CN108376797A - Resist the solid lithium ion conductors material and preparation method of lithium metal contact reduction - Google Patents

Resist the solid lithium ion conductors material and preparation method of lithium metal contact reduction Download PDF

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CN108376797A
CN108376797A CN201810031900.0A CN201810031900A CN108376797A CN 108376797 A CN108376797 A CN 108376797A CN 201810031900 A CN201810031900 A CN 201810031900A CN 108376797 A CN108376797 A CN 108376797A
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lithium ion
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doping
conductor material
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CN108376797B (en
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吕晓娟
黄珊
杨东昱
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North China Electric Power University
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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
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • 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
    • 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
    • H01M10/058—Construction or manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0068—Solid electrolytes inorganic
    • H01M2300/0071—Oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0088—Composites
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention belongs to solid lithium ion battery solid electrolyte material preparing technical fields, more particularly to resist the solid lithium ion conductors material and preparation method of lithium metal contact reduction.The conductor material use metal ions M6+Doping contains Ti4+NASICON types Li1+xAlxTi2‑x(PO4)3Or Ca-Ti ore type Li3yLa2/3‑yTiO3Conductor material, wherein metal M are W, Cr, Mo or Mn；And it is prepared using solid sintering technology；Conductor material provided by the invention, which has high lithium ion conduction performance and resists lithium metal, restores Ti4+Ability.

Description

Resist the solid lithium ion conductors material and preparation method of lithium metal contact reduction
Technical field
The invention belongs to solid lithium ion battery solid electrolyte material preparing technical fields, more particularly to resist metal The solid lithium ion conductors material and preparation method of lithium contact reduction.
Background technology
Energy and power density are high and clean lithium ion battery is ripe in the application of field of portable electronic apparatus, But it is applied to the leakage for also needing to solve liquid organic electrolyte on fixed equipment and motor vehicle, corroding electrode or even aoxidizes combustion The security hidden troubles such as burning, and be also required to further increase battery capacity and durability.With good thermal stability, antidetonation Property, wide chemical window, No leakage and free of contamination inorganic solid electrolyte be a selection well.But it is electric with organic liquid Solution matter is compared, and the ionic conductivity of inorganic solid electrolyte is relatively low, is not met by demand of the electric vehicle in terms of power, because The inoganic solids Lithium Ionic Conducting Materials of this exploitation high ionic conductivity energy are the key that solve the problems, such as this.
The solid lithium ion conductors material of most study has the Li of NASICON types at present1+xTi2-xAlx(PO4)3And perovskite The Li of type3yLa(2/3)-y□(1/3)-2yTiO3, wherein 0≤y≤0.16, represent Ca-Ti ore type Li3yLa(2/3)-y□(1/3)-2yTiO3 Vacancy in structure.At room temperature, the total conductivity of two kinds of materials is 10-4The S/cm orders of magnitude.But all due to both systems Titanium containing tetravalence exists and is reduced into titanous when being contacted with lithium metal, and lithium metal is oxidized to the defect of lithium ion, this to lack It is sunken to lead to electronic conduction, make battery that internal short-circuit occur, reduces the performance of battery.Therefore solve containing titanic solid-state lithium from When sub- conductor material is contacted with lithium metal the technical issues of oxidizable reduction, and its ionic conductivity is further increased, to lithium Ion battery solid state electrolysis Quality Research will produce important meaning with application.
Invention content
The solid lithium ion conductors material and preparation method restored the purpose of the present invention is to provide resistance lithium metal contact, Specific technical solution is：
A kind of solid lithium ion conductors material for resisting lithium metal contact reduction, the conductor material are to utilize metal ion M6+Doping contains Ti4+Solid lithium ion conductors material；The metal ions M6+For W6+、Cr6+、Mo6+Or Mn6+In one kind or It is two or more；
It is described to contain Ti4+Solid lithium ion conductors material be NASICON types Li1+xAlxTi2-x(PO4)3Or Ca-Ti ore type Li3yLa2/3-yTiO3, wherein 0 ＜ x ＜, 2,0 ＜ y ＜ 0.16；
The metal ions M6+It is doped in the form of metal oxide, doping is 0wt%~10wt%, preferably For 5wt%.
