CN108539182A - A kind of preparation method of composite sulfur positive electrode and its application in all solid state lithium-sulfur cell - Google Patents

A kind of preparation method of composite sulfur positive electrode and its application in all solid state lithium-sulfur cell Download PDF

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CN108539182A
CN108539182A CN201810458323.3A CN201810458323A CN108539182A CN 108539182 A CN108539182 A CN 108539182A CN 201810458323 A CN201810458323 A CN 201810458323A CN 108539182 A CN108539182 A CN 108539182A
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mixture
positive electrode
sulfur
preparation
composite
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CN108539182B (en
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高云智
曹毅
张瀚
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Harbin Institute of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

A kind of preparation method of composite sulfur positive electrode and its application in all solid state lithium-sulfur cell, belong to battery material preparing technical field.The method is as follows：Sulfur materials, solid electrolyte and conductive agent are scattered in solvent, solid content is 30 ~ 70%, after ball milling mixing is uniform, dry mixture one；Conductive agent is scattered in solvent, solid content is 30 ~ 70%, is then added into again in mixture one, is added according to the 5 ~ 10% of one mass of mixture, after ball milling mixing is uniform, dry mixture two；The solvated ion liquid of two mass 2 ~ 5% of mixture is added into mixture two, is uniformly mixed to get to composite sulfur positive electrode with mortar grinder.The composite sulfur anode is applied in all solid state lithium-sulfur cell.The present invention proposes the ionic liquid that the solvation compatible with each component on a small quantity is added simultaneously, is filled in solid particle gap, meanwhile, the ionic liquid of solvation has ionic conduction effect, can further strengthen the ionic conduction access of electrode interior sulfur materials.

