CN109755469A - A kind of lithium-sulfur cell lamelliform electrode and its preparation and application - Google Patents
A kind of lithium-sulfur cell lamelliform electrode and its preparation and application Download PDFInfo
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- CN109755469A CN109755469A CN201711095923.XA CN201711095923A CN109755469A CN 109755469 A CN109755469 A CN 109755469A CN 201711095923 A CN201711095923 A CN 201711095923A CN 109755469 A CN109755469 A CN 109755469A
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Abstract
The present invention relates to a kind of lithium-sulfur cell lamelliform porous electrode and its preparations and application, select low-freezing solvent, prepare active material slurry, lamelliform electrode is prepared by freeze-drying；Lamelliform electrode preparation method is simple, environmental friendly, and material structure is stablized, and lamelliform electrode structure is conducive to improve the performance of high load amount Li-S battery.
Description
Technical field
The present invention relates to a kind of lithium-sulfur cell electrode materials.
Background technique
In past 20 years, lithium ion battery is fast-developing, and captures the portable electrics such as battery of mobile phone, mobile power source rapidly
Sub- product field of batteries.But it is based on the lithium ion battery of " deintercalation " theory, theoretical specific capacity is currently less than 300mA h g-1, real
Border energy density is less than 200Wh kg-1, far from meeting the needs of people are to electronic equipment, electric car and unmanned plane.Lithium sulphur
Battery is different from traditional " rocking chair type lithium ion battery ", in discharge process as a kind of new electrochemical energy storage secondary cell
In, two electron reactions occur for active material sulphur and lithium metal, so that release is up to 1675mAh g-1Theoretical specific capacity and
2600Wh kg-1Theoretical specific energy, meanwhile, active material sulphur have natural abundance it is big, it is at low cost, low toxicity, it is environmental-friendly etc. excellent
Point.Therefore, lithium-sulfur cell is considered as one of the new secondary battery of alternative lithium ion battery, before having good application
Scape.
However, the material and system of lithium-sulfur cell are still faced with many challenges: 1) active material elemental sulfur and discharging product
Lithium sulfide Li2(conductivity is about 10 to S poorly conductive-30S cm-1), and then cause the internal electrochemical contact of sulphur anode bad, thus
Cause the biggish internal driving of battery；2) between sulphur and lithium sulfide the difference of density can cause during discharge nearly 80% body
Product expansion；3) reaction intermediate polysulfide is influenced to wear in positive and negative interpolar by electric field force and concentration gradient during the charging process
Shuttle, and side reaction can occur with sulphur anode and cathode of lithium, reduce coulombic efficiency；4) ethers electrolyte can be reacted with lithium metal,
Li dendrite is formed in negative terminal surface, and then causes safety problem；5) metallic lithium surface is passivated to form SEI film, reduces lithium metal
Effecting reaction site hinders further reaction.Thus poor circulation, low high rate performance is to restrict Li-S battery industryization hair
Exhibition.Start with from lithium sulfur battery anode material, can effectively solve above-mentioned part main problem.
Li-S battery rapidly developed in recent years, was less than 2mg cm in sulphur load amount-2When, cycle performance and high rate performance are equal
There is biggish promotion.Although problems can be effectively relieved in low load amount electrode, lower energy density is unable to satisfy reality
The requirement of application！Thus to develop high load amount lithium-sulfur cell and obtain higher energy density.However, the electrochemistry of high load amount battery
Performance is poor, main reason is that 1. based on knife coating prepare high load amount electrode when electrode it is easy to crack, active material is easy to fall off,
Keep electrode unstable when reacting in battery；2 high load amount electrode interior mass transfers are poor, and the electronics conduction of electrode interior and ion pass
It is defeated limited, sufficient electronics and ion can not be provided to react.The present invention improves electricity by providing a kind of lamelliform porous electrode
Pole internal mass transfer provides faster electronics and ion transmission path for electrode reaction, accelerates reaction and carries out, improves the circulation of battery
Performance and high rate performance.