The preparation method of the solid lithium ion conductors material, includes the following steps：
(1) raw material is weighed, uniformly mixes after grinding, is calcined in Muffle furnace, removes moisture and volatile materials；
(2) after the completion of calcining, after taking out, being fully ground, with tablet press machine compression moulding；
(3) material of compression moulding is subjected to solid-phase sintering using Muffle furnace；
Calcination temperature is 400~700 DEG C in the step (1), calcination time 2h；
Sintering temperature is 950 DEG C -1100 DEG C in the step (3), soaking time 4h.
The doping M that the conductor material or the preparation method are prepared6+Lithium Ionic Conducting Materials, smear silver paste, Filamentary silver is affixed, impedance is measured with electrochemical workstation and calculates ionic conductivity and lithium ion transference number, obtains material room temperature electricity Conductance reaches as high as 5.49 × 10-4S/cm, lithium ion transference number are 0.99, i.e., close to 1, illustrate that material is pure lithium ion Conductor.
The sample of preparation is contacted 96 hours in an inert atmosphere with metal lithium sheet, measures the front and back ionic conductivity of contact Variation finds doping W6+Material contacted with lithium metal after conductivity variations be significantly less than undoped lithium ion conductor material Material, i.e. performance are more stablized.
Beneficial effects of the present invention are：
(1) doping M provided by the invention6+The conductor material of metal ion, not only total conductivity be obviously improved, but also The M of doping6+The Ti being easily reduced can be protected4+, and then significantly reduce Lithium Ionic Conducting Materials and gone back when being contacted with lithium metal Risk that is former and generating electronic conductance；
(2) doping M provided by the invention6+The conductor material of metal ion, after high temperature sintering, M6+It has been fully immersed into Li1+xAlxTi2-x(PO4)3Lattice, XRD can't detect free MO3Phase, resulting materials are pure trigonal system NASICON； The microstructure of conductor material is in doping M6+Front and back not change significantly, structure is all very fine and close, homogeneous grain size.
Description of the drawings
Fig. 1 is Li in embodiment 1, embodiment 61.3Al0.3Ti1.7(PO4)3The XRD diffraction patterns of solid lithium ion conductors material；
Fig. 2 is Li in embodiment 11.3Al0.3Ti1.7(PO4)3The SEM photograph of solid lithium ion conductors material；
Fig. 3 is Li in embodiment 1-71.3Al0.3Ti1.7(PO4)3The total ionic conductance of room temperature of solid lithium ion conductors material Rate；
Fig. 4 is Li in embodiment 61.3Al0.3Ti1.7(PO4)3The SEM photograph of solid lithium ion conductors material；
Fig. 5 be embodiment 1,6 in sample contacted with metal lithium sheet after conductivity variations rate comparison diagram.
Specific implementation mode
The solid lithium ion conductors material and preparation method restored the present invention provides resistance lithium metal contact, with reference to The present invention is described further for drawings and examples.
Embodiment 1
Prepare undoped solid lithium ion conductors material Li1.3Al0.3Ti1.7(PO4)3, the specific steps are：
(1) according to chemical formula Li1.3Al0.3Ti1.7(PO4)3Stoichiometric ratio, weigh raw material Li2CO3、Al2O3、TiO2、 NH4H2PO4, wherein raw material Li2CO3It is 10% is weighed to compensate the loss of lithium under high temperature more；In mortar fully by the raw material of weighing Grinding is uniformly mixed；
(2) 700 DEG C are warming up to the rate of 5 DEG C/min in Muffle furnace, keep the temperature 2h；
(3) after the completion of step (2), take out and be fully ground, then use tablet press machine compression moulding, in Muffle furnace with 5 DEG C/ The rate of min is warming up to 950 DEG C, keeps the temperature 4h, coin sample is obtained after natural cooling.
The coin sample of gained is smeared into silver paste, affixes filamentary silver, impedance is measured with electrochemical workstation and calculates ion Conductivity and lithium ion transference number, testing result is specifically as shown in Fig. 3, statistics indicate that the material total ionic conductance at room temperature Rate is 1.80 × 10-4S/cm, lithium ion transference number 0.99, bright prepared material are pure Lithium Ionic Conducting Materials.
By the solid lithium ion conductors material Li of preparation1.3Al0.3Ti1.7(PO4)3XRD, SEM test are carried out, wherein XRD is surveyed Test result is specifically as shown in Fig. 1, and XRD tests show that the crystal form of material prepared is the NASICON of trigonal system, and space group is R-3C.SEM testing results are specifically as shown in Fig. 2, and SEM photograph shows that the microstructure of material prepared is very fine and close, crystal grain Size is at 1.5 μm or so.
