CN109592662A - A kind of preparation method of the biological carbon negative pole material of lithium-sulfur cell - Google Patents
A kind of preparation method of the biological carbon negative pole material of lithium-sulfur cell Download PDFInfo
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- CN109592662A CN109592662A CN201811459446.5A CN201811459446A CN109592662A CN 109592662 A CN109592662 A CN 109592662A CN 201811459446 A CN201811459446 A CN 201811459446A CN 109592662 A CN109592662 A CN 109592662A
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Abstract
A kind of lithium-sulfur cell preparation method of biological carbon negative pole material, kiwi peer is added to the water, neutral filtering is diluted to after concentrated acid reaction then is added thereto, is dried to obtain product C；The concentrated sulfuric acid and water are added in product C, is placed in reaction solution D in hydrothermal reaction kettle, solution D is diluted to neutral filtering, dry product E；By layer overlay electrically conductive graphite uniform on product, heating reaction obtains product F in tube furnace；Product F is rinsed, is filtered, drying obtains product G；Product G is mixed to obtain to mixture H with sulphur powder；Mixture H is placed in temperature reaction in tube furnace and obtains porous biological carbon lithium-sulfur cell negative electrode material.The present invention is using kiwi peer as biomass material, and using first mixed acid pre-soaking, rear hydro-thermal method prepares biological carbon matrix precursor, activation time is controlled in later period activation, regulation obtains being suitable for the biological carbon material for storing up sulphur, is applied to lithium-sulfur cell, promotes its chemical property.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium-sulfur cell negative electrode material, and in particular to a kind of lithium-sulfur cell biological carbon
The preparation method of negative electrode material.
Background technique
The development of portable electronic device is more more and more urgent for the demand of advanced energy storage.Advanced energy resource system it is fast
Fast demand for development material must have low cost, long-life, high safety, high-energy, high-power, advantages of environment protection.Lithium
Sulphur battery can preferably combine These characteristics, in following high-energy (2500Whkg-1) have in storage system compared with
Good application prospect.In the lithium-sulfur cell of high-energy density, the theoretical capacity of sulphur is 1672mAhg-1, lithium an- ode
Theoretical capacity is 3860mAhg-1.In charge and discharge process, lithium ion is generated from metal lithium electrode, is diffused by electrolyte
Sulfur electrode, electronics are flowed from external circuit, and final discharging product Li is generated at cathode2S.However, the technology of lithium-sulfur cell hinders
Hinder and limit its application, for example cycle period is short, the content of sulfur loaded is low.Reason mainly has the following: (1) due in sun
Polysulfide intermediate product is generated in pole and cathode, and complicated the Nomenclature Composition and Structure of Complexes variation is generated during forming polysulfide,
Easily dissolution causes capacitance loss to polysulfide in the electrolytic solution, and the cyclical stability of electrode is poor；(2) sulphur and discharging product Li2S
With ion and electronic isolation, the electric conductivity of material is reduced.(3) polysulfide moves in circles between the anode and the cathode,
The loss of active material is caused, coulombic efficiency is lower, and surface of metal electrode is passivated, and generates insulation product Li2S/Li2S2。
(4) loss of metal lithium electrode is prevented mainly due to the passivation on surface and the formation (SEI film) of unstable solid-liquid interphase
The long-range cyclical stability of lithium-sulfur cell.
In recent years, largely studies have shown that the above problem can be negative by introducing sulphur-carbon, sulphur-polymer composites
The methods of pole, novel battery system, stable lithium an- ode are realized.Result of study specifically includes that (1) introduces new battery composition
Material and structure (cathode, binder, electrolyte and anode).(2) mechanism study of Li-S redox chemistry reaction.(3) exist
Conducting base (such as: carbon, polymer, metal) is introduced in sulfur electrode.This method can promote the electric conductivity of material to a certain degree,
But its energy density can also reduce.Research for novel electrode structure, main includes using sulphur-carbon, sulphur-polymer nanocomposite
Composite material, the storage of porous polysulfide, porous current collector, binder, self-supporting combination electrode, cathode and separator interlayer
Away from, polysulfide cathode, surface covering separator, polysulfide cathode, sandwich cathode construction, lithium metal protection and Li2S is living
Change.Based on the studies above, the development and application of the following lithium-sulfur cell still have extensive prospect.
