CN110176597A - A kind of preparation and application of biomass carbon/sulphur composite material - Google Patents
A kind of preparation and application of biomass carbon/sulphur composite material Download PDFInfo
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- CN110176597A CN110176597A CN201910536528.3A CN201910536528A CN110176597A CN 110176597 A CN110176597 A CN 110176597A CN 201910536528 A CN201910536528 A CN 201910536528A CN 110176597 A CN110176597 A CN 110176597A
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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
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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
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention discloses a kind of biomass carbon/sulphur composite material preparation methods, are to crush shinyleaf yellowhorn shell after dehydrating, and add pore creating material, high temperature cabonization, obtains multiporous biological matter carbon material under inert gas atmosphere；Again by multiporous biological matter carbon material and sublimed sulfur after ground and mixed is uniform in certain proportion, sulphur is diffused into the hole of carbon by being heat-treated heating melting, then remove sulphur remained on surface using solvent dissolving method, biomass carbon/sulphur composite material is made.Sulphur is filled into porous carbon materials, increases the electrical contact ability of sulphur and carbon material, and promotes the volume energy density of composite material；The porous structure of carbon material can reach the effect for being anchored soluble polysulfide, and can accommodate volume change of sulphur during charge/discharge.Using the composite material as lithium sulfur battery anode material or anode material of lithium-ion battery in use, having good chemical property.
Description
Technical field
The present invention relates to a kind of preparations of carbon/sulphur composite material, are mainly used as lithium sulfur battery anode material or sodium ion electricity
The negative electrode material in pond, belongs to field of compound material and field of new energy technologies.
Background technique
Lithium-sulfur cell is using element sulphur as anode, and a kind of lithium battery of the lithium metal as cathode, specific capacity is up to
1675mAh/g, the capacity (< 150mAh/g) of significantly larger than commercial widely applied cobalt acid lithium battery.And sulphur is a kind of right
Environmental-friendly element does not pollute environment substantially, is a kind of very promising lithium ion battery.Though although lithium-sulfur cell
It so has many good qualities, but there is also some matter of science and technology, hinder the practical application of lithium-sulfur cell.Firstly, sulphur is a kind of
The very low insulator of conductivity, only 5 × 10-28 Sm-1, which has limited the utilizations of sulphur, reduce the high rate performance of lithium-sulfur cell；
Secondly, the intermediate product polysulfide generated in electrochemical reaction process is easily dissolved in electrolyte, since " shuttle effect for it
Answer " loss that leads to active material, reduce specific capacity and coulombic efficiency.In addition, conference is crossed in volume expansion in cyclic process
Lead to the cyclical stability of difference.
The complicated electrochemical reaction process of sulfur-bearing anode and its physical properties such as non-conductive determine the research and development of lithium-sulfur cell
Difficult point is mainly in positive electrode.For the application for realizing lithium-sulfur cell, the conductivity of positive electrode is improved, on the one hand to improve just
The utilization rate of pole active material improves the high rate performance of battery；On the other hand to inhibit the irreversible loss of capacity, also to improve
The cycle performance of battery.Conduction of the carbon material because being used as lithium ion secondary battery anode material always with good electric conductivity
The electric conductivity of anode not only can be improved using carbon/sulphur composite material as lithium-sulphur cell positive electrode in agent, can also inhibit and vulcanize
" the shuttle effect " that object is formed.
Due to sodium element and the same main group of elemental lithium, chemical property is similar, therefore sodium is directly used in lithium-ion electric by researcher
Sodium-ion battery has been obtained in pond body system.Sodium-ion battery has 3 outstanding advantages: (1) raw material resources compared with lithium ion battery
It is abundant, it is low in cost, it is widely distributed；(2) half-cell potential of sodium-ion battery 0.3 ~ 0.4V high compared with lithium ion potential, Ji Nengli
With the lower electrolyte solvent of decomposition potential and electrolytic salt, the range of choice of electrolyte is wider；(3) sode cell has relatively stable
Chemical property, use is safer.At the same time, there is also defects for sodium-ion battery, such as the relative atom of sodium element
Quality is more much higher than lithium, causes theoretical specific capacity small, and the 1/2 of insufficient lithium；Sodium ion radius ratio lithium ion radius is big by 70%, so that
Sodium ion is embedded in battery material to be more difficult with abjection.In sodium-ion battery, since the structural controllability of carbon material can be
The insertion and abjection of sodium ion provide place.