Summary of the invention
In order to solve the above technical problems, it is an object of that present invention to provide a kind of lamelliform electrode and its in lithium-sulfur cell
Using.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of positive material for lithium-sulfur battery,
Low-freezing solvent is selected, binder is made using solvable macromolecule resin, mixes carbon/sulfur compound and conductive carbon,
Coated in substrate, by freeze-drying in being prepared into lamelliform electrode in substrate；
The low-freezing solvent is water, amphene；It is preferred that: water；
When solvent is water, binder selects LA series, carboxymethyl cellulose-butadiene-styrene rubber (CMC-SBR), β-ring paste
It is one or two or more kinds of in essence, polyvinyl alcohol etc.；It is preferred that: CMC-SBR is bonded when solvent is amphene without macromolecule resin
Agent, but need mold as template；
Carbon/the sulfur compound is one of compound of carbon material and sulphur or two kinds or more.Carbon material is carbon nanometer
Pipe, graphene, carbon nano-fiber, BP2000, KB600, KB300, XC-72, Super-P, acetylene black, active carbon or its correlation are repaired
One or more of decorations or the carbon material of activation.
The conductive carbon can be one or more of above-mentioned carbon material, preferably graphene.
The lamelliform electrode may be designed as micropore, mesoporous or macroporous structure.
The lamelliform thickness of electrode be 20~500 μm, aperture size be 0.5~5000nm, porosity be 10~
90%, porosity 70% is preferred.
The lamelliform electrode, the quality of solvable macromolecule resin account for 2wt%~40wt% of electrode gross mass.
The lamelliform electrode, the quality of sulphur accounts for 20wt%~80wt% of gross mass in carbon-sulfur compound.
The preparation method of above-mentioned electrode, this method are prepared using following steps:
When selection low-freezing solvent is water:
(1) binder is added in water, stirs 0.5~2h at being 20~50 DEG C in temperature, forming mass concentration is 2-
40% Polymer Solution；Carbon/sulfur compound or carbon/sulfur compound are added in above-mentioned solution and the mixture of carbon material exists
Temperature is that 2~10h is sufficiently stirred at 20~50 DEG C, is prepared into slurry；Wherein solid content is between 5~40wt%, preferably 20-
30wt%；
(2) slurry prepared by step (1) is poured in substrate, blade coating is placed on low temperature environment A (- 200 DEG C~-10 DEG C)
Under, until solvent solidifies completely；Wherein, the loading of blade coating amount control sulphur is 0.5-20mg/cm2；The preferred 4-8mg/cm of loading2；
Substrate is one kind of aluminium foil, copper foil, carbon paper or carbon felt；
(3) solidifying body that step 2) obtains is dried in vacuo 6-24h under low temperature environment B (- 200 DEG C~-10 DEG C), prepared
Straticulation shape electrode；
(4) by step (3) preparation lamelliform electrode in room temperature~100 DEG C dry 2~for 24 hours after, obtain dry thin layer
Shape electrode；
When selection low-freezing solvent is amphene:
(1) carbon/sulfur compound or carbon/sulfur compound and conductive carbon are added directly into amphene, are 50-100 in temperature
2~10h is sufficiently stirred at DEG C, is prepared into slurry；Wherein solid content is between 5~40wt%, preferably 20-30wt%；
(2) slurry prepared by step (1) is toppled in a particular mold, then is placed in low temperature environment C (- 200 DEG C~40 DEG C)
Under, until solvent solidifies completely；Wherein, the loading for toppling over amount of slurry control sulphur is 0.5-20mg/cm2；The preferred 2- of loading
5mg/cm2；
(3) solidifying body that step (2) obtains is dried in vacuo 6-24h under low temperature environment D (- 200 DEG C~40 DEG C), prepared
Straticulation shape electrode；
(4) by step (3) preparation lamelliform electrode in room temperature~100 DEG C dry 2~for 24 hours after, obtain dry thin layer
Shape electrode；
Carbon/sulfur compound in carbon/sulfur compound and the mixture of conductive carbon: conductive carbon ratio is 2-19；
The lamelliform electrode is applied in lithium-sulfur cell as anode.
