CN105609767A - Cathode material containing additive Mg<x>Ni<1-x>O for lithium-sulfur battery and preparation method - Google Patents
Cathode material containing additive Mg<x>Ni<1-x>O for lithium-sulfur battery and preparation method Download PDFInfo
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- CN105609767A CN105609767A CN201610079714.5A CN201610079714A CN105609767A CN 105609767 A CN105609767 A CN 105609767A CN 201610079714 A CN201610079714 A CN 201610079714A CN 105609767 A CN105609767 A CN 105609767A
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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
- H01M4/58—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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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
The invention discloses a cathode material containing an additive Mg<x>Ni<1-x>O for a lithium-sulfur battery. The Mg<x>Ni<1-x>O and S are doped into a slice layer of KS-6; the mass ratio of the KS-6 to the S to the Mg<x>Ni<1-x>O is 4 to 6 to (0.5-2); the Mg<x>Ni<1-x>O is called a metal oxide; and x is smaller than 1.0 and greater than 0. The invention further discloses a preparation method of the cathode material containing the additive Mg<x>Ni<1-x>O for the lithium-sulfur battery. The Mg<x>Ni<1-x>O is added to the cathode material for the lithium-sulfur battery, so that the cathode material can physically absorb polysulfide, prevent and delay dissolution of the polysulfide in an electrolyte and can also catalyze cleavage of an S-S bond, so that the cycling stability and the coulombic efficiency of the lithium-sulfur battery are improved; the electrochemical properties of the battery material are improved; and the lifetime of the battery is prolonged.
Description
Technical field
The invention belongs to lithium-sulfur cell technical field, relate to one and contain additive MgxNi(1-x)The lithium sulphur of OCell positive material, the invention still further relates to this kind and contains additive MgxNi(1-x)The lithium-sulphur cell positive electrode material of OThe preparation method of material.
Background technology
Along with new energy technology develop rapidly, the R&D and promotion of high-energy density secondary battery becomes new energyThe study hotspot of source domain. Tradition lithium ion battery is subject to the theoretical specific discharge capacity (LiCoO of positive electrode2、LiNiO2And LiMn2O4Theoretical specific discharge capacity be respectively 274mAh/g, 274mAh/g and 148Etc. mAh/g) restriction of factor, is difficult to be used widely in the field such as the energy and traffic. Lithium sulphur secondaryBattery relies on the advantages such as its specific capacity is high, security good, cost is low, environmentally friendly, becomes at presentOne of power supply system of tool prospect. Lithium-sulfur rechargeable battery is made negative pole with lithium metal, and elemental sulfur or sulfenyl are multipleCondensation material is as positive pole, and the theoretical specific capacity of elemental sulfur is 1675mAh/g, and theoretical specific energy can reach 2600Wh/kg, and sulphur also has the advantages such as reserves are abundant, cheap and nontoxic.
But elemental sulfur does anodal lithium-sulfur cell wants really to move towards the practical following problem that also exists:(1) no matter be simple substance S or its reduzate Li2S is insulator, affects the transmission of electric charge; (2)Li2S invertibity is poor, easily loses electro-chemical activity; (3) due to Li2The density difference of S and S is larger,In charge and discharge process there is volumetric expansion contraction in positive and negative pole material circulation, can destroy electrode structure; (4) depositAt intermediate product polysulfide, soluble in electrolyte, and to negative pole migration, cause active material to damageLose and larger energy loss.
Nanometer oxide material generally has the features such as particle diameter is minimum, specific area is very big. Metal oxideGood semiconductor mostly, can be by load, filling or the method for modifying such as coated by nano metal oxygenCompound is introduced sulphur positive pole, improves the chemical property of elemental sulfur. Due to the Gao Bibiao of nano-metal-oxideArea and stronger suction-operated, add after sulfur electrode and can reach the dissolving diffusion that suppresses polysulfide,Improve the object of the chemical property of lithium-sulfur cell system.