Shiny-leaved yellowhorn (Classification system Xanthocerassorbifolia Bunge), also known as wood of shiny-leaved yellowhorn, Wen Guanguo, building melon,
Pawpaw, Wen Dange, belong to Sapindaceae, machaka or dungarunga plant, are a kind of distinctive edible oil materials tree species in China.Point
It is distributed in the ground such as northeast and North China and Shaanxi, Gansu, Ningxia, Anhui, Henan.Shiny-leaved yellowhorn is adaptable, careless sand ground, black fallow,
Mountain area, loess hill and gully of more stones etc., or even can normal growth and development on the side of precipice.The seed of shiny-leaved yellowhorn can be used
Next life generation diesel oil, and its shell is not effectively utilized as waste.Contain fatty acid, steroid in shinyleaf yellowhorn fruit shell
A variety of chemical components such as alcohol, saponin(e can be used for extracting furfural, manufacture absorbent charcoal material preferably.It therefore, is original with shinyleaf yellowhorn shell
Porous biomass porous carbon material made from material is cheap and easy to get, has important practical significance.
Summary of the invention
It is an object of the invention to provide a kind of preparation methods of the biomass carbon/sulphur carbon composite；
It is another object of the present invention to be used for lithium sulfur battery anode material and sodium-ion battery to biomass carbon/sulphur carbon composite
The performance of negative electrode material is studied.
One, biomass carbon/sulphur composite material preparation
1, the preparation of multiporous biological matter carbon material
(1) be by shinyleaf yellowhorn shell through 60 ~ 180 DEG C of dryings, dehydration 12 ~ 48 hours after crush, add the pore-creating of 0.5 ~ 4 times of its quality
Agent is uniformly mixed, and under inert gas atmosphere, 2 ~ 16 h of carbonization treatment at 600 ~ 1100 DEG C, products therefrom removes impurity elimination through pickling
Matter filters, cleaning, dry to get multiporous biological matter carbon material.
Pore creating material is using zinc chloride, potassium hydroxide etc.；Acid solution is the hydrochloric acid solution or sulfuric acid solution of 1 ~ 6M.
(2) preparation of biomass carbon/sulphur composite material is by biomass carbon material and sublimed sulfur with the mass ratio of 1:1.5 ~ 1:4
After ground and mixed is uniform, prior to 150 ~ 180 DEG C 10 ~ 24 h of heat treatment diffuse into sulphur in the hole of carbon, are cooled to room temperature progress
Grinding then with 0.5 ~ 2h of toluene agitator treating to remove sulphur remained on surface, then is centrifuged with dehydrated alcohol and washes away toluene, finally
In 60 ~ 80 DEG C of dry 10 ~ 12h to get biomass carbon/sulphur composite material.
Fig. 1 is the X-ray diffractogram (XRD) of biomass porous carbon material prepared by the present invention.It prepares as seen from Figure 1
Biomass carbon material crystalline structure, if figure at 23.6 ° and 43.7 ° there are two wide diffraction maximum, this is amorphous respectively
(002) crystal face of carbon and the diffraction maximum of (100) crystal face, show accurately to be prepared for biomass carbon material.
Fig. 2 is electric field emission scanning electron microscope (SEM) figure of biomass porous carbon material prepared by the present invention.The figure
It has been shown that, micron order biomass carbon material granule show apparent porous form during pore creating material is activated and is carbonized.
Fig. 3 is biomass carbon prepared by the present invention/sulphur composite material electric field emission scanning electron microscope (SEM) figure.
The figure shows that micron order biomass carbon material surface becomes relative smooth and without apparent sulfur granules, and it is successful to show sulphur
It enters inside carbon pores road and is uniformly dispersed.