Beneficial outcomes of the invention are as follows:
(1) when the present invention prepares electrode, traditional Kynoar (PVDF) is replaced using nontoxic water system glue, is avoided toxic
Solvent N- dimethyl pyrrolidone (NMP) harmful to human and environment；
(2) present invention replaces convection oven seasoning using freeze-drying, not only improves the electricity of conventional method preparation
It the problems such as pole cracking, active material falls off, can be also used for preparing high load amount electrode；
(3) electrode prepared by the present invention is lamelliform porous structure, and porosity is higher, is conducive to adsorb more electrolysis
The polysulfide for being dissolved in electrolyte is fixed on positive side, reduces polysulfide by liquid, the synergistic effect with lamelliform electrode
Shuttle, improve the cycle performance of battery；
(4) electrode prepared by the present invention is vertical thin porous layer structure, by longitudinal " thick electrode " of high load amount battery
It is changed into the transmission path that lateral " thin electrodes " shorten lithium ion, while layer structure also provides company for the conduction of electronics
Continuous conducting networks, thus the mass transport process of inside battery is accelerated, improve the high rate performance of battery；
The porous electrode of vertical distribution thin layer prepared by the present invention has good ion transport capability, and special stratiform
Electrode structure effectively fixes polysulfide, while lamellar structure shortens lithium ion transport path, thus the multiplying power of battery
Performance and cycle performance are all more excellent, and furthermore preparation process is simple, environmental-friendly.With the thin porous layer shape electricity of this vertical distribution
Pole effectively raises the cycle performance and high rate performance of battery as lithium sulfur battery anode material.
Detailed description of the invention
Fig. 1: the comparative example electrode (above) and embodiment electrode (following figure) photo of different sulphur load amounts；
Fig. 2: preference surface SEM figure (a, b), comparative example surface SEM figure (c, d) and embodiment surface SEM figure (e, f)；
Fig. 3: comparative example section SEM figure (a), embodiment section SEM figure (b) and preference section SEM figure (c)；
Fig. 4: comparative example, embodiment are compared with the porosity of preference；
Fig. 5: comparative example, embodiment are compared with the imbibition rate of preference；
Fig. 6: with the high rate performance test of comparative example, embodiment and preference assembling lithium-sulfur cell；
Fig. 7: with the cyclical stability test of comparative example, embodiment and preference assembling lithium-sulfur cell；
Fig. 8: the cyclical stability test of high load amount lithium-sulfur cell is assembled with preference.
Specific embodiment
The following examples are not intended to limit the scope of the invention to further explanation of the invention.
Carbon-sulfur compound preparation is by the way that 10g commercialization KB600 to be placed in tube furnace, under Ar protection, with 5 DEG C of min-1It rises
Temperature is 600mL min to steam activation 1.5h, vapor flow after 900 DEG C, is passed through-1, the carbon material after activation is denoted as A-
KB600.It takes 5g A-KB600 and 10g S after evenly mixing, is placed in tube furnace, be warming up to 155 DEG C, heating rate is 1 DEG C
min-1, constant temperature 20h, obtained product is denoted as S/A-KB600.
Comparative example
It takes 0.03g carboxymethyl cellulose (CMC) to be dissolved in 3g deionized water, stirs 1h, 0.8g S/A-KB600 is added
With 0.1g KB600, stir 5h, add 0.15g 40wt% butadiene-styrene rubber (SBR), mix slowly 0.5h, adjust scraper to
300 μm, film forming is scratched in aluminum laminated films, after 70 DEG C of dryings overnight, cutting into diameter is 14mm sequin, after weighing, 60 DEG C
After vacuum drying for 24 hours, to be coated with the sequin of S/KB600, for anode, (it is about 1.5mg cm that monolithic, which carries sulfur content,-2), lithium piece is negative
Pole, celgard 2325 is diaphragm, with bis- (trifluoromethyl semi-annular jade pendant acyl) the imine lithium solution (LiTFSI) of 1M plus 1%LiNO3For electrolysis
Matter solution, solvent are the mixed liquor (volume ratio v/v=1:1) of 1,3-dioxolane (DOL) and glycol dimethyl ether (DME), group
Packed battery carries out cycle performance of battery test under 0.2C multiplying power, carries out high rate performance test under 0.1C~2C multiplying power.