Therefore, nano metal oxide materials and elemental sulfur are compound is also of lithium sulfur battery anode materialImportant research direction. KS-6 serves as carrier and the conductive agent of sulphur, adds MgxNi(1-x)After O, it is coarseThe nutty structure on surface can effectively adsorb sulphur and many sulphions, slows down the effect of shuttling back and forth, and MgxNi(1-x)OFracture that can catalysis S-S key, can promote the redox reaction in lithium-sulfur cell, thereby improves lithium sulphur electricityThe cyclical stability in pond and coulomb efficiency, extending battery life.
Summary of the invention
The object of this invention is to provide one and contain additive MgxNi(1-x)The lithium sulfur battery anode material of O,Solved in prior art when elemental sulfur is as positive electrode, battery discharge specific capacity is low, cycle performance is poorProblem.
Another object of the present invention is to provide this kind and contains additive MgxNi(1-x)The lithium-sulphur cell positive electrode of OThe preparation method of material.
The technical solution adopted in the present invention is that one contains additive MgxNi(1-x)The lithium-sulfur cell of O justUtmost point material, by MgxNi(1-x)O and S are entrained in the lamella of KS-6, wherein KS-6:S:MgxNi(1-x)OThree's mass ratio is 4:6:0.5～2; MgxNi(1-x)O is called metal oxide, 0 < x < 1.0.
Another technical scheme of the present invention is that one contains additive MgxNi(1-x)The lithium sulphur electricity of OThe preparation method of pond positive electrode, implements according to following steps:
Step 1) magnesium salts and nickel salt are added in deionized water, ultrasonic dispersion makes it completely molten for 10～60 minutesSeparate, obtain solution A;
Step 2) get citric acid and add in solution A, the total addition level of magnesium salts and nickel salt and the quality of citric acidThan for 1:0.5～2.5, in water-bath, stir evaporation at 70～90 DEG C, until obtain thick greenGel precursors B;
Step 3) by gel precursors B in air dry oven 70 DEG C～90 DEG C after dry 24～48 hours, be placed inIn Muffle furnace, calcine 4～8 hours for 400 DEG C～800 DEG C, obtain MgxNi(1-x)O solid;
Step 4) by KS-6:S:MgxNi(1-x)O mixes according to mass ratio 4:6:0.5～2, machineryAfter ball milling 2 hours, be placed in hydrothermal reaction kettle, pass into after 20-30 minute argon gas, in 155～160 DEG C of guarantorsTemperature 5～20 hours, obtains MgxNi(1-x)O/KS-6/S lithium sulfur battery anode material.
The invention has the beneficial effects as follows, in lithium sulfur battery anode material of the present invention, add MgxNi(1-x)O，It can physical absorption polysulfide, prevents from and delay polysulfide being dissolved in electrolyte, can also urgeChange the fracture of S-S key, thereby improve cyclical stability and coulomb efficiency of lithium-sulfur cell, improve battery materialMaterial chemical property, extending battery life. The inventive method adopts sol-gel process to prepare nanoscaleMetal oxide MgxNi(1-x)O, processing step is simple, and raw material sources are extensive, and cost is low and repeatedGood, make Mg by ball milling and heat treatmentxNi(1-x)O-KS-6/S lithium sulfur battery anode material, electric discharge specific volumeAmount decay is slower, good cycling stability, and the industrialization that can be lithium-sulfur cell provides basis.
Brief description of the drawings
Fig. 1 is Mg prepared by the embodiment of the present invention 10.6Ni0.4The scanning electron microscope (SEM) photograph of O;
Fig. 2 is Mg prepared by the embodiment of the present invention 10.6Ni0.4The X-ray diffractogram of O;
Fig. 3 is Mg prepared by the embodiment of the present invention 10.6Ni0.4O-KS-6/S composite positive pole adds with nothingMg0.6Ni0.4The first charge-discharge curve of the KS-6/S composite positive pole of O under 0.1C;
Fig. 4 is Mg prepared by the embodiment of the present invention 10.6Ni0.4O-KS-6/S composite positive pole adds with nothingMg0.6Ni0.4The cycle performance figure of the KS-6/S composite positive pole of O under 0.1C.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The present invention contains additive MgxNi(1-x)The lithium sulfur battery anode material of O, by MgxNi(1-x)O and S mixMix in the lamella of KS-6, wherein KS-6:S:MgxNi(1-x)O three's mass ratio is 4:6:0.5～2;MgxNi(1-x)O is called metal oxide, 0 < x < 1.0, the granulation mass that metal oxide is spherical rough surfaceLong-pending forming, size is 20～100nm.