Two, biomass carbon/sulphur composite material Electrochemical Characterization
Test method: being assembled into button cell for carbon/sulphur composite material, and constant current charge-discharge survey is carried out on blue electric tester
Examination, current density are 200mA g-1With 50 mA g-1。
Fig. 3 is biomass carbon prepared by the present invention/sulphur composite material electrochemical property test figure.Fig. 3 is shown, for the first time may be used
Inverse specific capacity is 943 mAh g-1, coulombic efficiency, which is enclosed, from second substantially remains in 100% or so, later reversible of 200 circulations
Capacity is 371 mAh g-1, capacity retention rate is 37.8%.The composite material has good cyclical stability, is conducive to limit
The shuttle effect and electronics transfer of polysulfide, show excellent electrochemistry in cyclic process when being accordingly used in lithium-sulfur cell
Performance.
Fig. 4 is the electrochemical property test figure of multiporous biological matter carbon prepared by the present invention.Fig. 4 shows, for the first time reversible specific volume
Amount is 305 mAh g-1, coulombic efficiency 65.9% for the first time, coulombic efficiency reaches 100% or so after the 5th circulation, after 100 circulations
Reversible capacity is 152.3 mAh g-1, sodium-ion battery cathode negative electrode material can be used as.
In conclusion the present invention is using shinyleaf yellowhorn shell as raw material, pore-creating and in the presence of by carbonization porous carbon has been made
Material, then by biomass carbon material and sublimed sulfur with certain ratio ground and mixed it is uniform after, expand sulphur by being heat-treated heating melting
It dissipates into the hole of carbon, it is then uniform by ground and mixed, it is finally washed to remove extra sulphur, it is multiple that biomass carbon/sulphur is made
Condensation material.Since sulphur is filled into porous carbon material, porous carbon not only pass through introduce high conductivity carbon and it is shorter from
Son and electron channel substantially increase the electron conduction of sulphur anode, and due to porous structure, vulcanize the centre of dissolution mostly
Object is fixed, and adapts to volume change of the sulphur in charge/discharge process, therefore as lithium sulfur battery anode material and sodium ion
Cell negative electrode material has good chemical property and cyclical stability.
Detailed description of the invention
The XRD diagram of Fig. 1 biomass carbon material prepared by the present invention.
Fig. 2 is that the SEM of biomass carbon material prepared by the present invention schemes.
Fig. 3 is biomass carbon prepared by the present invention/sulphur composite material SEM figure.
Fig. 4 is biomass carbon prepared by the present invention/sulphur composite material electrochemical property test figure.
Fig. 5 is the electrochemical property test figure of biomass carbon material prepared by the present invention.
Specific embodiment
Biomass carbon of the present invention/sulphur composite material preparation method, structure and performance are made below by specific embodiment
Further instruction.
Embodiment 1
Shinyleaf yellowhorn shell is cleaned, is pulverized into powder after drying and dehydrating 12 ~ 48 hours through 60 ~ 180 DEG C spare.Weigh 2 g texts hat
Shell powder, 6g zinc chloride are contained in porcelain Noah's ark after grinding uniformly after mixing the two, with N in tube furnace2900 DEG C of protection
Calcine 2 h；The sample carbonized taking-up is put into beaker, 50 mL, 2 M HCl solution is added to be stirred overnight removal of impurities, then with steaming
Distilled water filters sufficiently washing, then with being dried overnight after ethanol washing one time at 80 DEG C to get to multiporous biological matter carbon material；
Weigh 0.1 g multiporous biological matter carbon material and 60% sublimed sulfur ground and mixed it is uniform after, make sulphur in 155 DEG C of 12 h of heat treatment
Into in the hole of carbon；Then it is cooled to room temperature and is ground, 4 mL toluene stirring, 0.5 h is then added and removes extra sulphur,
It is centrifuged with dehydrated alcohol after washing away toluene and is dried overnight at 80 DEG C to get biomass carbon/sulphur composite material again.
Biomass carbon material is assembled into button cell, constant current charge-discharge test is carried out on blue electric tester, electric current is close
Degree is 50 mA g-1.The results show that reversible specific capacity is 305 mAh g for the first time-1, coulombic efficiency 65.9%, the 5th recycle for the first time
Coulombic efficiency reaches 100% or so afterwards, and reversible capacity is 152.3 mAh g after 100 circulations-1(Fig. 4).
