；
The activator includes at least one of potassium hydroxide, zinc chloride, phosphoric acid.
Preferred scheme, activator and the mass ratio of ganoderma powder are 3~5 in the activator solution:1.When not adding
During activator, the obtained active carbon material being bar-like, specific surface area is small (to be less than 300m2/ g), pore volume is small (to be less than
0.3cm2g-1), when the mass ratio for adding activator and ganoderma powder is less than 2, what is obtained is granular active carbon material,
Specific surface area is small (to be less than 800m2/ g), pore volume is small (to be less than 0.6cm2g-1), both materials are all not as lithium ion or sodium
The optimal material of ion battery.When activator and the mass ratio of ganoderma powder are more than 2, the carbon material of preparation is sheet carbon materials
Material, and specific surface area and pore volume significantly improve (specific surface be 800~1100m2/ g, pore volume are 0.6~1.2cm2g-1), it is special
It is not that also there is the defects of more, is conducive to store up sodium and stores up lithium.And the yield of carbon material can be substantially reduced during activator excess, and
Coulombic efficiency for the first time when carbon material is as lithium ion battery or anode material of lithium-ion battery is substantially reduced.Therefore it preferably activates
The mass ratio of agent and ganoderma powder is 3~5:In the range of 1, high-quality carbon material can be not only obtained, and improve carbon material yield.
Preferred scheme, the activator solution are the near saturated solution containing activator, saturated solution or supersaturated solution.
Preferred activator is potassium hydroxide.Using potassium hydroxide as activating agent, the carbon material specific surface area for preparing and mesoporous contain
Amount is substantially higher in use zinc chloride and phosphoric acid as activator.
Preferred scheme, the ganoderma lucidum are Ganoderma Lucidum.It is had the following advantages using Ganoderma Lucidum：Ganoderma lucidum gives birth to
Long period is short, at low cost, and general artificial cultivation period is only 90 days, and about 25 yuan/kg at low cost, ganoderma lucidum belongs to Mycophyta, tool
There is a special fibre structure, and rich in organic composition, higher carbon rate is obtained in the relatively other biological energy sources of carbonisation, one
As higher than 30%, consider, using Ganoderma Lucidum as carbonized stock, compared to raw materials such as coconut husk, bamboos, cost compared with
It is low.Ganoderma lucidum rich in porous structure, by appropriate reaction condition, can further regulate and control pore structure in itself, obtain specific surface
For 800~1100m2/ g, pore volume are 0.6~1.2cm2g-1Two-dimensional sheet carbon material, be conducive to obtain high electrochemical activity
Lithium ion or sodium-ion battery material.
Preferred scheme, the carburizing temperature are 750~850 DEG C.When temperature is less than 750 DEG C, the two-dimensional sheet carbon of preparation
The specific surface area size and order degree of material are substantially reduced, and temperature be higher than 850 DEG C when, although two-dimensional sheet carbon material has
Sequence degree increases, but yield is significantly relatively low, therefore preferably carburizing temperature can not only obtain high-quality in the range of 750~850 DEG C
Two-dimensional sheet carbon material, and improve carbon material yield.
Preferred scheme, the time of the carbonization is 1~2h.At the same temperature, when carbonization time is more than 2h, during carbonization
Between extend the specific surface area and pore volume of carbon material be not obviously improved, and during less than 1 hour, specific surface area size and hole
Volume is significantly relatively low, it is therefore preferable that carbonization time is 1~2h.
Preferred scheme, heating rate are 8~12 DEG C/min.
The present invention provides a kind of ganoderma lucidum base carbon materials, are obtained by above-mentioned preparation method.
Preferred scheme, the specific surface of the ganoderma lucidum base carbon material is 800~1100m2/ g, pore volume for 0.6~
1.2cm2g-1。
The present invention also provides a kind of applications of ganoderma lucidum base carbon material, are born as lithium ion battery or sodium-ion battery
Pole material application.
The ganoderma powder of the present invention be by fresh glossy ganoderma through drying, washing, drying, pulverization process obtains.Ganoderma powder is
Flocculent structure.
The protective atmosphere of the present invention includes at least one of nitrogen, argon gas, helium.
The dipping process of the present invention is generally 5~for 24 hours, preferably 8~16h.
The drying of the present invention is forced air drying.
The carbonized product of the present invention generally uses neutralization, filtering, the washing and drying treatment of this field routine.
The N-process of the present invention is neutralized using diluted acid or dilute alkaline soln, and such as 1:20~1:5 dilute hydrochloric acid or 0.1~
The KOH solution of 1mol/L, preferred neutralization reagent are 1:10~1:8 dilute hydrochloric acid or the KOH solution of 0.5~0.8mol/L.
