CN105870412A - Preparation method for poplar catkin based biomass carbon/sulfur composite material - Google Patents
Preparation method for poplar catkin based biomass carbon/sulfur composite material Download PDFInfo
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- CN105870412A CN105870412A CN201610239326.9A CN201610239326A CN105870412A CN 105870412 A CN105870412 A CN 105870412A CN 201610239326 A CN201610239326 A CN 201610239326A CN 105870412 A CN105870412 A CN 105870412A
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
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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
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- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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Abstract
The invention discloses a preparation method for a poplar catkin based biomass carbon/sulfur composite material. The preparation method comprises the following steps of (1) enabling pre-processed poplar catkin to be immersed in a potassium hydroxide solution to be stirred for 3-12h, and then drying the obtained material in a drying oven; (2) carrying out high-temperature thermal processing on dried alkalized poplar catkin in a tubular furnace at a temperature of 600-900 DEG C for 1-3h, then washing the processed poplar catkin by a diluted hydrochloric acid solution and water alternately until the poplar catkin is neutral; and next, drying the poplar catkin in the drying oven to obtain carbon micron tube powder; and (3) enabling the carbon micron tube powder to be fully mixed with elementary sulfur and then to be subjected to thermal processing in the tubular furnace to finally obtain the poplar catkin based biomass carbon/sulfur composite material. According to the preparation method, only the simple potassium hydroxide activation method and the thermal processing method are adopted, so that simple process and the commercialized operation can be realized; and meanwhile, the poplar catkin based biomass carbon/sulfur composite material is quite high in electrochemical property, and the initial discharge capacity of the composite material can reach 1200 mAh/g under the current density of 0.1C.
Description
Technical field
The present invention relates to the preparation method of a kind of biomass carbon/sulfur composite being applied to lithium-sulfur cell, just belong to lithium ion battery
Pole Material Field.
Background technology
At present lithium ion battery has a wide range of applications in the work, life of people, such as at mobile phone, digital camera and
The portable type electronic products such as notebook computer and the aspect such as electric automobile, extensive energy storage device occupy critical role.Along with people
To equipment performance require raising, conventional lithium ion battery can not meet demand, therefore height ratio capacity, high security, height
The lithium ion battery of future generation of service life and low cost becomes the focus of people's research.
The positive pole of lithium ion battery is the key improving battery specific capacity.Elemental sulfur does the theoretical energy density of the lithium-sulfur cell of positive pole
For 2600Wh/Kg, specific capacity is up to 1675mAh/g, is the most commercial transition metal oxide positive pole theoretical specific capacity and ratio
Ten times of energy, and sulfur rich content, cheap, environmentally friendly in nature, be the electrification of great application prospect
Learn energy storage system, be widely studied in recent years.But elemental sulfur still has many shortcomings to govern lithium/sulfur battery as positive electrode
Commercial applications: one is that the electrical insulating property of elemental sulfur causes the utilization rate of active matter low；Two is intermediate product Li2Sx(2≤x≤8)
Dissolve in the electrolytic solution, make electrolyte viscosity increase, ion diffusion hindered, and the distribution change that active substance is in the electrodes
Change very big, agglomeration repeatedly occurs after circulation, departs from conductive agent, gradually lose reactivity.These impacts directly result in
The specific discharge capacity of lithium-sulfur cell is significantly decayed after initial circulation several times.
For the problems referred to above, research worker is improving the electric conductivity of sulfur, is improving the aspects such as battery cycle life and carried out extensive work,
Different methods is used to improve the problem of lithium-sulfur cell cyclicity difference, for example with carbon such as CNT, Graphene, mesoporous carbon
Material storage sulfur, is limited in sulfur in the duct of material with carbon element or utilizes the specific surface area that material with carbon element is high to limit the dissolving of polysulfide.
