CN105633392A - Nano lithium-lanthanum-titanium oxide material and preparation method and application thereof - Google Patents
Nano lithium-lanthanum-titanium oxide material and preparation method and application thereof Download PDFInfo
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- CN105633392A CN105633392A CN201410612714.8A CN201410612714A CN105633392A CN 105633392 A CN105633392 A CN 105633392A CN 201410612714 A CN201410612714 A CN 201410612714A CN 105633392 A CN105633392 A CN 105633392A
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Abstract
The invention relates to a nano lithium-lanthanum-titanium oxide material. The nano lithium-lanthanum-titanium oxide material is characterized in that a chemical formula of the nano lithium-lanthanum-titanium oxide material is Li3xLa2/3-xTiO3, wherein x is smaller than 0.16 and greater than 0; and the particle sizes of the nano lithium-lanthanum-titanium oxide material do not exceed 100nm. The nano lithium-lanthanum-titanium oxide material can be directly used for preparing a solid electrolyte film. The solid electrolyte film prepared by the nano lithium-lanthanum-titanium oxide material is applied to a lithium-ion battery and has the advantage of low grain boundary resistance.
Description
Technical field
The application relates to a kind of nanometer lithium lanthanum titanium oxide material, its preparation method and application, belongs to all-solid lithium-ion battery field.
Background technology
Lithium ion battery has been widely used for most electronic product, is applied to electric automobile including as large-scale energy storage device. At present, widely used lithium ion battery adopts liquid electrolyte mostly. There is hidden danger in liquid electrolyte, injured the application of lithium ion battery in safety. Inorganic solid electrolyte has the advantages such as security performance is good, have extended cycle life, energy density is high, high-temperature adaptability is good, it is possible to fundamentally solve the safety problem of lithium ion battery.
Lithium lanthanum titanium oxide is the one of inorganic solid electrolyte, has electrical conductivity height, synthesizes the advantages such as simple. Lithium lanthanum titanium oxide chemical formula is Li3xLa2/3-xTiO3, wherein 0 < x < 0.16. Under its room temperature, electrical conductivity can reach 10-3S/cm, can be used to replace liquid electrolyte in theory.
The lithium lanthanum titanium oxide granule of super-small is possible not only to prepare into ultra-thin solid electrolyte film, and can reduce the grain boundary resistance that bulky grain electrolyte brings. The preparation method of Li-La-Ti oxygen the earliest is solid sintering technology, it is necessary to high temperature sintering, not only consumes energy, and crystallite dimension is very big, and application also needs to later stage process, complex steps. Although general sol-gel process can prepare nano level Li-La-Ti oxygen granule, but cannot realize extra small size easily.
Summary of the invention
An aspect according to the application, it is provided that a kind of nanometer lithium lanthanum titanium oxide material, particle size is nanoscale, can be directly used for preparing solid electrolyte film. Compared with general lithium lanthanum titanium oxide material, what adopt the solid electrolyte film prepared of the application nanometer lithium lanthanum titanium oxide material has the advantages that grain boundary resistance is low.
Described nanometer of lithium lanthanum titanium oxide material, it is characterised in that the chemical formula of described nanometer of lithium lanthanum titanium oxide material is Li3xLa2/3-xTiO3, 0 < x < 0.16; The particle diameter of described nanometer of lithium lanthanum titanium oxide material is less than 100nm.
Preferably, the particle size range upper limit of described nanometer of lithium lanthanum titanium oxide material is optionally from 100nm, 90nm, 80nm, 70nm, 60nm, 50nm, and lower limit is optionally from 10nm, 20nm, 30nm. It is further preferred that the particle diameter of described nanometer of lithium lanthanum titanium oxide material is 10nm��100nm. It is further preferred that the particle diameter of described nanometer of lithium lanthanum titanium oxide material is 30nm��80nm. It is further preferred that the particle diameter of described nanometer of lithium lanthanum titanium oxide material is 20nm��50nm.