The present invention contains additive MgxNi(1-x)The preparation method of the lithium sulfur battery anode material of O, according toLower step is implemented:
Step 1) by magnesium salts (one or both in magnesium nitrate and magnesium acetate) and nickel salt (nickel nitrate and secondOne or both in acid nickel) add in deionized water, ultrasonic dispersion dissolves it in 10～60 minutes completely,Obtain solution A;
Step 2) get citric acid and add in solution A, the total addition level of magnesium salts and nickel salt and the quality of citric acidThan for 1:0.5～2.5, in water-bath, stir evaporation at 70～90 DEG C, until obtain thick greenGel precursors B;
Step 3) by gel precursors B in air dry oven 70 DEG C～90 DEG C after dry 24～48 hours, be placed inIn Muffle furnace, calcine 4～8 hours for 400 DEG C～800 DEG C, obtain MgxNi(1-x)O solid;
Step 4) by KS-6:S:MgxNi(1-x)O mixes according to mass ratio 4:6:0.5～2, machineryAfter ball milling 2 hours, be placed in hydrothermal reaction kettle, pass into after 20-30 minute argon gas, in 155～160 DEG C of guarantorsTemperature 5～20 hours, obtains MgxNi(1-x)O/KS-6/S lithium sulfur battery anode material.
The assembling of battery: anode sizing agent is by lithium sulfur battery anode material, the 10wt% of 70wt%～80wt%The conductive agent (KS-6, conductive black, acetylene black) of～20wt% and the binding agent of 10wt%～20wt%(PVDF) be mixed, solvent is 1-METHYLPYRROLIDONE, is modulated into even pulpous state, is coated with laggardRow is dried compressing tablet, and positive plate is made in cut-parts; Using lithium sheet as negative plate, electrolyte is for containing 1%LiNO in addition31mol/LLiTFSI/DOL – DME (1:1, V%), barrier film is Celgard2300, is assembled into CR2025Button cell.
Embodiment 1
1) 23.1g magnesium nitrate and 11.6g nickel nitrate are added in 150ml deionized water to 20 points of ultrasonic dispersionsClock dissolves it completely, obtains solution A;
2) get 18g citric acid and add in solution A, in water-bath, 90 DEG C are stirred evaporation until obtain thicknessThe gel precursors B of shape green;
3) by gel precursors B in air dry oven 80 DEG C after dry 24 hours, forge in 700 DEG C of Muffle furnacesBurn 5 hours, obtain Mg0.6Ni0.4O solid;
4) by KS-6:S:Mg0.6Ni0.4O mixes according to mass ratio 4:6:1, and mechanical ball milling 2 is littleShi Hou, is placed in hydrothermal reaction kettle, passes into after 20 minutes argon gas, in 156 DEG C of insulations 10 hours, obtainsMg0.6Ni0.4O-KS-6/S composite;
The assembling of battery: anode sizing agent is by the lithium sulfur battery anode material of 70wt%, the conductive agent of 20wt%The binding agent (PVDF) of KS-6 and 10wt% is mixed, and solvent is 1-METHYLPYRROLIDONE, modulationBecome even pulpous state, dry compressing tablet after coating, positive plate is made in cut-parts, in addition using lithium sheet as negative poleSheet, electrolyte is for containing 1%LiNO31mol/LLiTFSI/DOL – DME (1:1, V%), barrier filmCelgard2300, is assembled into CR2025 button cell.
With reference to Fig. 1, the Mg preparing for embodiment 10.6Ni0.4O scanning electron microscope (SEM) photograph, passes through as can be seen from Figure 1Mg prepared by sol-gel process0.6Ni0.4O particle diameter, in 40nm left and right, is shaggy spheric granules.