Summary of the invention:
The purpose of the present invention is to provide a kind of preparation process is simple, raw material is easy to get, the biological carbon material of obtained load sulphur
With environment friendly, and it is able to ascend the preparation method of the biological carbon negative pole material of lithium-sulfur cell of lithium-sulfur cell capacity.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
1) it is dried after taking 2-8g kiwi peer to wash, obtains product A；
2) 100mL water is added in product A, the concentrated acid of 10-60mL is then added thereto, being stirred with glass bar makes it sufficiently
Reaction, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 1-5mL concentrated sulfuric acid is added in product C, 45-49mL water is placed in hydrothermal reaction kettle at 160-180 DEG C, reaction
8-30h obtains solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 5-10 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 0-10h, is obtained
Product F；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G.
8) by product G with sulphur powder with (1-9): the mass ratio of (9-1) mixes, grinding obtain mixture H；
9) mixture H is laid in white alumina porcelain boat, is placed in the tube furnace of argon atmosphere from room temperature with 5-10
DEG C/heating rate of min is warming up to 155-165 DEG C, reaction 12-24h obtains lithium-sulfur cell biology carbon negative pole material.
The step 1), which is adopted, to be washed with distilled water.
The concentrated acid of the step 2) is to be separately added into the concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid with volume ratio 4:3:3.
Step 2) the mixing time is 10-30min.
The step 6,9) argon gas flow velocity are 60-100sccm.
The present invention is using kiwi peer as biomass material, and using first mixed acid pre-soaking, rear hydro-thermal method prepares biological carbon
Predecessor controls activation time in later period activation, and regulation obtains being suitable for the biological carbon material for storing up sulphur, is applied to lithium sulphur electricity
Pond promotes its chemical property.
The beneficial effects of the present invention are embodied in:
1) present invention is using first mixed acid pre-soaking, and the mode of rear hydro-thermal process handles biological carbon matrix precursor, and then at heat
Reason obtains biological carbon material.Biomass exocuticle organic aldehyde, oxidation of ketones are obtained carboxyl structure by acid soak, so hydro-thermal process
Biomass endepidermis is further etched on this basis, and endepidermis lignin from biomass content is higher, thus needs high temperature height
Pressure could homogeneous reaction.
2) synergistic effect of electrically conductive graphite is heat-treated and is added in tube furnace by hydrothermal product to be promoted in the present invention
The electric conductivity of material.Under the protection of inert gas, carboxylic acid molecules, which are decomposed, generates carbon dioxide generation hole, remaining carbon atom
Arrangement recombination forms carbon hexatomic ring, and structure is more orderly, and degree of graphitization is higher.At the same time, hydrothermal product surface is oxygen-containing
Functional group can promote the degree of graphitization and electric conductivity of material entirety with electrically conductive graphite stable bond.
3) in the soaking step of mixed acid of the present invention, the additional proportion and mixing time of mixed acid will affect acid to biomass
The degree of oxidation and etching degree of outer surface, and then influence the structure and post-processing mode of biological carbon in heat treatment process.
4) kiwi peer is a kind of biomass castoff, if it is possible to will be answered with very extensive applied to lithium-sulfur cell
Use prospect.Phenolic substances rich in and actinidine in kiwi peer, are easy to be aoxidized by strong acid and generate hole, and quality compared with
Gently, the specific discharge capacity of prepared electrode is higher.
5) preparation process of the invention is relatively simple, and raw material is easy to get, and the biological carbon material of obtained load sulphur has environment friend
Good property.
6) skeleton of biological carbon of the invention as sulfur loaded, it is suppressed that polysulfide is in the electrolytic solution in charge and discharge process
Dissolution, while carburizing temperature and carrying the control of sulfur content and can change the electric conductivity of carbon material.
