CN109534402A - Chain structure transition metal polysulfide positive electrode for lithium-sulfur cell - Google Patents
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- C01G39/06—Sulfides
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of chain structure transition metal polysulfide positive electrode for lithium-sulfur cell, and the positive electrode has chain structure, chemical formula MSX, wherein M represents transition metal, is selected from one of molybdenum, titanium, vanadium, iron, niobium；X=3-6.The present invention is also proposed with lithium-sulfur cell made of the chain structure transition metal polysulfide positive electrode.The present invention proposes the preparation method of chain transition metal polysulfide, and simple heating equipment can meet, which has the characteristics that easy to operate, simple process.Using method of the invention, when obtaining transition metal polysulfide as secondary lithium-sulfur battery anode, can improve relevant issues, the batteries such as the dissolution shuttle of lithium-sulfur cell polysulfide has more stable cycle performance and longer cycle life.
Description
Technical field
The invention belongs to battery material fields, and in particular to a kind of electrode material of lithium-sulfur cell and the battery containing it.
Background technique
With the rapid development of portable device, the energy density (~150Wh/kg) of existing commercial Li-ion batteries is
It is unable to satisfy the growing energy requirement of portable device, is badly in need of developing new high-energy density secondary battery.Numerous
In candidate battery, lithium-sulfur cell is because its high-energy density, work and storage life are long, safety operation performance is high and cost is relatively low
The advantages that become one of the secondary cell of most potentiality to be exploited.
Elemental sulfur is considered the most potential positive electrode of rechargeable lithium battery, it has high theoretical specific capacity
(1675mAh·cm-2), the property outstanding such as cheap, environment-protecting and non-poisonous, safe.But sulphur anode is also faced and is much chosen simultaneously
War, maximum challenge are capacity attenuation caused by the conductivity problems of the sulphur of lithium-sulfur cell, and " polysulfide shuttle ", follow
The problem of ring service life difference.It is currently used inhibit polysulfide shuttle method by: adjustment electrolyte form, sulphur anode structure be transformed,
New additive agent is added, molecular conformation or existence form of positive sulphur etc. are changed.Above-mentioned three classes method is set out from different perspectives
It can play the role of inhibiting " polysulfide shuttle ", but certain limiting factor is individually present.The essence dissolved from more lithium sulfides
For upper, the product for regulating and controlling molecular conformation or the existence form of sulphur to control in charge and discharge process can fundamentally solve more sulphur
The problems of dissolution of compound, therefore suitable polysulfide is selected in the design based on molecular structure, fundamentally it can regulate and control to fill
Discharging product avoids generating soluble more lithium sulfides.
For seeking to positive electrode preferably, we expect being similar to organic sulfur compound, the inorganic chemical of sulfur-bearing
Object (such as transient metal sulfide or polysulfide) may have unexpected prospect, as " sulphur of equal value " positive electrode, I
Wish that these materials can be without elemental sulfur, but can show the electrochemical behavior similar with elemental sulfur.We are to their emerging
Interest is that their reaction path may not be related to forming soluble polysulfide intermediate.This may evade traditional lithium sulphur electricity
Long term life defect existing for pond, and eventually lead to the fabulous necessary battery cycle life for business lithium-sulfur cell.
Summary of the invention
For shortcoming existing for this field, the present invention is directed to propose a kind of chain structure transition for lithium-sulfur cell
Metal polysulfide complex positive electrode, the present invention is using elemental sulfur or sulfur-containing compound as sulphur source, with transition metal organic/inorganic chemical combination
Object is molybdenum source, and above-mentioned material is made by one step of solution heating means.
It is another object of the present invention to propose a kind of lithium-sulfur cell, just with the chain structure transition metal polysulfide
Pole material is made.
Realize the technical solution of the object of the invention are as follows:
A kind of chain structure transition metal polysulfide positive electrode for lithium-sulfur cell, which is characterized in that it is described just
Pole material has chain structure, chemical formula MSX, wherein M represents transition metal, is selected from one of molybdenum, titanium, vanadium, iron, niobium (M
=Mo, V, Ti, Nb etc.；X=3~6)；X=3~6.
Further, the positive electrode is molybdenum trisulfide or four vanadic sulfides.
Further, the positive electrode molybdenum trisulfide, be powder of the partial size between 50~200nm or it is described just
Pole material is four vanadic sulfides, is powder of the partial size between 0.1~1 μm.