With reference to Fig. 2, the Mg preparing for embodiment 10.6Ni0.4The X-ray diffractogram of O, all diffraction peaksPut all and match with standard spectrogram JCPDSNo.34-0410, prove to prepare product and beMg0.6Ni0.4O。
With reference to Fig. 3, the Mg preparing for embodiment 10.6Ni0.4O-KS-6/S composite positive pole adds with nothingMg0.6Ni0.4The first charge-discharge curve of the KS-6/S composite positive pole of O under room temperature 0.1C multiplying power.Mg0.6Ni0.4The first discharge specific capacity of O-KS-6/S composite positive pole is 1224mAh/g, puts at 2.1VLevel platform is longer, and without adding Mg0.6Ni0.4The KS-6/S composite positive pole first discharge specific capacity of O onlyFor 676mAh/g, shorter at 2.1V discharge platform, prove to add Mg0.6Ni0.4O can significantly improve batteryFirst discharge specific capacity, and can extend discharge platform.
With reference to Fig. 4, the Mg preparing for embodiment 10.6Ni0.4O-KS-6/S composite positive pole adds with nothingMg0.6Ni0.4The cycle performance figure of the KS-6/S composite positive pole of O under 0.1C. As can be seen from Figure 4Mg0.6Ni0.4Specific discharge capacity 492mAh/g after O-KS-6/S composite positive pole circulation 30 times, capacity is protectedHoldup is 40.2%, without adding Mg0.6Ni0.4Specific volume discharges after the KS-6/S composite positive pole circulation 30 times of OAmount 257mAh/g, capability retention is 38.0%, by contrast, the cycle performance of the present embodiment has had aobviousWork improves.
Embodiment 2
1) 15.4g magnesium nitrate and 17.4g nickel nitrate are added in 150ml deionized water to 15 points of ultrasonic dispersionsClock dissolves it completely, obtains solution A;
2) get 17g citric acid and add in solution A, stir evaporation until obtain thick in 70 DEG C of water-bathsGreen gel precursors B;
3) by gel precursors B 70 DEG C of air dry ovens after dry 48 hours, in 800 DEG C of calcinings 4 of Muffle furnaceHour, obtain Mg0.4Ni0.6O；
4) by KS-6:S:Mg0.4Ni0.6O mixes according to mass ratio 4:6:2, and mechanical ball milling 2 is littleShi Hou, is placed in hydrothermal reaction kettle, passes into after 25 minutes argon gas, in 158 DEG C of insulations 20 hours, to obtain final productKS-6/S/Mg0.4Ni0.6O composite.
The assembling of battery: anode sizing agent is by the lithium sulfur battery anode material of 80wt%, the conductive agent of 10wt%The binding agent (PVDF) of KS-6 and 10wt% is mixed, and solvent is 1-METHYLPYRROLIDONE, modulationBecome even pulpous state, dry compressing tablet after coating, positive plate is made in cut-parts, in addition using lithium sheet as negative poleSheet, electrolyte is for containing 1%LiNO31mol/LLiTFSI/DOL – DME (1:1, V%), barrier filmCelgard2300, is assembled into CR2025 button cell.
Gained battery is 30 cycle charge-discharges under room temperature 0.1C multiplying power, and first discharge specific capacity is 1142MAh/g, Capacitance reserve is at 462mAh/g after 30 times, and capability retention is 40.5%.
Embodiment 3
1) 15g magnesium nitrate and 17g nickel nitrate are added in 150ml deionized water, ultrasonic dispersion makes for 45 minutesIt dissolves completely, obtains solution A;
2) get 16g citric acid and add in solution A, stir evaporation until obtain thick in 80 DEG C of water-bathsGreen gel precursors B;
3) by gel precursors B 80 DEG C of air dry ovens after dry 36 hours, in 500 DEG C of calcinings 8 of Muffle furnaceHour, obtain Mg0.4Ni0.6O；
4) by KS-6:S:Mg0.4Ni0.6O mixes according to mass ratio 4:6:1.5, mechanical ball milling 2After hour, be placed in hydrothermal reaction kettle, pass into after 30 minutes argon gas, in 160 DEG C of insulations 15 hours,Obtain KS-6/S/Mg0.4Ni0.6O composite.