Preferably, described nanometer of lithium lanthanum titanium oxide material is Li0.35La0.55TiO3And/or Li0.5La0.5TiO3, particle diameter is 10��80nm.
Described lithium lanthanum titanium oxide is also known as lanthanium titanate lithium (being abbreviated as LLTO), for having the compound of perovskite structure or similar structures.
Another aspect according to the application, it is provided that a kind of method preparing described nanometer lithium lanthanum titanium oxide material, it is characterised in that containing following steps:
A) by titanium source, lithium source, lanthanum source, solvent, dispersant, the colloidal sol with following molar ratio is obtained:
Ti:Li:La: solvent: dispersant=1:0.25��1:0.5��0.8:50��250:0.25��2;
B) step a) gained colloidal sol ageing is obtained gel;
C) step b) gained gel drying, grinding, sintering curing obtain described nanometer lithium lanthanum titanium oxide material.
Titanium source described in step a) is selected from the organic compound containing titanium elements and/or inorganic compound. Preferably, described titanium source at least one in titanate compound.
Molar ratio in the described colloidal sol of step a), Ti is the molal quantity of titanium elements in colloidal sol; Li is the molal quantity of elemental lithium in colloidal sol; La is the molal quantity of lanthanum element in colloidal sol; Solvent is the molal quantity of solvent; Dispersant is the molal quantity of dispersant.
It is further preferred that described titanate compound is selected from least one having in the compound of the chemical structural formula as shown in Formulas I:
It is further preferred that R in described Formulas I1, R2, R3, R4It is the alkyl of 1��10 independently selected from any carbon number. Described alkyl is linear paraffin or branched paraffin loses the group that any hydrogen atom is formed.
It is further preferred that R in described Formulas I1, R2, R3, R4For identical alkyl.
It is further preferred that titanium source described in step a) is butyl titanate and/or isopropyl titanate.
Lithium source described in step a) is selected from the organic compound containing elemental lithium and/or inorganic compound. Preferably, described lithium source at least one in inorganic lithium salt, carboxylic acid lithium salt, alcohol lithium compound.
Preferably, described inorganic lithium salt is lithium nitrate and/or lithium chloride.
Preferably, described carboxylic acid lithium salt is R selected from molecular formula5At least one in the compound of COOLi, R5It is the alkyl of 1��10 for any carbon number. It is further preferred that R5It is the alkyl of 1��5 for any carbon number.
Preferably, described alcohol lithium compound is R selected from molecular formula6At least one in the compound of OLi, R6It is the alkyl of 1��10 selected from any carbon number.
Preferably, described lithium source at least one in lithium nitrate, lithium chloride, lithium methoxide, lithium ethoxide, Quilonorm (SKB), tert-butyl alcohol lithium, tert-pentyl alcohol lithium. It is further preferred that described lithium source is Quilonorm (SKB) and/or lithium nitrate.
Lanthanum source described in step a) is selected from the organic compound containing lanthanum element and/or inorganic compound. Preferably, described lanthanum source at least one in inorganic lanthanum salt. It is further preferred that described lanthanum source is Lanthanum (III) nitrate and/or lanthanum chloride. It is further preferred that described lanthanum source is Lanthanum (III) nitrate.
Preferably, at least one in organic alcohols solvent of the solvent described in step a). It is further preferred that described solvent is R selected from molecular formula7At least one in the alcohol compound of OH, R7It is the alkyl of 1��10 selected from any carbon number. It is further preferred that described solvent is isopropanol.
Preferably, described dispersant at least one in the organic compound containing acetyl group. It is further preferred that at least one that described dispersant is in ethyl acetate, acetylacetone,2,4-pentanedione, ethyl acetoacetate.
Preferably, the molar ratio in colloidal sol described in step a) is Ti:Li:La: solvent: dispersant=1:0.3��0.6:0.4��0.6:60��70:0.25��1.
Preferably, the molar ratio in described colloidal sol is Ti:Li:La: solvent: dispersant=1:0.5��0.6:0.5��0.6:65��75:0.25��0.6.