Description

The preparation method of a kind of composite sulfur positive electrode and its in all solid state lithium-sulfur cell Using
Technical field
The invention belongs to battery material preparing technical fields, and in particular to a kind of preparation method of composite sulfur positive electrode and Its application in all solid state lithium-sulfur cell.
Background technology
All-solid-state battery is a kind of modern high security lithium-ion electric for replacing conventional liquid electrolyte with solid electrolyte Pond, electrolyte are broadly divided into solid polyelectrolyte and inorganic solid electrolyte.Wherein, due to higher safety Property, inorganic solid electrolyte has obtained extensive concern and quickly development.Meanwhile it dressing and setting from intelligence with lithium ion battery The standby expansion for arriving scale energy storage field again to electric vehicle, energy density and power density to battery are proposed higher want It asks, in numerous lithium battery systems, all solid state lithium-sulfur cell is considered as one of the battery system of most application prospect.
However, all solid state lithium-sulfur cell still has problem.Compared to liquid lithium-sulfur cell, solid-state lithium-sulfur cell is due to using Solid electrolyte inhibits " shuttle effect " present in liquid lithium-sulfur cell well, but for sulfur materials electronic conduction Problem with ionic conductivity difference still without good solution, meanwhile, for volume change of the sulphur in charge and discharge process Caused by capacitance loss, do not find good alleviation method yet.To solve the above problems, sulphur, solid need to be researched and developed The combination process and electrode fabrication of electrolyte and conductive agent.
Invention content
The purpose of the present invention is to solve existing sulphur anode composite electronic conductions and ionic conductivity poor, capacitance loss The problem of, the preparation method for providing a kind of composite sulfur positive electrode and its application in all solid state lithium-sulfur cell, described answers Closing sulphur anode has good ion and electronic conduction channel, has using all solid state lithium-sulfur cell of composite sulfur anode good Cyclical stability and capacity retention ratio, realize the big multiplying power discharging of solid-state lithium-sulfur cell, have stronger practicability.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of composite sulfur positive electrode, the method are as follows：
Step 1：By sulfur materials, solid electrolyte and conductive agent according to 40 ~ 60：20~40：5 ~ 10 mass ratio is scattered in solvent In, solid content is 30 ~ 70%, 10 ~ 40 h of ball milling mixing, rotating speed 200 ~ 500r/min, it is to be mixed uniformly after, be placed in 60 DEG C of conditions Lower 24 h of drying obtains mixture one；
Step 2：Conductive agent is scattered in solvent, solid content is 30 ~ 70%, is then added into again in mixture one, according to The 5 ~ 10% of one mass of mixture are added, 10 ~ 40 h of ball milling mixing, rotating speed 30 ~ 50r/min, it is to be mixed uniformly after, be placed in 60 DEG C Under the conditions of dry 24 h, obtain mixture two；
Step 3：The solvated ion liquid of two mass 2 ~ 5% of mixture is added into mixture two, is mixed with mortar grinder equal It is even to get to composite sulfur positive electrode.
A kind of application of the composite sulfur positive electrode of above-mentioned preparation, the composite sulfur anode are applied to all solid lithium sulphur electricity Chi Zhong.
The advantageous effect of the present invention compared with the existing technology is：
1, ball-milling method is typically used at present prepare composite sulfur positive electrode, since rotational speed of ball-mill is higher, the structure of electrode material It is more easily damaged in mechanical milling process and electrode performance is caused to decline, the present invention proposes that two step ball-milling methods, the first step are turned using high Fast ball milling realizes each component micro-nanoization in electrode, and realizes that each component micro/nano level uniformly mixes, greatly increase sulphur anode with Three phase boundary between electrolyte and conductive agent；Second step supplements conductive agent to suitable electrode ratio again, and uses low turn Fast ball milling maintains the self structure of conductive agent material, the conductive agent structure destroyed in first step ball milling is repaired, to construct Good ion needed for electrode interior sulfur materials charge and discharge and electronic conduction road.
2, since solid electrode is difficult to realize 100% consistency, the present invention proposes to be added simultaneously compatible with each component on a small quantity The ionic liquid of solvation is filled in solid particle gap, meanwhile, the ionic liquid of solvation has ionic conduction effect, can Further strengthen the ionic conduction access of electrode interior sulfur materials.
3, the addition of the solvated ion liquid with certain fluidity can also solve sulfur materials in charge and discharge well The problem of front and back sulfur materials caused by volume change detach with electrolyte and conductive agent and cause capacitance loss.
Description of the drawings
Fig. 1 is capacity circulating curve graph of the composite sulfur anode of the invention being prepared in all solid state lithium-sulfur cell；
Fig. 2 is charging and discharging curve figure of the composite sulfur anode of the invention being prepared in all solid state lithium-sulfur cell；
Fig. 3 is capacity circulating curve graph of the sulfur electrode that is prepared of commonsense method in liquid lithium-sulfur cell；
Fig. 4 is charging and discharging curve figure of the sulfur electrode that is prepared of commonsense method in liquid lithium-sulfur cell.
Specific implementation mode