The positive electrode can be obtained using manner known in the art.Here, providing preferred preparation method such as
Under:
Wherein, the positive electrode is prepared by the following method and obtains:
(1) sulphur source and transistion metal compound are added in organic solvent after mixing and are reacted；The sulphur source is to rise
Magnificent sulphur, sedimentation sulphur, thiocarbamide, one of thioacetamide or a variety of；The transistion metal compound is selected from hexacarbonylmolybdenum, molybdic acid
Ammonium, ammonium metavanadate, vanadic anhydride, one of sodium vanadate；
(2) mixed solution that reaction obtains isolates solid phase and drying, obtains transition metal polysulfide positive electrode.
Wherein, the organic solvent is 1,2- o-dichlorohenzene, n-hexane, chlorobenzene, methylene chloride, one of methanol.This
Two kinds of substances in a solvent all can unlimited ratio dissolution.
Wherein, the time of the reaction be 1~for 24 hours,
Wherein, controlled at 150~250 DEG C when reaction.
Wherein, the molar ratio of the transistion metal compound and sulphur source is 1:(3~24).To react fully.
A kind of lithium-sulfur cell is made with the chain structure transition metal polysulfide positive electrode.
The invention has the following advantages over the prior art:
Chain transition metal polysulfide proposed by the present invention, wherein molybdenum trisulfide can reside in temperature lower than 335 DEG C
Amorphous state.The discussion of its molecular structure may be by molybdenum ion referring to Fig. 1, the molecular structure of unformed molybdenum trisulfide
It links, bridge joint is two kinds of ligands, and the chemical formula of a kind of monosulfide, a kind of disulphide, gained chemical substance is
(S2-)、(S2 2-) or MoS3.It is well known that non-crystalline material is not particularly suited for the reason of many applications are such as electronics or photoelectric device is
Their structure disturbance is to electron transmission nocuousness.However, they have and apply well to catalysis and energy storage.Using without fixed
Shape MoS3The advantages of be multiple.1D chain has more open sites to store to active lithium-ion, reaches the 25% of theoretical capacity；
It promotes the quick diffusion of lithium ion, therefore has potential ability, has better chemical property；Its amorphism
Matter also has lower activation energy, hinders the structural rearrangement in conversion reaction.Four vanadic sulfides with similar chain structure are (see figure
2), it is expected to which there is better chemical property.
The present invention proposes the preparation method of chain transition metal polysulfide, and simple heating equipment can meet, the work
Skill has the characteristics that easy to operate, simple process.Using method of the invention, transition metal polysulfide is obtained as secondary
When lithium galvanic battery anode, can improve relevant issues, the batteries such as the dissolution shuttle of lithium-sulfur cell polysulfide has more stable cyclicity
It can be with longer cycle life.
Detailed description of the invention
Fig. 1 is the structural model figure of molybdenum trisulfide,
Fig. 2 is the structural model figure of four vanadic sulfides,
Fig. 3 is the X ray diffracting spectrum of molybdenum trisulfide；
Fig. 4 is the chemical property curve of molybdenum trisulfide electrode,
Fig. 5 is the microscopic appearance of molybdenum trisulfide material,
Fig. 6 is the X ray diffracting spectrum of four vanadic sulfides,
Fig. 7 is the chemical property curve of four vanadic sulfides.
Fig. 8 is the microscopic appearance of four vanadic sulfide materials.
Specific embodiment
Following specific embodiments should not be construed as limiting the invention for illustrating the present invention.
In embodiment, unless otherwise instructed, technological means used is this field conventional technology.
Embodiment 1:
A kind of lithium-sulfur cell chain structure transition metal polysulfide positive electrode is prepared by following steps:
(1) sulphur source and transition metal organometallic compound are added to 1 by sulphur source and transistion metal compound after evenly mixing,
In 2- o-dichlorohenzene organic solvent, and reacted by the way of heating.In the present embodiment, sulphur source is sublimed sulfur；Transition gold
Category compound is hexacarbonylmolybdenum, and the molar ratio of sulphur source and hexacarbonylmolybdenum is 10:1 (gross mass 1g), and above-mentioned material uniformly mixes,
It is added in 35mL dichloro-benzenes, stirring to mixed liquor is clear solution.