Preferably, the molar ratio of the titanium elements in colloidal sol described in step a), elemental lithium and lanthanum element is Ti:Li:La=2:1:1.
It is further preferred that the time of ageing described in step b) was no less than 1 hour. It is further preferred that the time of ageing described in step b) is 1��48 hour. It is further preferred that described digestion time is 8��48 hours.
Preferably, the temperature of ageing described in step b) is 10��50 DEG C. It is further preferred that described Aging Temperature is 25��35 DEG C. Further preferred, described Aging Temperature is room temperature.
Dry described in step c) and oven for drying can be directly placed into for sample, it is also possible to for vacuum drying. Preferably, dry described in step b) temperature is 50 DEG C��150 DEG C. Further preferentially, baking temperature range limit described in step c) is optionally from 150 DEG C, 120 DEG C, 100 DEG C, and lower limit is optionally from 50 DEG C, 60 DEG C, 70 DEG C.
Preferably, drying time described in step c) is 1��20 hour. It is further preferred that upper limit drying time described in step c) is optionally from 20 hours, 16 hours, 15 hours or 10 hours, lower limit is optionally from 1 hour or 2 hours. It is further preferred that drying time described in step c) is 1��10 hour.
Preferably, the temperature of the described sintering curing of step c) is 300 DEG C��1000 DEG C, and the time was no less than 1 hour. It is further preferred that the temperature range upper limit of described sintering curing is optionally from 900 DEG C, 800 DEG C, 700 DEG C, 650 DEG C, 600 DEG C, 550 DEG C, lower limit is optionally from 300 DEG C, 350 DEG C, 400 DEG C. It is further preferred that the temperature of described sintering curing is 300 DEG C��650 DEG C, the time is 1��24 hour. It is further preferred that the temperature of described sintering curing is 400 DEG C��650 DEG C, the time is 1��12 hour. Described sintering curing, it is possible to select a certain temperature in said temperature scope to carry out Isothermal sinter solidification; In described temperature range, the temperature match curing conditions such as temperature programming can also be adopted to be sintered solidifying.
Another aspect according to the application, it is provided that a kind of lithium ion battery, it is characterised in that containing any of the above-described nanometer of lithium lanthanum titanium oxide material and/or nanometer lithium lanthanum titanium oxide material for preparing according to any of the above-described method. Any of the above-described nanometer of lithium lanthanum titanium oxide material and/or nanometer lithium lanthanum titanium oxide material prepared according to any of the above-described method, there is nano-grade size, can be directly used for the preparation of solid electrolyte film in lithium ion battery, there is the advantage that grain boundary resistance is low.
Described lithium ion battery comprises anode pole piece, cathode pole piece, isolating membrane and solid electrolyte film; Described solid electrolyte film contains any of the above-described nanometer of lithium lanthanum titanium oxide material and/or nanometer lithium lanthanum titanium oxide material prepared according to any of the above-described method.
Herein described technical scheme includes following beneficial effect:
(1) herein described method sintering curing temperature is low, and energy consumption is low, safety is high, is suitable for large-scale industrial production.
(2) described herein nanometer of lithium lanthanum titanium oxide scantling is nanoscale, and without ball-milling treatment, is directly obtained by preparation method, and step is simple.
(3) the application adopts raw material and reagent all commercially, are suitable for large-scale production.
(4) repeatability of herein described method is good, and productivity is high.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of sample 2#.
Fig. 2 is the stereoscan photograph of sample 2#.
Fig. 3 is the transmission electron microscope photo of sample 2#.
Detailed description of the invention
Below in conjunction with drawings and Examples, the application is expanded on further. Should be understood that these drawings and Examples are merely to illustrate the application rather than restriction scope of the present application.
When not doing specified otherwise, in embodiment, the particle size distribution range of sample and volume average particle size all record on Malvern laser particle analyzer.