The water-washing process of the present invention is using deionized water, and washing lotion is neutrality after the completion of cleaning.
The present invention prepares the preferred method of high specific surface area porous two-dimensional sheet carbon material：Dry ganoderma powder is placed in hydrogen
After being impregnated in potassium oxide solution, drying is placed under protective atmosphere, 750~850 DEG C of carbon is warming up to the rate of 8~12 DEG C/min
It is 800~1100m to change 1~2h to get specific surface area2/ g, pore volume are 0.6~1.2cm2g-1Carbon material, wherein, the hydrogen
Potassium hydroxide and the mass ratio of ganoderma powder are 3~5 in potassium oxide solution:1.The preferred scheme is ensureing that carbon material is higher
Under the premise of yield, can prepare high-specific surface area, high pore volume and carbon material that order is suitable.
The present invention also provides the application of high specific surface area porous two-dimensional sheet carbon material, as lithium ion battery or
Anode material of lithium-ion battery application.The specific preparation method of lithium ion and anode material of lithium-ion battery is：By carboxymethyl fibre
It is after dimension plain (CMC) is dissolved in water stirring 4-6 hours, the carbon material being prepared, conductive carbon black grinding half an hour is mixed above
Adhesive solution is added in after even to continue after stirring 12 hours, is placed in vacuum drying chamber coated on copper foil, treating that water volatilizees
Dry 12h at 80 DEG C, you can obtain lithium from battery and sodium-ion battery electrode.Carbon material material, carboxymethyl cellulose
(CMC), conductive carbon black in mass ratio 70:15:15.
Compared with the prior art, the advantageous effects that technical scheme of the present invention is brought：
1st, carbon material specific surface of the invention is up to 800~1100m2/ g, pore volume is up to 0.6~1.2cm2g-1, and it is rich
Containing defect, be conducive to store up lithium and store up sodium.
2nd, the preparation process of carbon material of the invention is prepared using a step activation method, and step is simple, and low energy consumption, cost
It is low, be conducive to industrialized production.
3. the carbon material of the present invention uses the ganoderma lucidum of artificial culture as raw material, cultivation period is short (being only 90 days), at low cost
(about 25 yuan/kg), are of relatively low cost.
4th, carbon material of the invention can be used for preparing lithium ion battery or sodium-ion battery electrode material.
Description of the drawings
【Fig. 1】It is the stereoscan photograph of ganoderma lucidum base carbon material obtained in comparative example 1；
【Fig. 2】It is the stereoscan photograph of ganoderma lucidum base carbon material obtained in comparative example 2；
【Fig. 3】It is the stereoscan photograph of ganoderma lucidum base carbon material obtained in comparative example 3；
【Fig. 4】It is the stereoscan photograph of ganoderma lucidum base carbon material obtained in embodiment 1；
【Fig. 5】It is the nitrogen adsorption desorption curve of the ganoderma lucidum base carbon material obtained in embodiment 1；
【Fig. 6】It is the Raman test chart of ganoderma lucidum base carbon material obtained in embodiment 1；
【Fig. 7】It is the stereoscan photograph of ganoderma lucidum base carbon material obtained in embodiment 2；
【Fig. 8】It is the cycle performance figure of the electrode assembled in embodiment 3；
【Fig. 9】It is the cycle performance figure of the electrode assembled in embodiment 4.
Specific embodiment
Following embodiment is in order to which the present invention is explained in greater detail, these embodiments do not form any restrictions to the present invention,
The present invention can be implemented as the either type described in invention content.
Comparative example 1
Ganoderma lucidum tap water is rinsed 4-5 times, dry crush afterwards for 24 hours is placed in 80 DEG C of air dry ovens and obtains cotton-shaped ganoderma lucidum
Powder.2g glossy ganoderma powders are placed in porcelain boat, under inert gas shielding, 800 DEG C of calcining 2h, heating rate is 10 DEG C/min, is dropped naturally
Temperature, the product grind into powder that will be obtained are filtered after ultrasonic 5min, then clean 4-5 after with deionized water, are placed in vacuum drying
12h is dried in vacuo at 110 DEG C of case, obtains ganoderma lucidum base carbon material.Fig. 1 is its scanning electron microscope diagram piece, and it is rodlike to find it
Structure, nitrogen adsorption desorption curve show that its specific surface area is 160m2g-1, total pore volume 0.11cm3g-1, yield is 43% (phase
Dry glossy ganoderma powder is calculated).