First circle specific discharge capacity is 907mA h g under 0.2C multiplying power-1, 100 circulation after specific capacity maintain 610mA h
g-1, capacity retention ratio 67.3%；When multiplying power is promoted to 2C, specific discharge capacity is 451mA h g-1。
Embodiment 1
It takes 0.03g carboxymethyl cellulose (CMC) to be dissolved in 3g deionized water, stirs 1h, 0.8g S/A-KB600 is added
With 0.1g KB600, stir 5h, add 0.15g 40wt% butadiene-styrene rubber (SBR), mix slowly 0.5h, adjust scraper to
, film forming is scratched in aluminum laminated films, is quickly immersed into liquid nitrogen, takes out after 10min, rapidly transfer refrigeration lyophilizer by 300 μm
Dry 10h, 50 DEG C of dryings overnight in (- 50 DEG C of temperature, vacuum degree < 10).Subsequent electrode preparation and the same comparative example of battery assembly.
First circle specific discharge capacity is 926mA h g under 0.2C multiplying power-1, 100 circulation after specific capacity maintain 721mA h
g-1, capacity retention ratio 77.9%；When multiplying power is promoted to 2C, specific discharge capacity is mA h g-1。
Embodiment 2 (preference)
It takes 0.03g carboxymethyl cellulose (CMC) to be dissolved in 4g deionized water, stirs 1h, 0.8g S/A-KB600 is added
With 0.1g graphene, stir 5h, add 0.15g 40wt% butadiene-styrene rubber (SBR), mix slowly 0.5h, adjust scraper to
300 μm, 1000 μm (it is about 8mg cm that monolithic, which carries sulfur content,-2) film forming is scratched in aluminum laminated films, quickly it is immersed into liquid nitrogen,
It is taken out after 10min, dry 10h, 50 DEG C of dryings overnight in transfer refrigeration lyophilizer (- 50 DEG C of temperature, vacuum degree < 10) rapidly.
Subsequent electrode preparation and the same comparative example of battery assembly.
First circle specific discharge capacity is 1203mA h g under 0.2C multiplying power-1, 100 circulation after specific capacity maintain 768mA h
g-1, capacity retention ratio is 78.3% (being calculated based on third circle)；When multiplying power is promoted to 2C, specific discharge capacity is 675mA h g-1。
As shown in Figure 1, comparative example electrode is in load amount 1.5mg cm-2When, electrode cracking, with the raising of load amount, active matter
Matter gradually falls off from Al foil.And embodiment electrode is whole more smooth, does not see obvious shortcoming, and remain tightly with collector
Load amount can be increased to 15mg cm by close connection-2.Preference is identical as embodiment preparation method, using different conductive carbon and
With the preparation of different solid contents, thus macro morphology is similar to embodiment.But from microscopic appearance shown in Fig. 2, embodiment and
Preference electrode is thin porous layer shape electrode, can clearly be seen that a large amount of hole path, and electrode (shown in Fig. 3) from section
It remains with collector and closely contacts.Preference electrode is because solid content is even more suitable, thus layer structure is more evenly, and channel is more
Obviously.And the dry electrode of convection oven is in island (shown in such as Fig. 2 b, d), contacts also defective tightness with collector.Such as Fig. 4,
Shown in 5, the imbibition rate and porosity of embodiment and preference electrode are higher, are conducive to the transmission of electrode interior ion.Based on porous
The above feature of lamelliform electrode, as shown in fig. 6, having preferable using embodiment and preference as the battery of positive electrode
High rate performance, this may be to be conducive to the transmitting of electronics because 1) contact of the material with substrate is more preferable in lamelliform electrode；2) electric
Pole is not cracked, and is layer structure, provides continuous electronics conducting networks for electronics conduction；3) hole of lamelliform porous electrode
Rate is higher, and sufficient Li is provided for micro- reaction zone+；4) porous laminated electrode shortens ion transmission path, accelerates ion transmission.