But, above-mentioned material with carbon element cost intensive, complex process, it is unsuitable for production and the application of large-scale commercial.Biomass carbon material
Material is by including that timber, forest garbage, agricultural wastes, water plant, city and industrial organic wastes etc. process
A kind of porous carbon.Biomass carbon material with the thermostability of its uniqueness, high-termal conductivity, high conductivity, and natural fiber is poroid
Structure all makes it show potential researching value in lithium-sulfur cell.The compound electric conductivity that not only can improve positive pole of sulfur/carbon, also may be used
With the volumetric expansion of active substance in the suppression polysulfide ion diffusion to negative pole and charge and discharge process.Such as CN 104681800 A
Report the preparation method of a kind of biomass carbon/sulfur composite, corn straw carbon dust KOH is activated, obtains biological carbon
Material；The biological carbon material HCL solution obtained and water are cleaned to pH value be 7；The biomass carbon material dipping that will obtain
In the particular solution of sulfur, it is dried to obtain biological carbon/sulfur composite.But biological carbon prepared by above-mentioned technology/sulfur composite
Chemical property is unsatisfactory, and this is that the material with carbon element prepared due to it carries out mechanical mixture with sulfur, little to the adsorptivity of sulfur, lithium
Sulfur battery capacity is low, decay is fast.Therefore, in preparing biomass carbon/sulfur composite, sulfur is dispersed in biomass carbon material
It material is the key improving lithium-sulfur cell chemical property.In the present invention, for the deficiency in traditional handicraft and problem, poplar is wadded a quilt with cotton
The activated carbon prepared fully mixes with sulfur, and uses heat-treating methods to be filled in the material with carbon element of porous by sulfur, to realize
In biomass carbon/sulfur composite, sulfur is dispersed, thus inhibits the dissolving of polysulfide, improves the capacity of lithium-sulfur cell.
Summary of the invention
The technical problem to be solved is: in lithium-sulfur cell, sulfur is non-conductive, and polysulfide is soluble in electrolyte etc.
Not enough, it is provided that the preparation method of a kind of biomass carbon/sulfur composite based on poplar wadding.The method utilizes the side of activation and heat treatment
Method is prepared the porous carbon with good cavernous structure by biological material, is then sufficiently mixed with sulfur, through to sulfur/carbon mix
Simple thermal treatment, by control heat treatment temperature, prepare biomass carbon/sulfur composite.The present invention makes sulfur really real
It is scattered in the hole of biomass carbon the most uniformly, thus improves the capacity of lithium-sulfur cell.
The technical scheme is that
The preparation method of a kind of biomass carbon/sulfur composite based on poplar wadding, comprises the steps:
(1) the poplar wadding through pretreatment being immersed stirring 3h-12h in potassium hydroxide solution, then solution is through being evaporated in vacuo, being dried,
Obtain the poplar wadding that alkalizes；Wherein, mass ratio is the poplar wadding through pretreatment: contained KOH=1:1～5 in solution；
(2) alkalization poplar is wadded a quilt with cotton in tube furnace, obtain poplar wadding powder after processing 1-3h at 600-900 DEG C, then use dilute hydrochloric acid solution
Alternately washed to neutral with water, be then put in drying baker and be dried, obtain carbon micron tube powder；
(3) carbon micron tube powder is added to the water, adds sulfur simple substance, ultrasonic disperse 2～5 hours, after drying, 150-300 DEG C
Lower insulation 3-5h, finally obtains biomass carbon/sulfur composite based on poplar wadding；Wherein, mass ratio is carbon micron tube powder: sulfur
Simple substance=1:1～1:3；
The concentration range of described potassium hydroxide solution is 0.5～2mol/L.
The poplar wadding of pretreatment in described step (1) refers to wad a quilt with cotton the poplar of collection wash, and is then dried.
The preparation method of above-mentioned biomass carbon/sulfur composite, wherein involved raw material is all obtained by open channel or be purchased
Obtaining (wherein poplar wadding is to gather and obtain), equipment used and technique are all known to those skilled in the art.
The invention have the benefit that
(1), in design process of the present invention, these pollutant of being wadded a quilt with cotton by poplar first are prepared as biomass carbon material and are sufficiently mixed use with sulfur
In lithium-sulfur cell, and effectively utilizing poplar wadding, with low cost, raw material selection is innovated.And the fibre structure that poplar wadding is natural,
It is beneficial to the attachment of sulfur, and energy density is high.
(2), design process of the present invention, only with simple activation of potassium hydroxide and heat-treating methods, technique is simple, is suitable for business
Industryization operates, and by the control to its heat treatment temperature, can prepare the biomass carbon with good cavernous structure, thus have
Imitate improves sulfur being uniformly distributed in material with carbon element, therefore can increase substantially the chemical property of lithium-sulfur cell.