Comparative example 2
Ganoderma lucidum tap water is rinsed 4-5 times, dry crush afterwards for 24 hours is placed in 80 DEG C of air dry ovens and obtains cotton-shaped ganoderma lucidum
Powder.2g glossy ganoderma powders are placed in porcelain boat, under inert gas shielding, 1000 DEG C of calcining 2h, heating rate is 10 DEG C/min, is dropped naturally
Temperature, the product grind into powder that will be obtained are filtered after ultrasonic 5min, then clean 4-5 after with deionized water, are placed in vacuum drying
12h is dried in vacuo at 110 DEG C of case, obtains ganoderma lucidum base carbon material.Fig. 2 is its scanning electron microscope diagram piece, and it is rodlike to find it
Structure, but size is significantly less than the carbon material that comparative example 1 obtains, and nitrogen adsorption desorption curve shows that its specific surface area is
230m2g-1, total pore volume 0.24cm3g-1, yield is 38% (being calculated with respect to dry glossy ganoderma powder).
Comparative example 3
Ganoderma lucidum tap water is rinsed 4-5 times, dry crush afterwards for 24 hours is placed in 80 DEG C of air dry ovens and obtains cotton-shaped ganoderma lucidum
Powder.5g potassium hydroxide is dissolved in 15mL deionized waters, 5g glossy ganoderma powders is added in, is sufficiently stirred, 55 DEG C are transferred to after sealing and standing 12h
Air dry oven dries 12h.The grinding of partial immersion object is taken to be placed on porcelain boat, under inert gas shielding, 700 DEG C of calcining 2h rise
Warm rate be 10 DEG C/min, Temperature fall, the product grind into powder that will be obtained, add in 1:6 salt acid for adjusting pH for it is neutral extremely
Faintly acid is filtered after ultrasonic 5min, and obtained product cleans 4-5 after with deionized water again, is placed at 110 DEG C of vacuum drying chamber
12h is dried in vacuo, obtains ganoderma lucidum base carbon material.Fig. 3 is its scanning electron microscope diagram piece, is found to be irregular particle shape knot
Structure, nitrogen adsorption desorption curve show that its specific surface area is 760m2g-1, total pore volume 0.58cm3g-1, yield is 34% (opposite
Dry glossy ganoderma powder calculates).
Embodiment 1
Ganoderma lucidum tap water is rinsed 4-5 times, dry crush afterwards for 24 hours is placed in 80 DEG C of air dry ovens and obtains cotton-shaped ganoderma lucidum
Powder.15g potassium hydroxide is dissolved in 30mL deionized waters, 5g glossy ganoderma powders is added in, is sufficiently stirred, 55 are transferred to after sealing and standing 12h
DEG C air dry oven drying 12h.The grinding of partial immersion object is taken to be placed on porcelain boat, under inert gas shielding, 800 DEG C of calcining 2h,
Heating rate be 10 DEG C/min, Temperature fall, the product grind into powder that will be obtained, add in 1:6 salt acid for adjusting pH is neutrality
It to faintly acid, is filtered after ultrasonic 5min, obtained product cleans 4-5 after with deionized water again, is placed in 110 DEG C of vacuum drying chamber
Lower vacuum drying 12h obtains ganoderma lucidum base carbon material.Fig. 4 is its scanning electron microscope diagram piece, is found to be laminated structure, nitrogen
Adsorption desorption curve (Fig. 5) shows that its specific surface area is 980m2g-1, total pore volume 0.78cm3g-1, yield is 31% (relatively dry
Glossy ganoderma powder calculates), Raman collection of illustrative plates shows that the ratio at (Fig. 6) its D peak and G peaks is 0.86, it was demonstrated that there are a large amount of crystal defects.