(2) sulphur source and transistion metal compound are dissolved in dichloro-benzenes to be placed in container, are kept the temperature under the conditions of 185 DEG C of high temperature
2h；
(3) by mixed solution centrifugal drying obtained in (2), positive electrode transition metal polysulfide is obtained.Gained produces
Object is powder, and SEM observes its partial size between 50~200nm (referring to Fig. 5).X-ray diffraction result is shown in Fig. 3, meets trisulfides
The diffractive features peak value of molybdenum.
Embodiment 2:
A kind of lithium-sulfur cell chain structure transition metal polysulfide positive electrode is prepared by following steps:
(1) sulphur source and transition metal organometallic compound are added to first by sulphur source and transistion metal compound after evenly mixing
In alcohol organic solvent, and reacted by the way of heating.In the present embodiment, sulphur source is thioacetamide；Transition metal
Conjunction object is ammonium metavanadate, and the mass ratio of sulphur source and ammonium metavanadate is 5:1 (gross mass 1g).
(2) sulphur source and transistion metal compound are dissolved in 35mL methanol, stirring 30min is placed in container, high temperature 160
12h is kept the temperature under the conditions of DEG C；
(3) by mixed solution centrifugal drying obtained in (2), positive electrode transition metal polysulfide is obtained.Gained produces
Object is powder, and the result of X-ray diffraction is shown in Fig. 6, it was demonstrated that product is four vanadic sulfides.The pattern that SEM observes its four vanadic sulfide is two
Laminated structure is tieed up, as a result nanometer sheet partial size is shown in Fig. 8 in 0.1-1um.
Embodiment 3:
A kind of lithium-sulfur cell chain structure transition metal polysulfide positive electrode is prepared by following steps:
(1) sulphur source and transition metal organometallic compound are added to 1 by sulphur source and transistion metal compound after evenly mixing,
In 2- o-dichlorohenzene organic solvent, and reacted by the way of heating.In the present embodiment, sulphur source is sublimed sulfur；Transition gold
Category compound is hexacarbonylmolybdenum, and the molar ratio of sulphur source and hexacarbonylmolybdenum is 10:1 (gross mass 1g), and above-mentioned material uniformly mixes,
It is added in 35mL dichloro-benzenes, stirring to mixed liquor is clear solution.
(2) sulphur source and transistion metal compound are dissolved in dichloro-benzenes to be placed in container, are kept the temperature under the conditions of 185 DEG C of high temperature
12h；
(3) by mixed solution centrifugal drying obtained in (2), positive electrode transition metal polysulfide is obtained.Gained produces
Object is powder, and SEM observes its partial size between 100~250nm.
Embodiment 4:
A kind of lithium-sulfur cell chain structure transition metal polysulfide positive electrode is prepared by following steps:
(1) sulphur source and transition metal organometallic compound are added to two by sulphur source and transistion metal compound after evenly mixing
In chlorobenzene organic solvent, and reacted by the way of heating.In the present embodiment, sulphur source is sublimed sulfur；Transition metal compound
Object is sodium vanadate, and the molar ratio of sulphur source and sodium vanadate is 5:1 (gross mass 1g).
(2) sulphur source and transistion metal compound are dissolved in methanol to be placed in container, are kept the temperature for 24 hours under the conditions of 180 DEG C of high temperature；
(3) by mixed solution centrifugal drying obtained in (2), positive electrode transition metal polysulfide is obtained.Gained produces
Object is powder, and the pattern that SEM observes its four vanadic sulfide of partial size is two-dimensional sheet structure, and temperature is higher, and the reaction time increases, two dimension
Nanometer sheet is accumulated, and the packed structures of 0.5-5um are formed.
Battery performance test
CR2032 type button cell is made in positive electrode made from embodiment 1 to test, wherein the preparation side of anode
Method are as follows: positive electrode, super P Li conductive agent polyvinylidene fluoride (PVDF) 7:2:1 in mass ratio of the preparation of embodiment 1 are mixed
It closes, is ground so that uniform sizing material is made, then the uniform sizing material is coated on aluminium foil, then 60 degree of vacuum dryings, it
After take out in glove box, argon gas protection under assembled battery.The cathode of battery is lithium piece, and diaphragm is PP (polypropylene), electrolyte
For 1.0M LiTFSI in DME:DOL=1:1V%.Referring to fig. 4, the reversible capacity of battery reaches 450mAhg-1, and without obviously declining
Subtract.