(3), compared with prior art CN 104681800 A, elemental sulfur is limited in the hole of material with carbon element by the present invention in the design process
In road, the specific surface area that material with carbon element is high is utilized to limit the dissolving of many lithium sulfides.In heating process, sulfur distillation is diffused to biomass
In the hole of carbon, due to the high-specific surface area of biomass carbon, elemental sulfur has been left in the hole of material with carbon element during cooling,
The pore surface of material with carbon element is coated with by sulfur uniformly, ultimately generates biomass carbon/sulfur composite.The biology of preparation in the present invention
Not having obvious sulfur granules in matter carbon/sulfur composite, sulfur distribution is uniform, and the size of sulfur is up to nanoscale, overcomes tradition work
In skill, sulfur is oversize in material with carbon element, or skewness even cannot realize the problems such as real sulfur cladding.With traditional handicraft system
Standby sulfur/carbon composite is compared, and biomass carbon prepared by this technique/sulfur composite material exhibits goes out good chemical property, its
Discharge capacity first under electric current density is 0.1C reaches 1200mAh/g.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of sulfur, biomass carbon, biomass carbon/sulfur composite；
Fig. 2 is the thermogravimetric curve figure of biomass carbon/sulfur composite that embodiment 1 obtains；
Fig. 3 is that biomass carbon/sulfur composite of obtaining of embodiment 1 is as the discharge and recharge under 0.1C multiplying power during lithium ion cell positive
Curve chart.
Detailed description of the invention
Embodiment 1
(1) collect a certain amount of poplar wadding, the poplar wadding deionized water collected is washed 12 times, is then placed in drying baker
90 degree are dried 12h, obtain the poplar through pretreatment and wad a quilt with cotton；
(2) will be sufficiently stirred for 3h in the poplar wadding immersion 1mol/L potassium hydroxide solution of pretreatment, wherein, mass ratio is warp
The poplar crossing pretreatment is wadded a quilt with cotton: contained KOH=1:2 in solution, then by obtained material in vacuum condition transpiring moisture, afterwards
In drying baker the driest, at baking temperature 70 DEG C be dried 12h；
(3) dry alkalization poplar is wadded a quilt with cotton in tube furnace, it is heated to 700 DEG C of insulations with the heating rate of 5 DEG C/min under an inert atmosphere
1h, carries out high-temperature heat treatment, obtains poplar wadding powder；
(4) dilute hydrochloric acid solution and the water alternately washing of the poplar wadding powder 0.1mol/L after heat treatment, to neutral, are then put
In drying baker, 90 DEG C of 12h the driest obtain carbon micron tube powder；
(5) dry carbon micron tube powder 2g is dissolved in 100ml water, ultrasonic disperse, then mixes with elemental sulfur, ultrasonic
3h is to ensure that carbon micron tube powder is sufficiently mixed with sulfur, and wherein, mass ratio is carbon micron tube powder: sulfur=1:2；
(6) mixed solution obtained in (5) is placed in drying baker the driest, at 60 DEG C, is dried 12h；
(7) being mixed thing and carry out heat treatment in tube furnace, temperature is 150 DEG C, 2.5 DEG C/min of heating rate, is incubated 3h,
Finally give biomass carbon/sulfur composite.
(8) biomass carbon/sulfur composite that the present embodiment is prepared and conductive agent Super P and binding agent Kynoar
(PVDF) it is fully ground mixing with mass ratio 8:1:1, then instills N-methyl pyrrolidinone solvent and be ground to pulpous state, and all
Even it is coated in aluminum foil current collector, at 60 DEG C, is dried 12h, re-uses tablet machine and depress to thin slice at 5MPa pressure, thus make
Obtain biomass carbon/sulfur based lithium-ion battery positive plate；Positive plate and metal lithium sheet are assembled CR2025 in the glove box of full argon
Button cell.
Fig. 1 is X-ray diffraction (XRD) figure of the biomass carbon obtained by sulfur, the present embodiment and biomass carbon/sulfur composite.
The biomass carbon of X-ray diffractogram explanation preparation is amorphous state.In the X-ray diffractogram of biomass carbon/sulfur composite the brightest
The characteristic diffraction peak of aobvious sulfur, illustrates to achieve being uniformly distributed of sulfur in the composite.
Fig. 2 is the thermogravimetric curve figure of biomass carbon/sulfur composite that the present embodiment obtains, it can be seen from the graph that biomass carbon/sulfur is multiple
In condensation material, the content of sulfur is about 44%.
Prepared sample is carried out chemical property analysis (BTS-5V5mA, new prestige).Fig. 3 is the biology that the present embodiment obtains
Matter carbon/sulfur composite is as the charging and discharging curve figure of lithium ion cell positive, it may be seen that biomass carbon/sulfur composite exists
Electric current density is that the discharge capacity first under 0.1C is up to 1200mAh/g.