The sample of preparation is contacted 96 hours in an inert atmosphere with metal lithium sheet, measures the front and back ionic conductivity of contact Variation, it is specific as shown in Fig. 5, from attached drawing 5 as can be seen that undoped Li1.3Al0.3Ti1.7(PO4)3Conductor material ions electricity Conductance change rate is 62% or so, i.e. Ti in material4+Redox reaction occurs with lithium metal, produces electronic conduction, influences The ionic conductivity of material.
Embodiment 2
In solid lithium ion conductors material Li1.3Al0.3Ti1.7(PO4)3Middle doping 1wt%WO3, preparation method includes following Step：
(1) according to chemical formula Li1.3Al0.3Ti1.7(PO4)3Raw material Li is weighed with stoichiometric ratio2CO3、Al2O3、TiO2、 NH4H2PO4, and add the WO of 1wt%3, wherein Li2CO3More titles 10% are to compensate the loss of lithium under high temperature；The raw material of weighing is existed It is fully ground, is uniformly mixed in mortar；
(2) 700 DEG C are warming up to the rate of 5 DEG C/min in Muffle furnace, keep the temperature 2h；
(3) after the completion of step (2), take out and be fully ground, then use tablet press machine compression moulding, in Muffle furnace with 5 DEG C/ The rate of min is warming up to 950 DEG C, keeps the temperature 4h, coin sample is obtained after natural cooling.
The coin sample of gained is smeared into silver paste, affixes filamentary silver, impedance is measured with electrochemical workstation and calculates ion Conductivity and lithium ion transference number, testing result are specifically as shown in Fig. 3；Statistics indicate that doping 1wt%WO3's Li1.3Al0.3Ti1.7(PO4)3Total ionic conductivity is 2.66 × 10 to conductor material at room temperature-4S/cm, than undoped WO3's Material electric conductivity improves 48%, and lithium ion transference number 0.99 illustrates that prepared material is pure Lithium Ionic Conducting Materials.
Embodiment 3
In solid lithium ion conductors material Li1.3Al0.3Ti1.7(PO4)3Middle doping 2wt%WO3, preparation method and embodiment 2 It is identical.
The coin sample of gained is smeared into silver paste, affixes filamentary silver, impedance is measured with electrochemical workstation and calculates ion Conductivity and lithium ion transference number, testing result are specifically as shown in Fig. 3；Statistics indicate that doping 2wt%WO3's Li1.3Al0.3Ti1.7(PO4)3Total ionic conductivity is 2.92 × 10 to conductor material at room temperature-4S/cm, than undoped WO3With And it is doped with 1wt%WO3Material electric conductivity increase, lithium ion transference number 0.99 illustrates that prepared material is pure Lithium Ionic Conducting Materials.
Embodiment 4
In solid lithium ion conductors material Li1.3Al0.3Ti1.7(PO4)3Middle doping 3wt%WO3, preparation method and embodiment 2 It is identical.
The coin sample of gained is smeared into silver paste, affixes filamentary silver, impedance is measured with electrochemical workstation and calculates ion Conductivity and lithium ion transference number, testing result are specifically as shown in Fig. 3；Statistics indicate that doping 3wt%WO3's Li1.3Al0.3Ti1.7(PO4)3Total ionic conductivity is 4.03 × 10 to conductor material at room temperature-4S/cm, than undoped WO3With And it is doped with 1wt%, 2wt%WO3Material electric conductivity increase, lithium ion transference number 0.99 illustrates prepared material Material is pure Lithium Ionic Conducting Materials.
Embodiment 5
In solid lithium ion conductors material Li1.3Al0.3Ti1.7(PO4)3Middle doping 4wt%WO3, preparation method and embodiment 2 It is identical.
The coin sample of gained is smeared into silver paste, affixes filamentary silver, impedance is measured with electrochemical workstation and calculates ion Conductivity and lithium ion transference number, testing result are specifically as shown in Fig. 3；Statistics indicate that doping 4wt%WO3's Li1.3Al0.3Ti1.7(PO4)3Total ionic conductivity is 4.54 × 10 to conductor material at room temperature-4S/cm, than undoped WO3With And it is doped with 1wt%, 2wt%, 3wt%WO3Material electric conductivity increase, lithium ion transference number 0.99 illustrates made Standby material is pure Lithium Ionic Conducting Materials.