Technical scheme of the present invention is further described with reference to the accompanying drawings and examples, however, it is not limited to this, It is every that technical solution of the present invention is modified or replaced equivalently, without departing from the spirit of the technical scheme of the invention and range, It should all cover in protection scope of the present invention.
Specific implementation mode one：That present embodiment is recorded is a kind of preparation method of composite sulfur positive electrode, the side Method is as follows：
Step 1：By sulfur materials, solid electrolyte and conductive agent according to 40 ~ 60：20~40：5 ~ 10 mass ratio is scattered in solvent In, solid content is 30 ~ 70%, 10 ~ 40 h of ball milling mixing, rotating speed 200 ~ 500r/min, it is to be mixed uniformly after, be placed in 60 DEG C of conditions Lower 24 h of drying obtains mixture one；
Step 2：Conductive agent is scattered in solvent, solid content is 30 ~ 70%, is then added into again in mixture one, according to The 5 ~ 10% of one mass of mixture are added, 10 ~ 40 h of ball milling mixing, rotating speed 30 ~ 50r/min, it is to be mixed uniformly after, be placed in 60 DEG C Under the conditions of dry 24 h, obtain mixture two；
Step 3：The solvated ion liquid of two mass 2 ~ 5% of mixture is added into mixture two, is mixed with mortar grinder equal It is even to get to composite sulfur positive electrode.
Specific implementation mode two：A kind of preparation method of composite sulfur positive electrode described in specific implementation mode one, step One and step 2 in, the solvent be carbon disulfide, acetonitrile, rosin, dimethylbenzene, tetrahydrofuran, low alkane, alcohols or One or more mixtures in ether solvent.
Specific implementation mode three：A kind of preparation method of composite sulfur positive electrode described in specific implementation mode one, step In one, the sulfur materials are the one or more of sulphur or metal sulfide；The metal sulfide is TiS2、CoS2、 FeS2、NiS、Cu2S、SnS、SnS2、MoS2、SeS2Or ZnS.
Specific implementation mode four：A kind of preparation method of composite sulfur positive electrode described in specific implementation mode one, step In one, the solid electrolyte material is sulfide-based inorganic solid electrolyte, polymer matrix solid electrolyte or oxide It is inorganic solid electrolyte；The sulfide-based inorganic solid electrolyte is Li10GeP2S12、75Li2S-25P2S5、70Li2S- 30P2S5、50Li2S-10P2S5- 10LiCl or 50Li2S-10P2S5-10Li3N、Li6PS5Cl、Li10SnP2S12、 Li9.54P3S12Si1.74P1.44S11.7Cl0.3、75 Li2S-24P2S5-P2O5.The polymer matrix solid electrolyte is poly- for PEO bases Polymer electrolyte, LLZO, LAGP, LATP or LLZTO.
Specific implementation mode five：A kind of preparation method of composite sulfur positive electrode described in specific implementation mode one, step One and step 2 in, the conductive agent be gas-phase growth of carbon fibre（VGCF）, carbon nanotube, one in activated carbon or acetylene black Kind.
Specific implementation mode six：A kind of preparation method of composite sulfur positive electrode described in specific implementation mode one, it is special Sign is：In step 3, the solvated ion liquid be equimolar than triethylene glycol dimethyl ether（Triglyme, G3）With Bis trifluoromethyl sulfimide lithium（LiTFSI）Mixture（LiG3）（The ionic liquid of ether-based solvent）, equimolar than four Glycol dimethyl ether（Tetraglyme, G4）With bis trifluoromethyl sulfimide lithium（LiTFSI）Mixture（LiG4）（Ether The ionic liquid of solvation）Li [TFSA]-[DEME][TFSA]（lithium bis-（trifluoromethane- sulfonyl）Amide-N, N-diethlsulfonyl）-amide）、1-ethyl-3methyl-imidazolium-bis （trifluoromethane-sulfonyl）imide （[EMI][TFSI]）、 1-ethyl-3methyl-imidazolium- tetrafluoro-borate（[EMI][BF4]）、 1-buthyl-3methyl-imidazoliumbis （trifluoromethane-sulfonyl）imide （[BMI][TFSI]）、1-buthyl-3methyl-imidazolium- tetrafluoro-borate （[BMI][BF4]）、1-buthyl-3methyl-imidazolium iodide （[BMI] [I]）.
Specific implementation mode seven：A kind of composite sulfur anode prepared by one to six any specific implementation mode of specific implementation mode The application of material, the composite sulfur anode are applied in all solid state lithium-sulfur cell.
Embodiment 1：
A kind of preparation method of composite sulfur positive electrode, the method are as follows：
Step 1：By sulfur materials, solid electrolyte and conductive agent according to 40：40：10 mass ratio is scattered in solvent, solid content Be 40%, 10 h of ball milling mixing, rotating speed 250 r/min, it is to be mixed uniformly after, dry 24 h, are mixed under the conditions of being placed in 60 DEG C Object one；
Step 2：Conductive agent is scattered in solvent, solid content is 30 ~ 70%, is then added into again in mixture one, according to The 5 ~ 10% of one mass of mixture are added, 10 h of ball milling mixing, rotating speed 30 r/min, it is to be mixed uniformly after, be placed under the conditions of 60 DEG C Dry 24 h, obtain mixture two；
Step 3：The solvated ion liquid of two mass 3% of mixture is added into mixture two, is uniformly mixed with mortar grinder, Obtain composite sulfur positive electrode.
Embodiment 2：
5mL rosin is taken first, and sulphur 0.4 g, Li is added10GeP2S120.4 0.1 g of g, VGCF of solid electrolyte, ball milling are mixed 10 h are closed, then 250 revs/min of rotating speed dries 24 h, drying temperature is 60 DEG C, obtains mixture one；Again into mixture one 0.1 g VGCF and 5mL rosin, 10 h of ball milling mixing is added, then 30 revs/min of rotating speed dries 24 h, drying temperature is 60 DEG C, obtain mixture two；0.03 g LiG3 are finally added into mixture two, are uniformly mixed with mortar, obtain composite sulfur anode Material.
Composite sulfur that the present embodiment is prepared anode, measures its discharge capacity and cycle performance, and with commonsense method system The discharge capacity and cycle performance of standby composite sulfur anode are compared, and obtain Fig. 1 ~ Fig. 4, and in figure, #1 indicates the present embodiment system Standby composite sulfur anode, #2 indicate composite sulfur anode prepared by commonsense method, it can be seen that the discharge capacity of material of the present invention and Cycle performance is significantly improved.