The assembling of battery: anode sizing agent is by the lithium sulfur battery anode material of 80wt%, the conductive agent of 10wt%The binding agent (PVDF) of KS-6 and 10wt% is mixed, and solvent is 1-METHYLPYRROLIDONE, modulationBecome even pulpous state, dry compressing tablet after coating, positive plate is made in cut-parts, in addition using lithium sheet as negative poleSheet, electrolyte is for containing 1%LiNO31mol/LLiTFSI/DOL – DME (1:1, V%), barrier filmCelgard2300, is assembled into CR2025 button cell.
Gained battery is 30 cycle charge-discharges under room temperature 0.1C multiplying power, and first discharge specific capacity is 1140MAh/g, Capacitance reserve is at 463mAh/g after 30 times, and capability retention is 40.6%.
Claims (4)
1. one kind contains additive MgxNi(1-x)The lithium sulfur battery anode material of O, is characterized in that: byMgxNi(1-x)O and S are entrained in the lamella of KS-6, wherein KS-6:S:MgxNi(1-x)O three's matterAmount is than being 4:6:0.5～2; MgxNi(1-x)O is called metal oxide, 0 < x < 1.0.
2. the additive Mg that contains according to claim 1xNi(1-x)The lithium sulfur battery anode material of O,It is characterized in that: described metal oxide size is 20～100nm.
3. one kind contains additive MgxNi(1-x)The preparation method of the lithium sulfur battery anode material of O, its featureBe, implement according to following steps:
Step 1) magnesium salts and nickel salt are added in deionized water, ultrasonic dispersion makes it completely molten for 10～60 minutesSeparate, obtain solution A;
Step 2) get citric acid and add in solution A, the total addition level of magnesium salts and nickel salt and the quality of citric acidThan for 1:0.5～2.5, in water-bath, stir evaporation at 70～90 DEG C, until obtain thick greenGel precursors B;
Step 3) by gel precursors B in air dry oven 70 DEG C～90 DEG C after dry 24～48 hours, be placed inIn Muffle furnace, calcine 4～8 hours for 400 DEG C～800 DEG C, obtain MgxNi(1-x)O solid;
Step 4) by KS-6:S:MgxNi(1-x)O mixes according to mass ratio 4:6:0.5～2,Machinery ball milling, after 2 hours, is placed in hydrothermal reaction kettle, passes into after 20-30 minute argon gas, in 155～160 DEG CBe incubated 5～20 hours, obtain MgxNi(1-x)O/KS-6/S lithium sulfur battery anode material.
4. the additive Mg that contains according to claim 3xNi(1-x)The lithium sulfur battery anode material of OPreparation method, is characterized in that: described magnesium salts is selected one or both in magnesium nitrate and magnesium acetate;Nickel salt is selected one or both in nickel nitrate and nickel acetate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107910584A (en) * | 2017-10-23 | 2018-04-13 | 西安理工大学 | A kind of production method of Soft Roll lithium-sulfur cell |
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| US20110070491A1 (en) * | 2009-08-28 | 2011-03-24 | Sion Power Corporation | Electrochemical cells comprising porous structures comprising sulfur |
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| CN104752702A (en) * | 2015-03-16 | 2015-07-01 | 长沙矿冶研究院有限责任公司 | Cathode material of lithium sulphur battery, preparation method of cathode material, cathode of lithium sulphur battery and lithium sulphur battery |
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| US20110070491A1 (en) * | 2009-08-28 | 2011-03-24 | Sion Power Corporation | Electrochemical cells comprising porous structures comprising sulfur |
| CN103972580A (en) * | 2013-02-06 | 2014-08-06 | 苏州宝时得电动工具有限公司 | Lithium sulfur battery |
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| CN107910584A (en) * | 2017-10-23 | 2018-04-13 | 西安理工大学 | A kind of production method of Soft Roll lithium-sulfur cell |
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