Button cell is ibid made in material prepared by embodiment 2, carries out electro-chemical test.Referring to Fig. 7, the initial appearance of battery
Amount reaches 600mAhg-1, capacity is maintained at 470mAhg when circulation for the second time-1, capacity is maintained at when third time recycles
360mAhg-1。
Above example is only that a specific embodiment of the invention is described, and is not carried out to the scope of the present invention
It limits, those skilled in the art can also do numerous modifications and variations on the basis of existing technology, not depart from design of the present invention
Under the premise of spirit, all variations and modifications that this field ordinary engineering and technical personnel makes technical solution of the present invention,
It should fall within the scope of protection determined by the claims of the present invention.
Claims (9)
1. a kind of chain structure transition metal polysulfide positive electrode for lithium-sulfur cell, which is characterized in that the anode
Material has chain structure, chemical formula MSX, wherein M represents transition metal, is selected from one of molybdenum, titanium, vanadium, iron, niobium；X=
3~6.
2. chain structure transition metal polysulfide positive electrode according to claim 1, which is characterized in that the anode
Material is molybdenum trisulfide or four vanadic sulfides.
3. chain structure transition metal polysulfide positive electrode according to claim 2, which is characterized in that the anode
Material molybdenum trisulfide is powder of the partial size between 50~200nm；Or the positive electrode is four vanadic sulfides, is partial size 0.1
Powder between~1 μm.
4. described in any item chain structure transition metal polysulfide positive electrodes, feature exist according to claim 1~3
In the positive electrode is prepared by the following method and obtains:
(1) be added in organic solvent and reacted after sulphur source and transistion metal compound mixing, the sulphur source be sublimed sulfur,
Settle one of sulphur, thiocarbamide or a variety of；The transistion metal compound is selected from hexacarbonylmolybdenum, ammonium molybdate, ammonium metavanadate, five oxygen
Change two vanadium, one of sodium vanadate；
(2) mixed solution that reaction obtains isolates solid phase and drying, obtains transition metal polysulfide positive electrode.
5. chain structure transition metal polysulfide positive electrode according to claim 4, which is characterized in that described organic
Solvent is 1,2- o-dichlorohenzene, n-hexane, chlorobenzene, methylene chloride, one of methanol.
6. chain structure transition metal polysulfide positive electrode according to claim 4, which is characterized in that the reaction
Time be 1~for 24 hours.
7. chain structure transition metal polysulfide positive electrode according to claim 4, which is characterized in that reaction time control
Temperature processed is 150~250 DEG C.
8. chain structure transition metal polysulfide positive electrode according to claim 4, which is characterized in that the transition
The molar ratio of metallic compound and sulphur source is 1:(3~24).
9. a kind of lithium-sulfur cell, which is characterized in that with the more sulphur of chain structure transition metal according to any one of claims 1 to 8
Compound positive electrode is made.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923652A (en) * | 2016-04-29 | 2016-09-07 | 陕西科技大学 | Multilevel-structured VS4 nano-powder, and preparation method and application thereof |
| CN107381636A (en) * | 2017-07-11 | 2017-11-24 | 陕西科技大学 | A kind of vanadic sulfide powder of nano-particles self assemble three dimensional micron cauliflower-shaped four and its preparation method and application |
-
2018
- 2018-10-23 CN CN201811240672.4A patent/CN109534402A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923652A (en) * | 2016-04-29 | 2016-09-07 | 陕西科技大学 | Multilevel-structured VS4 nano-powder, and preparation method and application thereof |
| CN107381636A (en) * | 2017-07-11 | 2017-11-24 | 陕西科技大学 | A kind of vanadic sulfide powder of nano-particles self assemble three dimensional micron cauliflower-shaped four and its preparation method and application |
Non-Patent Citations (4)
| Title |
|---|
| HUALIN YE等: "Amorphous MoS3 as the sulfur-equivalent cathode material for room-temperature Li–S and Na–S batteries", 《PNAS》 * |
| WEI ZHANG等: "Water-Soluble MoS3 Nanoparticles for Photocatalytic H2 Evolution", 《CHEMSUSCHEM》 * |
| YANRONG WANG等: "Highly Branched VS4 Nanodendrites with 1D Atomic-Chain Structure as a Promising Cathode Material for Long-Cycling Magnesium Batteries", 《ADV. MATER.》 * |
| 胡坤宏: "纳米二硫化钼制备工艺及其摩擦学性能研究", 《中国优秀博硕士学位论文全文数据库 (硕士) 工程科技Ⅰ辑》 * |
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Application publication date: 20190329 |