Claims (7)

1. a kind of preparation method of composite sulfur positive electrode, it is characterised in that：The method is as follows：
Step 1：By sulfur materials, solid electrolyte and conductive agent according to 40 ~ 60：20~40：5 ~ 10 mass ratio is scattered in solvent In, solid content is 30 ~ 70%, 10 ~ 40 h of ball milling mixing, rotating speed 200 ~ 500r/min, it is to be mixed uniformly after, be placed in 60 DEG C of conditions Lower 24 h of drying obtains mixture one；
Step 2：Conductive agent is scattered in solvent, solid content is 30 ~ 70%, is then added into again in mixture one, according to The 5 ~ 10% of one mass of mixture are added, 10 ~ 40 h of ball milling mixing, rotating speed 30 ~ 50r/min, it is to be mixed uniformly after, be placed in 60 DEG C Under the conditions of dry 24 h, obtain mixture two；
Step 3：The solvated ion liquid of two mass 2 ~ 5% of mixture is added into mixture two, is mixed with mortar grinder equal It is even to get to composite sulfur positive electrode.
2. a kind of preparation method of composite sulfur positive electrode according to claim 1, it is characterised in that：Step 1 and step In two, the solvent is carbon disulfide, acetonitrile, rosin, dimethylbenzene, tetrahydrofuran, low alkane, alcohols or ether solvent In one or more mixtures.
3. a kind of preparation method of composite sulfur positive electrode according to claim 1, it is characterised in that：In step 1, institute The sulfur materials stated are the one or more of sulphur or metal sulfide.
4. a kind of preparation method of composite sulfur positive electrode according to claim 1, it is characterised in that：In step 1, institute The solid electrolyte material stated is that sulfide-based inorganic solid electrolyte, polymer matrix solid electrolyte or oxide system are inorganic solid Body electrolyte；The sulfide-based inorganic solid electrolyte is Li10GeP2S12、75Li2S-25P2S5、70Li2S-30P2S5、 50Li2S-10P2S5- 10LiCl or 50Li2S-10P2S5-10Li3N、Li6PS5Cl、Li10SnP2S12、 Li9.54P3S12Si1.74P1.44S11.7Cl0.3、75 Li2S-24P2S5-P2O5.The polymer matrix solid electrolyte is poly- for PEO bases Polymer electrolyte, LLZO, LAGP, LATP or LLZTO.
5. a kind of preparation method of composite sulfur positive electrode according to claim 1, it is characterised in that：Step 1 and step In two, the conductive agent is one kind in gas-phase growth of carbon fibre, carbon nanotube, activated carbon or acetylene black.
6. a kind of preparation method of composite sulfur positive electrode according to claim 1, it is characterised in that：In step 3, institute The solvated ion liquid stated be equimolar than triethylene glycol dimethyl ether and bis trifluoromethyl sulfimide lithium mixture, etc. The tetraethyleneglycol dimethyl ether of molar ratio and the mixture of bis trifluoromethyl sulfimide lithium, [EMI] [BF4], [BMI] [I], Li [TFSA]-[DEME][TFSA]、[EMI][TFSI]、[BMI][TFSI]、[BMI][BF4]。
7. a kind of application of composite sulfur positive electrode prepared by claim 1 ~ 6 any claim, it is characterised in that：Described Composite sulfur anode is applied in all solid state lithium-sulfur cell.
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CN109888378A (en) * 2019-04-17 2019-06-14 宁波容百新能源科技股份有限公司 A kind of high ionic conductivity sulfide solid electrolyte and preparation method thereof based on liquid phase method
CN110148781A (en) * 2019-04-22 2019-08-20 华中科技大学 A kind of ionic liquid gel electrolyte, preparation method and application
CN110350158A (en) * 2019-06-13 2019-10-18 华中科技大学 A kind of sulphur composite positive pole and its preparation method and application
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CN111834625A (en) * 2020-08-25 2020-10-27 中南大学 Selenium composite positive electrode material, preparation method thereof and all-solid-state lithium selenium battery
CN111952551A (en) * 2019-05-17 2020-11-17 康宁股份有限公司 Improved composite positive electrode for solid-state lithium-sulfur battery and preparation method thereof
CN112234185A (en) * 2020-10-28 2021-01-15 珠海冠宇电池股份有限公司 Positive pole piece and application thereof
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CN113131001A (en) * 2021-04-21 2021-07-16 郑州航空工业管理学院 Solvating ionic liquid electrolyte with adjustable structure, preparation method thereof and lithium-sulfur battery