Sulphur/carbon composite is assembled into button cell, constant current charge-discharge test, electric current are carried out on blue electric tester
Density is 200mA g-1.Reversible specific capacity is 1148 mAh g for the first time-1, reversible specific volume after bad activation process is followed by 100 times
Amount is still up to 344.5 mAh g-1.(Fig. 5)
Embodiment 2
Shinyleaf yellowhorn shell is cleaned, is pulverized into powder after drying and dehydrating 12 ~ 48 hours through 60 ~ 180 DEG C spare.Weigh 2 g texts hat
Shell powder, 4 g zinc chloride grind uniformly after mixing, then contain in porcelain Noah's ark, with N in tube furnace2800 DEG C are protected to burn 2
h；The sample carbonized taking-up is put into beaker, 50 mL, 2 M sulfuric acid solution is added to be stirred overnight removal of impurities；Then taken out with distilled water
Filter sufficiently washing, then with ethanol washing one time, be then dried overnight at 80 DEG C, multiporous biological matter carbon material can be obtained.
Weigh the biomass porous carbon material of 0.1 g and 60% sublimed sulfur ground and mixed it is uniform after, in 155 DEG C of 12 h of heat treatment
Enter sulphur in the hole of carbon；It is cooled to room temperature and is ground, 4 mL toluene stirring, 0.5 h is then added and removes extra sulphur,
Toluene is washed away with dehydrated alcohol centrifugation again, is then dried overnight at 80 DEG C to get biomass carbon/sulphur composite material.
Multiporous biological matter carbon material is assembled into button cell, constant current charge-discharge test is carried out on blue electric tester, electricity
Current density is 50 mA g-1.The results show that reversible specific capacity is 286 mAh g for the first time-1, 100 times circulation after reversible capacity be
124mAh g-1。
Sulphur/carbon composite is assembled into button cell, constant current charge-discharge test, electric current are carried out on blue electric tester
Density is 200mA g-1.Reversible specific capacity is 898.4mAh g for the first time-1, reversible specific volume after bad activation process is followed by 200 times
Amount is still up to 414.2mAh g-1, coulombic efficiency 100%.
Embodiment 3
Shinyleaf yellowhorn shell is cleaned, is pulverized into powder after drying and dehydrating 12 ~ 48 hours through 60 ~ 180 DEG C spare.Weigh 2 g texts hat
Shell powder, 2 g potassium hydroxide grind uniformly after mixing, then contain in porcelain Noah's ark, with N in tube furnace2700 DEG C of protection
Burn 2 h；The sample carbonized taking-up is put into beaker, 50 mL, 2 M sulfuric acid solution is added to be stirred overnight removal of impurities；Then with distillation
Water filters sufficiently washing, then with after ethanol washing one time, 80 DEG C are dried overnight to get multiporous biological matter carbon material.
Weigh 0.1 g biomass carbon material and 60% sublimed sulfur ground and mixed it is uniform after, make sulphur in 155 DEG C of 12 h of heat treatment
Into in the hole of carbon；It is cooled to room temperature and is ground, 4 mL toluene stirring, 0.5 h is then added and removes extra sulphur, then uses
Dehydrated alcohol centrifugation washes away toluene, is then dried overnight at 80 DEG C to get biomass carbon/sulphur composite material.
Multiporous biological matter carbon material is assembled into button cell, constant current charge-discharge test is carried out on blue electric tester, electricity
Current density is 50 mA g-1.The results show that reversible specific capacity is 270mAh g for the first time-1, 200 times circulation after reversible capacity be
110mAh g-1, coulombic efficiency 100%.
Sulphur/carbon composite is assembled into button cell, constant current charge-discharge test, electric current are carried out on blue electric tester
Density is 200mA g-1.Reversible specific capacity is 383.9 mAh g for the first time-1, reversible ratio after bad activation process is followed by 200 times
Capacity is still up to 301 mAh g-1, coulombic efficiency 100%.