Embodiment 2
Ganoderma lucidum tap water is rinsed 4-5 times, dry crush afterwards for 24 hours is placed in 80 DEG C of air dry ovens and obtains cotton-shaped ganoderma lucidum
Powder.20g potassium hydroxide is dissolved in 45mL deionized waters, 5g glossy ganoderma powders is added in, is sufficiently stirred, 55 are transferred to after sealing and standing 12h
DEG C air dry oven drying 12h.The grinding of partial immersion object is taken to be placed on porcelain boat, under inert gas shielding, 850 DEG C of calcining 2h,
Heating rate be 10 DEG C/min, Temperature fall, the product grind into powder that will be obtained, add in 1:6 salt acid for adjusting pH is neutrality
It to faintly acid, is filtered after ultrasonic 5min, obtained product cleans 4-5 after with deionized water again, is placed in 110 DEG C of vacuum drying chamber
Lower vacuum drying 12h obtains ganoderma lucidum base carbon material.Fig. 7 is its scanning electron microscope diagram piece, finds it as laminated structure, and
It is significantly less than the carbon material that embodiment 3 obtains.Nitrogen adsorption desorption curve shows that its specific surface area is 1040m2g-1, total pore volume
For 0.82cm3g-1, yield is 29% (being calculated with respect to dry glossy ganoderma powder)
Embodiment 3
After carboxymethyl cellulose (CMC) is dissolved in water stirring 4-6 hours, by the carbon material being prepared in embodiment 1, lead
Electrical carbon black grinding half an hour it is mixed above uniformly after add in after adhesive solution continues stirring 12 hours, coated on copper foil,
It treats that water volatilization is placed in vacuum drying chamber at 80 DEG C dry 12h, obtains lithium from electrode material for battery.It is negative using the electrode
Cathode is done in pole, metal lithium sheet, and polypropylene is diaphragm, the LiPF of 1M6Do electrolyte.Electrochemical property test shows (Fig. 8), obtains
Ganoderma lucidum base carbon material for lithium ion battery have preferable chemical property, its charge-discharge test is shown in 0.1A g-1
Current density under, capacity is up to 557mAh g-1；In 0.1A g-1Current density under recycle 200 times after, reversible specific volume
Amount is still up to 180mAh g-1.The material also shows good cycle performance.In 6.4A g-1Current density under, it is reversible
Specific capacity still has 80mAh g-1。
Embodiment 4
After carboxymethyl cellulose (CMC) is dissolved in water stirring 4-6 hours, by the carbon material being prepared in embodiment 4, lead
Electrical carbon black grinding half an hour it is mixed above uniformly after add in after adhesive solution continues stirring 12 hours, coated on copper foil,
It treats that water volatilization is placed in vacuum drying chamber at 80 DEG C dry 12h, obtains sodium from electrode material for battery.It is negative using the electrode
Cathode is done in pole, metallic sodium, and polypropylene is diaphragm, the NaClO of 1M4Do electrolyte.Electrochemical property test shows (Fig. 9), obtains
Ganoderma lucidum base carbon material for sodium-ion battery have preferable chemical property, its charge-discharge test is shown in 0.1A g-1
Current density under recycle 200 times after, reversible specific capacity still be up to 170mAh g-1。
Claims (10)
1. a kind of preparation method of ganoderma lucidum base two-dimensional sheet carbon material, it is characterised in that：Ganoderma powder is placed in activator solution
After middle dipping, drying under an inert atmosphere, 600~1100 DEG C of 0.5~10h of carbonization is warming up to the rate of 5~15 DEG C/min,
To obtain the final product；
Activator and the mass ratio of ganoderma powder are 2~8 in the activator solution:1；
The activator includes at least one of potassium hydroxide, zinc chloride, phosphoric acid.
2. the preparation method of ganoderma lucidum base two-dimensional sheet carbon material according to claim 1, it is characterised in that：The activator
Activator and the mass ratio of ganoderma powder are 3~5 in solution:1.
3. the preparation method of ganoderma lucidum base two-dimensional sheet carbon material according to claim 2, it is characterised in that：The activator
Solution is the near saturated solution containing activator, saturated solution or supersaturated solution.
4. the preparation method of ganoderma lucidum base two-dimensional sheet carbon material according to claim 1, it is characterised in that：The ganoderma lucidum is
Ganoderma Lucidum.
5. the preparation method of Claims 1 to 4 any one of them ganoderma lucidum base two-dimensional sheet carbon material, it is characterised in that：It is described
Carburizing temperature is 750~850 DEG C.
6. the preparation method of ganoderma lucidum base two-dimensional sheet carbon material according to claim 5, it is characterised in that：The carbonization
Time is 1~2h.
7. the preparation method of ganoderma lucidum base two-dimensional sheet carbon material according to claim 5, it is characterised in that：Heating rate is
8~12 DEG C/min.
8. a kind of ganoderma lucidum base two-dimensional sheet carbon material, it is characterised in that：It is obtained by any one of claim 1~7 preparation method.
9. ganoderma lucidum base two-dimensional sheet carbon material according to claim 8, it is characterised in that：The ratio of the ganoderma lucidum base carbon material
Surface is 800~1100m2/ g, pore volume are 0.6~1.2cm2g-1。
10. the application of the ganoderma lucidum base two-dimensional sheet carbon material described in claim 8 or 9, it is characterised in that：As lithium ion battery
Or anode material of lithium-ion battery application.
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| CN111072007A (en) * | 2019-12-12 | 2020-04-28 | 广西大学 | Preparation method and application of biomass-based three-dimensional multi-cavity graphene-like carbon capsule |
| CN114715985A (en) * | 2022-04-12 | 2022-07-08 | 南京大学 | Electrochemical desalination system constructed from mycelium-derived carbon |
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| CN111072007A (en) * | 2019-12-12 | 2020-04-28 | 广西大学 | Preparation method and application of biomass-based three-dimensional multi-cavity graphene-like carbon capsule |
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