It is more preferable (as shown in Figure 7) as the cyclical stability of the battery of positive electrode using embodiment and preference compared with comparative example, this side
Face be since electrode surface is more smooth do not occur slight crack, meanwhile, the layer structure of electrode is conducive to hinder polysulfide
Shuttle, on the other hand, the imbibition rate of porous laminated electrode is higher, it is meant that more electrolyte dissolved with polysulfide are fixed
In positive side, shuttle effect is alleviated, improves the cyclical stability of battery.And preference is because its solid content is more suitable, layer
Shape structure is uniform, and pore structure is more moderate, quickly transmits conducive to ion, because obtaining better chemical property.
Furthermore it is preferred that example can also prepare high load amount electrode (8mg cm-2), with its assembled battery in 0.1C specific discharge capacity
Stablize in 769mAh g-1, 75 circulation after capacity retention ratio 87.6%, specific chemical property is as shown in Figure 8.Illustrate this
The prospect that porous laminated electrode is applied in high load amount lithium-sulfur cell.
Claims (8)
1. a kind of lithium-sulfur cell lamelliform electrode, it is characterised in that:
Low-freezing solvent is selected, carbon/sulfur compound or carbon/sulfur compound and carbon material mixture are blended in solvent, is led to
It crosses freeze-drying method and lamelliform electrode is prepared；The low-freezing solvent is water or amphene；It is preferred that water.
2. electrode according to claim 1, it is characterised in that: lamelliform electrode is prepared by such as by freeze-drying
Lower detailed process is prepared,
When selection low-freezing solvent is water:
(1) binder is added in water, stirs 0.5~2h at being 20~50 DEG C in temperature, forming mass concentration is 2-40%'s
Polymer Solution；Carbon/sulfur compound or carbon/sulfur compound are added in above-mentioned solution and the mixture of carbon material is in temperature
2~10h is sufficiently stirred at 20~50 DEG C, is prepared into slurry；Wherein solid content is between 5~40wt%, preferably 20-30wt%；
(2) slurry prepared by step (1) is poured in substrate, blade coating is placed under low temperature environment A, until solvent solidifies completely；
Wherein, the loading of blade coating amount control sulphur is 0.5-20mg/cm2；The preferred 4-8mg/cm of loading2；Substrate is aluminium foil, copper foil, carbon
One kind of paper or carbon felt；
(3) solidifying body that step 2) obtains is dried in vacuo 6-24h at low temperature environment B, is prepared into lamelliform electrode；
(4) the lamelliform electrode of step (3) preparation is dried 2 in room temperature~100 DEG C~for 24 hours after, obtain dry lamelliform electricity
Pole；
Wherein, low temperature environment A and low temperature environment B range are at -200 DEG C~-10 DEG C；
When selection low-freezing solvent is amphene:
(1) carbon/sulfur compound or carbon/sulfur compound and conductive carbon are added directly into amphene, in the case where temperature is 50-100 DEG C
2~10h is sufficiently stirred, is prepared into slurry；Wherein solid content is between 5~40wt%, preferably 20-30wt%；
(2) slurry prepared by step (1) is toppled in a mold, then be placed under low temperature environment C, until solvent solidifies completely；Wherein,
The loading for toppling over amount of slurry control sulphur is 0.5-20mg/cm2；The preferred 2-5mg/cm of loading2；
(3) solidifying body that step (2) obtains is dried in vacuo 6-24h at low temperature environment D, is prepared into lamelliform electrode；
(4) the lamelliform electrode of step (3) preparation is dried 2 in room temperature~100 DEG C~for 24 hours after, obtain dry lamelliform electricity
Pole；
Wherein, low temperature environment C and low temperature environment D range are at -200 DEG C~40 DEG C；
Carbon/sulfur compound in carbon/sulfur compound and the mixture of conductive carbon: conductive carbon ratio is 2-19.
3. electrode according to claim 1, it is characterised in that: when solvent is water, binder is LA series, carboxymethyl fibre
It ties up one or two or more kinds of in element-butadiene-styrene rubber (CMC-SBR), beta-cyclodextrin, polyvinyl alcohol etc.；It is preferred that CMC-SBR.