Embodiment 2
(1) collect a certain amount of poplar wadding, the poplar wadding deionized water collected is washed 15 times, is then placed in drying baker
60 degree are dried 12h, obtain the poplar through pretreatment and wad a quilt with cotton；
(2) will wad a quilt with cotton to immerse in 1mol/L potassium hydroxide solution through the poplar of pretreatment and be sufficiently stirred for 5h, wherein, mass ratio is
Wad a quilt with cotton to the poplar through pretreatment: contained KOH=1:3 in solution, then by obtained material in vacuum condition transpiring moisture,
The driest in drying baker afterwards, it is dried 12h at baking temperature 90 DEG C；
(3) dry alkalization poplar is wadded a quilt with cotton in tube furnace, it is heated to 900 DEG C of insulations with the heating rate of 5 DEG C/min under an inert atmosphere
1.5h, carries out high-temperature heat treatment, obtains poplar wadding powder；
(4) dilute hydrochloric acid solution and the water alternately washing of the poplar wadding powder 0.5mol/L after heat treatment, to neutral, are then put
In drying baker, 90 DEG C of 12h the driest obtain carbon micron tube powder；
(5) dry carbon micron tube powder 2.5g is dissolved in 100ml water, ultrasonic disperse, then mixes with elemental sulfur, ultrasonic
5h is to ensure that carbon micron tube powder is sufficiently mixed with sulfur, and wherein, mass ratio is carbon micron tube powder: sulfur=1:3；
(6) mixed solution obtained in (5) is placed in drying baker the driest, at 60 DEG C, is dried 12h；
(7) being mixed thing and carry out heat treatment in tube furnace, temperature is 300 DEG C, 5 DEG C/min of heating rate, is incubated 5h,
Finally give biomass carbon/sulfur composite.
(8) biomass carbon/sulfur composite that the present embodiment is prepared and conductive agent Super P and binding agent Kynoar
(PVDF) it is fully ground mixing with mass ratio 8:1:1, then instills N-methyl pyrrolidinone solvent and be ground to pulpous state, and all
Even it is coated in aluminum foil current collector, at 60 DEG C, is dried 12h, re-uses tablet machine and depress to thin slice at 5MPa pressure, thus make
Obtain biomass carbon/sulfur based lithium-ion battery positive plate；Positive plate and metal lithium sheet are assembled CR2025 in the glove box of full argon
Button cell.
When the biomass carbon that the present embodiment obtains/sulfur composite is as lithium ion cell positive, under electric current density is 0.1C,
Discharge capacity is 1153mAh/g first.
Unaccomplished matter of the present invention is known technology.
Claims (3)
1. a preparation method for biomass carbon/sulfur composite based on poplar wadding, is characterized by comprise the steps:
(1) immersing in potassium hydroxide solution by the poplar wadding of pretreatment, stir 3h-12h, then solution is through being evaporated in vacuo, being dried, and obtains alkalization poplar wadding；Wherein, mass ratio is the poplar wadding through pretreatment: contained KOH=1:1 ~ 5 in solution；
(2) dry alkalization poplar wadding is placed in tube furnace, obtains poplar wadding powder after processing 1-3h at 600-900 DEG C, more alternately washed to neutral with dilute hydrochloric acid solution and water, be then put in drying baker and be dried, obtain carbon micron tube powder；
(3) carbon micron tube powder is added to the water, adds sulfur simple substance, ultrasonic disperse 2 ~ 5 hours, after drying, at 150-300 DEG C, be incubated 3-5h, finally obtain biomass carbon/sulfur composite based on poplar wadding；Wherein, mass ratio is carbon micron tube powder: sulfur simple substance=1:1 ~ 1:3.
2. the preparation method of the biomass carbon/sulfur composite wadded a quilt with cotton based on poplar as claimed in claim 1, is characterized by that the concentration range of described potassium hydroxide solution is 0.5 ~ 2 mol/L.