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CN111146438A (en) * 2018-11-05 2020-05-12 比亚迪股份有限公司 Positive active material, preparation method thereof, battery positive plate and lithium battery
CN109638240A (en) * 2018-11-27 2019-04-16 华中科技大学 A kind of all solid state lithium-sulfur cell and preparation method thereof
CN109671895A (en) * 2018-12-10 2019-04-23 青岛大学 Lithium-sulfur cell diaphragm and lithium-sulfur cell comprising the diaphragm
CN109888378A (en) * 2019-04-17 2019-06-14 宁波容百新能源科技股份有限公司 A kind of high ionic conductivity sulfide solid electrolyte and preparation method thereof based on liquid phase method
CN110148781A (en) * 2019-04-22 2019-08-20 华中科技大学 A kind of ionic liquid gel electrolyte, preparation method and application
CN111952551A (en) * 2019-05-17 2020-11-17 康宁股份有限公司 Improved composite positive electrode for solid-state lithium-sulfur battery and preparation method thereof
CN110350158A (en) * 2019-06-13 2019-10-18 华中科技大学 A kind of sulphur composite positive pole and its preparation method and application
CN110350158B (en) * 2019-06-13 2021-07-27 华中科技大学 Sulfur composite cathode material and preparation method and application thereof
CN110957483A (en) * 2019-12-03 2020-04-03 武汉理工大学 Preparation method and application of sulfur composite cathode material
CN111834625A (en) * 2020-08-25 2020-10-27 中南大学 Selenium composite positive electrode material, preparation method thereof and all-solid-state lithium selenium battery
CN111834625B (en) * 2020-08-25 2021-09-03 中南大学 Selenium composite positive electrode material, preparation method thereof and all-solid-state lithium selenium battery
CN112234185A (en) * 2020-10-28 2021-01-15 珠海冠宇电池股份有限公司 Positive pole piece and application thereof
CN112599759A (en) * 2020-11-26 2021-04-02 东北师范大学 All-solid-state lithium-sulfur battery composite positive electrode material and preparation method thereof
CN112599759B (en) * 2020-11-26 2022-06-07 吉林省东驰新能源科技有限公司 All-solid-state lithium-sulfur battery composite positive electrode material and preparation method thereof
CN113131001A (en) * 2021-04-21 2021-07-16 郑州航空工业管理学院 Solvating ionic liquid electrolyte with adjustable structure, preparation method thereof and lithium-sulfur battery

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