4. electrode according to claim 1, it is characterised in that: the carbon/sulfur compound is the compound of carbon material and sulphur,
Wherein the quality of sulphur accounts for carbon/sulfur compound gross mass 20wt%~80wt%；Carbon material is carbon nanotube, graphene, carbon are received
One or more of rice fiber, BP2000, KB600, KB300, XC-72, Super-P, acetylene black, active carbon；It is preferred that
Graphene.
5. electrode according to claim 1, it is characterised in that: the electrode is lamellar structure, and lamellar structure is vertical
It is distributed in substrate, thin layer spacing is 0.05~10 μm, and thickness of thin layer is 0.05~10 μm；Thin layer is porous structure, and hole includes
Micropore, mesoporous and macropore, wherein micropore is less than 2nm, and mesoporous is 2~50nm, and macropore is 50~5000nm, and wherein Micropore volume accounts for
It is 20-70% that all well, which is held,.
6. electrode according to claim 1, it is characterised in that: the thickness of electrode be 20~900 μm, porosity be 10~
90%, it is preferred that porosity, which is 70%,.
7. a kind of preparation method of the lamelliform electrode as described in claim 1-6 is any, it is characterised in that: the lamelliform electricity
Pole is prepared according to the following procedure,
When selection low-freezing solvent is water:
(1) binder is added in water, stirs 0.5~2h at being 20~50 DEG C in temperature, forming mass concentration is 2-40%'s
Polymer Solution；Carbon/sulfur compound or carbon/sulfur compound are added in above-mentioned solution and the mixture of carbon material is in temperature
2~10h is sufficiently stirred at 20~50 DEG C, is prepared into slurry；Wherein solid content is between 5~40wt%, preferably 20-30wt%；
(2) slurry prepared by step (1) is poured in substrate, blade coating is placed under low temperature environment A, until solvent solidifies completely；
Wherein, the loading of blade coating amount control sulphur is 0.5-20mg/cm2；The preferred 4-8mg/cm of loading2；Substrate is aluminium foil, copper foil, carbon
One kind of paper or carbon felt；
(3) solidifying body that step 2) obtains is dried in vacuo 6-24h at low temperature environment B, is prepared into lamelliform electrode；
(4) the lamelliform electrode of step (3) preparation is dried 2 in room temperature~100 DEG C~for 24 hours after, obtain dry lamelliform electricity
Pole；
Low temperature environment A and low temperature environment B range are at -200 DEG C~-10 DEG C；
When selection low-freezing solvent is amphene:
(1) carbon/sulfur compound or carbon/sulfur compound and carbon material are added directly into amphene, in the case where temperature is 50-100 DEG C
2~10h is sufficiently stirred, is prepared into slurry；Wherein solid content is between 5~40wt%, preferably 20-30wt%；
(2) slurry prepared by step (1) is toppled in a particular mold, then be placed under low temperature environment C, until solvent solidifies completely；
Wherein, the loading for toppling over amount of slurry control sulphur is 0.5-20mg/cm2；The preferred 2-5mg/cm of loading2；
(3) solidifying body that step (2) obtains is dried in vacuo 6-24h at low temperature environment D, is prepared into lamelliform electrode；
(4) the lamelliform electrode of step (3) preparation is dried 2 in room temperature~100 DEG C~for 24 hours after, obtain dry lamelliform electricity
Pole；
Wherein, low temperature environment C and low temperature environment D range are at -200 DEG C~40 DEG C；
Carbon/sulfur compound in the mixture of carbon/sulfur compound and carbon material: carbon material ratio is 2-19.
8. a kind of application of the lamelliform electrode as described in claim 1-6 is any, it is characterised in that: the lamelliform electrode conduct
Anode is applied in lithium-sulfur cell.
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| CN114551811A (en) * | 2022-02-22 | 2022-05-27 | 北京航空航天大学 | Preparation method of vertical MXene array pole piece, vertical MXene array pole piece and application |
| WO2022110592A1 (en) * | 2020-11-25 | 2022-06-02 | 中国科学院上海高等研究院 | Electrode freeze-coating equipment and manufacturing method |
| CN115692615A (en) * | 2021-07-30 | 2023-02-03 | 华中科技大学 | Low-tortuosity thick electrode based on aqueous binder, and preparation and application thereof |
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