3. the preparation method of the biomass carbon/sulfur composite wadded a quilt with cotton based on poplar as claimed in claim 1, is characterized by that the poplar wadding of pretreatment in described step (1) referring to wad a quilt with cotton the poplar of collection wash, is then dried.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106532012A (en) * | 2016-12-23 | 2017-03-22 | 浙江大学 | Sulfur-biomass carbon/transition metal composite electrode material and preparation method and application thereof |
| CN106898746A (en) * | 2017-03-14 | 2017-06-27 | 天津大学 | Hierarchical porous structure nano-sized carbon/sulphur composite and the application in lithium-sulfur cell are prepared by raw material of Hawaii shell |
| CN107565116A (en) * | 2017-08-31 | 2018-01-09 | 陕西科技大学 | A kind of preparation method of integrated lithium sulfur battery anode material |
| CN107746050A (en) * | 2017-10-17 | 2018-03-02 | 天津工业大学 | A kind of preparation method of carbon pipe |
| CN108232176A (en) * | 2018-02-07 | 2018-06-29 | 中南大学 | A kind of lithium-sulfur cell cathode material and preparation method thereof |
| CN108417806A (en) * | 2018-03-19 | 2018-08-17 | 河南师范大学 | A kind of universality preparation method of lithium-sulfur cell sulphur/carbon composite anode material |
| CN108736012A (en) * | 2018-04-23 | 2018-11-02 | 江汉大学 | A kind of biomass micro-pipe and carbon nano-tube hybridization carbon material and preparation method thereof |
| CN109273272A (en) * | 2018-09-03 | 2019-01-25 | 南京师范大学 | The preparation method and its sulfur doping carbon micron tube of a kind of sulfur doping carbon micron tube and application |
| CN109285993A (en) * | 2017-07-19 | 2019-01-29 | 中国科学院过程工程研究所 | A kind of sulphur carbon flexible electrode material and its preparation method and application |
| CN109360970A (en) * | 2018-11-20 | 2019-02-19 | 肇庆市华师大光电产业研究院 | A kind of lithium sulphur one-shot battery positive electrode and preparation method thereof |
| CN110660968A (en) * | 2019-09-17 | 2020-01-07 | 天津大学 | Composite lithium metal negative electrode and preparation method thereof |
| CN113039623A (en) * | 2018-09-14 | 2021-06-25 | 新罗纳米技术有限公司 | Battery electrode compositions comprising biomass-derived carbon |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106532012A (en) * | 2016-12-23 | 2017-03-22 | 浙江大学 | Sulfur-biomass carbon/transition metal composite electrode material and preparation method and application thereof |
| CN106898746A (en) * | 2017-03-14 | 2017-06-27 | 天津大学 | Hierarchical porous structure nano-sized carbon/sulphur composite and the application in lithium-sulfur cell are prepared by raw material of Hawaii shell |
| CN109285993A (en) * | 2017-07-19 | 2019-01-29 | 中国科学院过程工程研究所 | A kind of sulphur carbon flexible electrode material and its preparation method and application |
| CN107565116A (en) * | 2017-08-31 | 2018-01-09 | 陕西科技大学 | A kind of preparation method of integrated lithium sulfur battery anode material |
| CN107746050A (en) * | 2017-10-17 | 2018-03-02 | 天津工业大学 | A kind of preparation method of carbon pipe |
| CN108232176A (en) * | 2018-02-07 | 2018-06-29 | 中南大学 | A kind of lithium-sulfur cell cathode material and preparation method thereof |
| CN108232176B (en) * | 2018-02-07 | 2020-11-13 | 中南大学 | Lithium-sulfur battery cathode material and preparation method thereof |
| CN108417806A (en) * | 2018-03-19 | 2018-08-17 | 河南师范大学 | A kind of universality preparation method of lithium-sulfur cell sulphur/carbon composite anode material |
| CN108736012A (en) * | 2018-04-23 | 2018-11-02 | 江汉大学 | A kind of biomass micro-pipe and carbon nano-tube hybridization carbon material and preparation method thereof |
| CN109273272A (en) * | 2018-09-03 | 2019-01-25 | 南京师范大学 | The preparation method and its sulfur doping carbon micron tube of a kind of sulfur doping carbon micron tube and application |
| CN109273272B (en) * | 2018-09-03 | 2020-06-16 | 南京师范大学 | Preparation method of sulfur-doped carbon micro-tube, sulfur-doped carbon micro-tube and application of sulfur-doped carbon micro-tube |
| CN113039623A (en) * | 2018-09-14 | 2021-06-25 | 新罗纳米技术有限公司 | Battery electrode compositions comprising biomass-derived carbon |
| US11688855B2 (en) | 2018-09-14 | 2023-06-27 | Sila Nanotechnologies, Inc. | Battery electrode composition comprising biomass-derived carbon |
| CN109360970A (en) * | 2018-11-20 | 2019-02-19 | 肇庆市华师大光电产业研究院 | A kind of lithium sulphur one-shot battery positive electrode and preparation method thereof |
| CN109360970B (en) * | 2018-11-20 | 2022-04-08 | 肇庆市华师大光电产业研究院 | Positive electrode material of lithium-sulfur primary battery and preparation method of positive electrode material |
| CN110660968A (en) * | 2019-09-17 | 2020-01-07 | 天津大学 | Composite lithium metal negative electrode and preparation method thereof |
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