Claims (6)
1. a kind of biomass carbon/sulphur composite material preparation method, comprising the following steps:
(1) preparation of multiporous biological matter carbon material: shinyleaf yellowhorn shell is crushed after dehydrating, and adds 0.5 ~ 4 times of its quality
Pore creating material is uniformly mixed, then under inert gas atmosphere, 2 ~ 16 h of carbonization treatment, products therefrom are removed through pickling at 600 ~ 1100 DEG C
Decontamination filters, cleaning, dry to get multiporous biological matter carbon material；
(2) biomass carbon/sulphur composite material preparation: by multiporous biological matter carbon material and sublimed sulfur with the quality of 1:1.5 ~ 1:4
After more uniform than ground and mixed, prior to 150 ~ 180 DEG C 10 ~ 24 h of heat treatment diffuse into sulphur in the hole of carbon；Be cooled to room temperature into
Row grinding then with 0.5 ~ 2h of toluene agitator treating to remove sulphur remained on surface, then is centrifuged with dehydrated alcohol and washes away toluene, most
Afterwards in 60 ~ 80 DEG C of dry 10 ~ 12h to get biomass carbon/sulphur composite material.
2. a kind of preparation method of biomass carbon/sulphur composite material as described in claim 1, it is characterised in that: dehydration and drying is
It is handled 12 ~ 48 hours at 60 ~ 180 DEG C.
3. a kind of preparation method of biomass carbon/sulphur composite material as described in claim 1, it is characterised in that: pore creating material uses
Zinc chloride, potassium hydroxide.
4. a kind of preparation method of biomass carbon/sulphur composite material as described in claim 1, it is characterised in that: the acid solution is 1
The hydrochloric acid solution or sulfuric acid solution of ~ 6M.
5. biomass carbon/application of the sulphur composite material as lithium sulfur battery anode material of method preparation as described in claim 1.
6. biomass carbon/sulphur composite material of method preparation as described in claim 1 is answered as anode material of lithium-ion battery
With.
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Cited By (7)
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| CN111370671A (en) * | 2020-03-20 | 2020-07-03 | 东莞东阳光科研发有限公司 | Preparation method of lithium-sulfur battery positive electrode material |
| CN112875675A (en) * | 2021-01-08 | 2021-06-01 | 杭州昶辰科技有限公司 | Preparation and application of biomass porous carbon microsphere-based positive electrode active material |
| CN114583146A (en) * | 2022-05-06 | 2022-06-03 | 湖南大学 | Preparation method of sodium-sulfur battery positive electrode material |
| CN114628683A (en) * | 2022-03-25 | 2022-06-14 | 浙江大学 | Biological carbon/(CuNiCo) for lithium-sulfur battery3P composite material and preparation method thereof |
| CN115893371A (en) * | 2022-12-28 | 2023-04-04 | 蜂巢能源科技(马鞍山)有限公司 | Sulfur, nitrogen and phosphorus doped porous carbon material and preparation and application thereof |
| CN116239098A (en) * | 2023-01-11 | 2023-06-09 | 上海屹锂新能源科技有限公司 | Preparation method of vulcanized porous carbon positive electrode active material |
| CN115893371B (en) * | 2022-12-28 | 2024-07-05 | 蜂巢能源科技(马鞍山)有限公司 | Sulfur, nitrogen and phosphorus doped porous carbon material and preparation and application thereof |
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| CN114628683B (en) * | 2022-03-25 | 2024-04-05 | 浙江大学 | biochar/(CuNiCo) for lithium-sulfur battery 3 P composite material and preparation method thereof |
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| CN115893371A (en) * | 2022-12-28 | 2023-04-04 | 蜂巢能源科技(马鞍山)有限公司 | Sulfur, nitrogen and phosphorus doped porous carbon material and preparation and application thereof |
| CN115893371B (en) * | 2022-12-28 | 2024-07-05 | 蜂巢能源科技(马鞍山)有限公司 | Sulfur, nitrogen and phosphorus doped porous carbon material and preparation and application thereof |
| CN116239098A (en) * | 2023-01-11 | 2023-06-09 | 上海屹锂新能源科技有限公司 | Preparation method of vulcanized porous carbon positive electrode active material |
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