Embodiment 6
In solid lithium ion conductors material Li1.3Al0.3Ti1.7(PO4)3Middle doping 5wt%WO3, preparation method and embodiment 2 It is identical.
The coin sample of gained is smeared into silver paste, affixes filamentary silver, impedance is measured with electrochemical workstation and calculates ion Conductivity and lithium ion transference number, testing result are specifically as shown in Fig. 3；Statistics indicate that doping 5wt%WO3's Li1.3Al0.3Ti1.7(PO4)3Total ionic conductivity is 5.49 × 10 to conductor material at room temperature-4S/cm, than undoped WO3With And it is doped with 1wt%, 2wt%, 3wt%, 4wt%WO3Material electric conductivity increase, rise to undoped with WO3Conductivity of material 3 times of rate；Lithium ion transference number is 0.99, illustrates that prepared material is pure Lithium Ionic Conducting Materials.
By above-mentioned doping 5wt%WO3Li1.3Al0.3Ti1.7(PO4)3Conductor material carries out XRD, SEM test, wherein XRD Test result is specifically as shown in Fig. 1, and XRD can't detect free WO3Phase, i.e. W6+It has been fully immersed into Li1+xAlxTi2-x(PO4)3 Lattice, resulting materials be pure trigonal system NASICON, space group R-3C.SEM testing results are as shown in Fig. 4；SEM Photo shows that the microstructure of material prepared is very fine and close, and grain size is relatively uniform, and grain size is at 1.0 μm or so, doping Crystallite dimension after tungsten slightly reduces.
The sample of preparation is contacted 96 hours in an inert atmosphere with metal lithium sheet, measures the front and back ionic conductivity of contact Variation, it is specific as shown in Fig. 5, from attached drawing 5 as can be seen that doping 5wt%WO3Li1.3Al0.3Ti1.7(PO4)3Conductor material Ionic conductivity change rate is only 17% or so, compared to undoped WO in embodiment 13The ionic conductivity of material 62% changes Rate has an apparent improvement, Ti in material4+Obviously weaken with the redox condition of lithium metal.
Embodiment 7
In solid lithium ion conductors material Li1.3Al0.3Ti1.7(PO4)3Middle doping 6wt%WO3, preparation method and embodiment 2 It is identical.
The coin sample of gained is smeared into silver paste, affixes filamentary silver, impedance is measured with electrochemical workstation and calculates ion Conductivity and lithium ion transference number, testing result are specifically as shown in Fig. 3；Statistics indicate that doping 6wt%WO3's Li1.3Al0.3Ti1.7(PO4)3Total ionic conductivity is 4.18 × 10 to conductor material at room temperature-4S/cm, than undoped WO3With And it is doped with 1wt%, 2wt%, 3wt%, 4wt%, WO3Material electric conductivity increase, but with than being doped with 5wt%WO3 Material compare, conductivity is begun to decline, illustrate optimum doping amount be 5wt%；Lithium ion transference number is 0.99, is illustrated made Standby material is pure Lithium Ionic Conducting Materials.

Claims (6)

1. a kind of solid lithium ion conductors material for resisting lithium metal contact reduction, which is characterized in that the conductor material is profit Use metal ions M6+Doping contains Ti4+Solid lithium ion conductors material；The metal ions M6+For W6+、Cr6+、Mo6+Or Mn6+ One or more of.
2. conductor material according to claim 1, which is characterized in that described to contain Ti4+Solid lithium ion conductors material be NASICON types Li1+xAlxTi2-x(PO4)3Or Ca-Ti ore type Li3yLa2/3-yTiO3, wherein 0 ＜ x ＜, 2,0 ＜ y ＜ 0.16.
3. conductor material according to claim 1, which is characterized in that the metal ions M6+In the form of metal oxide It is doped, doping is 0wt%~10wt%.
4. conductor material according to claim 1, which is characterized in that the metal ions M6+Doping be 5wt%.
5. according to the preparation method of conductor material described in claim 1-4, which is characterized in that the preparation method includes following step Suddenly：
(1) raw material is weighed, uniformly mixes after grinding, is calcined in Muffle furnace；
(2) after the completion of calcining, after taking out, being fully ground, with tablet press machine compression moulding；
(3) material of compression moulding is subjected to solid-phase sintering using Muffle furnace.
6. preparation method according to claim 5, which is characterized in that calcination temperature is 400~700 DEG C in the step (1), Calcination time is 2h；Sintering temperature is 950 DEG C -1100 DEG C in the step (3), soaking time 4h.
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