Detailed description of the invention
Fig. 1 is the SEM figure of the biological carbon negative pole material of lithium-sulfur cell prepared by the embodiment of the present invention 6.
Specific embodiment
Embodiment 1:
1) take 2g kiwi peer adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 4:3:3
With the total 10mL of concentrated nitric acid, stirring 10min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 1mL concentrated sulfuric acid is added in product C, 49mL water is placed in hydrothermal reaction kettle at 160 DEG C, reacts 30h, obtain
Solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 5 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 10h, obtains product
F, wherein argon gas flow velocity is 60sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 1:9, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 5 DEG C/
The heating rate of min is warming up to 155 DEG C, and reaction 12h obtains the biological carbon negative pole material of lithium-sulfur cell, and wherein argon gas flow velocity is
60sccm。
Embodiment 2:
1) take 8g kiwi peer adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 4:3:3
With the total 60mL of concentrated nitric acid, stirring 10min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 5mL concentrated sulfuric acid is added in product C, 45mL water is placed in hydrothermal reaction kettle at 180 DEG C, and reaction for 24 hours, obtains
Solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 10 DEG C/min from room temperature in the tube furnace of atmosphere and obtains product F, and wherein argon gas flow velocity is
60sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 8:2, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 7 DEG C/
The heating rate of min is warming up to 155 DEG C, and reaction 12h obtains the biological carbon negative pole material of lithium-sulfur cell, and wherein argon gas flow velocity is
100sccm。
Embodiment 3:
1) take 8g kiwi peer adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 4:3:3
With the total 60mL of concentrated nitric acid, stirring 10min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 5mL concentrated sulfuric acid is added in product C, 45mL water is placed in hydrothermal reaction kettle at 180 DEG C, and reaction for 24 hours, obtains
Solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 8 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 2h, obtains product F,
Wherein argon gas flow velocity is 60sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 8:2, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 5 DEG C/
The heating rate of min is warming up to 155 DEG C, and reaction 12h obtains the biological carbon negative pole material of lithium-sulfur cell, and wherein argon gas flow velocity is
100sccm。
Embodiment 4:
1) take 8g kiwi peer adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 4:3:3
With the total 60mL of concentrated nitric acid, stirring 10min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 5mL concentrated sulfuric acid is added in product C, 45mL water is placed in hydrothermal reaction kettle at 180 DEG C, and reaction for 24 hours, obtains
Solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 6 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 5h, obtains product F,
Wherein argon gas flow velocity is 60sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 8:2, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 8 DEG C/
The heating rate of min is warming up to 155 DEG C, and reaction 12h obtains the biological carbon negative pole material of lithium-sulfur cell, and wherein argon gas flow velocity is
100sccm。
Embodiment 5:
1) take 6g kiwi peer adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 4:3:3
With the total 45mL of concentrated nitric acid, stirring 30min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 3mL concentrated sulfuric acid is added in product C, 47mL water is placed in hydrothermal reaction kettle at 160 DEG C, reacts 8h, obtain molten
Liquid D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 10 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 8h, obtains product
F, wherein argon gas flow velocity is 80sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 6:4, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 5 DEG C/
The heating rate of min is warming up to 160 DEG C, and reaction obtains the biological carbon negative pole material of lithium-sulfur cell for 24 hours, and wherein argon gas flow velocity is
100sccm。
Embodiment 6:
1) take 4g kiwi peer adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 4:3:3
With the total 20mL of concentrated nitric acid, stirring 28min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 5mL concentrated sulfuric acid is added in product C, 45mL water is placed in hydrothermal reaction kettle at 170 DEG C, reacts 10h, obtain
Solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 10 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 8h, obtains product
F, wherein argon gas flow velocity is 100sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 9:1, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 10 DEG C/
The heating rate of min is warming up to 165 DEG C, and reaction 20h obtains the biological carbon negative pole material of lithium-sulfur cell, and wherein argon gas flow velocity is
80sccm。
From figure 1 it appears that the proportion and volume of control acid, the degree for the treatment of of kiwi peer is different.The addition of nitric acid
It is stronger compared to adsorptivity of the pure carbon material to sulphur since nitrogen has electronegativity to introduce nitrogen-containing functional group in biological carbon；Dense sulphur
Sour strong oxidizing property is stronger, can be carbonized in advance to kiwi peer, while more oxygen atom is introduced on surface, and oxygen atom electricity is negative
Property is weaker with respect to nitrogen, but still can adsorb sulphur simple substance；Hydrochloric acid is easy to produce escaping gas, easily on kiwi peer surface and
Internal pore-creating, and chlorine atom is introduced on surface.It, can be on kiwi peer surface and interior by the concentration and additional proportion of control acid
Under conditions of portion's pore-creating, introduce a certain amount of nitrogen-atoms, oxygen atom and chlorine atom, due to three atom pair sulphur adsorption capacity not
Together, the ability for storing up sulphur is also different.
Claims (5)
1. a kind of lithium-sulfur cell preparation method of biological carbon negative pole material, it is characterised in that:
1) it is dried after taking 2-8g kiwi peer to wash, obtains product A；
2) 100mL water is added in product A, the concentrated acid of 10-60mL is then added thereto, being stirred with glass bar keeps it sufficiently anti-
It answers, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 1-5mL concentrated sulfuric acid is added in product C, 45-49mL water is placed in hydrothermal reaction kettle at 160-180 DEG C, reacts 8-
30h obtains solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon atmosphere
Tube furnace in from room temperature be warming up to 1000 DEG C with the heating rate of 5-10 DEG C/min, in 1000 DEG C of reaction 0-10h, obtain product
F；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G.
8) by product G with sulphur powder with (1-9): the mass ratio of (9-1) mixes, grinding obtain mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 5-10 DEG C/
The heating rate of min is warming up to 155-165 DEG C, and reaction 12-24h obtains the biological carbon negative pole material of lithium-sulfur cell.
2. the lithium-sulfur cell according to claim 1 preparation method of biological carbon negative pole material, it is characterised in that: the step
Rapid 1) adopt is washed with distilled water.
3. the lithium-sulfur cell according to claim 1 preparation method of biological carbon negative pole material, it is characterised in that: the step
Rapid concentrated acid 2) is to be separately added into the concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid with volume ratio 4:3:3.
4. the lithium-sulfur cell according to claim 1 preparation method of biological carbon negative pole material, it is characterised in that: the step
Rapid 2) mixing time is 10-30min.
5. the lithium-sulfur cell according to claim 1 preparation method of biological carbon negative pole material, it is characterised in that: the step
Rapid 6,9) argon gas flow velocity be 60-100sccm.
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Cited By (2)
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| CN110299537A (en) * | 2019-06-26 | 2019-10-01 | 陕西科技大学 | A kind of preparation process of the biomass porous carbon nano-electrode material of long circulating lithium ion battery sulfur doping |
| CN111554926A (en) * | 2020-05-15 | 2020-08-18 | 陕西科技大学 | Preparation method of wheat straw/carbon nanotube for long-cycle nitrogen-doped lithium battery negative electrode material |
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| KR20180017975A (en) * | 2016-08-12 | 2018-02-21 | 주식회사 엘지화학 | Sulfur-carbon composite and lithium-sulfur battery including the same |
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| CN103515614A (en) * | 2013-10-02 | 2014-01-15 | 中国地质大学（武汉） | Additive for battery, cathode material containing same and preparation method for cathode material |
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| CN106099110A (en) * | 2016-07-11 | 2016-11-09 | 杭州电子科技大学 | A kind of method utilizing algae to prepare Li S cell positive material as carbon source |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110299537A (en) * | 2019-06-26 | 2019-10-01 | 陕西科技大学 | A kind of preparation process of the biomass porous carbon nano-electrode material of long circulating lithium ion battery sulfur doping |
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