Embodiment 1 sample 1#��sample 6#Preparation and granulometry
In beaker, add solvent, under agitation, be added dropwise over dispersant, stir 10min, add 1mol titanium source, stir 30min, be sequentially added into lanthanum source, lithium source, to be dissolved completely after, ageing a period of time, drying, grind after, sintering curing.
Gained sample 1#��sample 6#The kind of numbering and raw material and the relation of proportioning, aging condition, drying condition and sintering curing condition as shown in Table 1 below. On Malvern laser particle analyzer, the granularity of gained sample being detected, testing result refers to table 1 data.
Table 1
The XRD of embodiment 2 sample characterizes
To sample 1 on BrukerD8Advance type X-ray diffractometer#��sample 6#Crystal structure characterize, result shows, gained sample is lithium lanthanum titanium oxide material. With sample 2#For Typical Representative, its XRD spectra is as it is shown in figure 1, the XRD spectra of other samples and sample 2#Close, namely the peak position of diffraction maximum is essentially identical, the strong slightly difference in the peak of each diffraction maximum.
The SEM of embodiment 3 sample characterizes
To sample 1 in HITACHIS4800 type scanning electron microscope#��sample 6#Pattern characterize, result shows, sample is the granule of nano-scale and uniform particle sizes. With sample 2#For Typical Representative, its stereoscan photograph is as shown in Figure 2.
The TEM of embodiment 4 sample characterizes
On FEITecnaiF20 type transmission electron microscope, sample 2# being characterized, result is as shown in Figure 3. As seen from the figure, sample is nano-sized particles, and particle size distribution, at 10-50nm, several is distributed in about 20nm.
The ICP of embodiment 5 sample characterizes
To sample 1 on Perkin-ElmerOptima2100 type inductive coupling plasma emission spectrograph#��sample 6#Composition be analyzed, result is as shown in table 2.
Table 2
| Sample number into spectrum | The elementary composition analysis result of product |
| 1# | Li0.5La0.5TiO3 |
| 2# | Li0.35La0.55TiO3 |
| 3# | Li0.35La0.55TiO3 |
| 4# | Li0.35La0.55TiO3 |
| 5# | Li0.35La0.55TiO3 |
| 6# | Li0.375La0.505TiO3 |
The foregoing is only the preferred embodiment of the application, be not limited to the application, for a person skilled in the art, the application can have various modifications and variations. All within spirit herein and principle, any amendment of making, equivalent replacement, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. one kind of nanometer of lithium lanthanum titanium oxide material, it is characterised in that the chemical formula of described nanometer of lithium lanthanum titanium oxide material is Li3xLa2/3-xTiO3, 0 < x < 0.16; The particle diameter of described nanometer of lithium lanthanum titanium oxide material is less than 100nm.
2. according to claim 1 nanometer of lithium lanthanum titanium oxide material, it is characterised in that described nanometer of lithium lanthanum titanium oxide material is Li0.35La0.55TiO3And/or Li0.5La0.5TiO3, particle diameter is 10��80nm.
3. the method for nanometer lithium lanthanum titanium oxide material described in preparation claim 1, it is characterised in that containing following steps:
A) by titanium source, lithium source, lanthanum source, solvent, dispersant, the colloidal sol with following molar ratio is obtained:
Ti:Li:La: solvent: dispersant=1:0.25��1:0.5��0.8:50��250:0.25��2;
B) step a) gained colloidal sol ageing is obtained gel;
C) step b) gained gel drying, grinding, sintering curing obtain described nanometer lithium lanthanum titanium oxide material.
4. method according to claim 3, it is characterised in that step a) described titanium source at least one in titanate compound; Described lithium source at least one in inorganic lithium salt, carboxylic acid lithium salt, alcohol lithium compound; Described lanthanum source at least one in inorganic lanthanum salt; Described solvent at least one in organic alcohols solvent; Described dispersant at least one in the organic compound containing acetyl group.
5. method according to claim 3, it is characterised in that titanium source described in step a) is butyl titanate and/or isopropyl titanate; Described lithium source is Quilonorm (SKB) and/or lithium nitrate; Described lanthanum source is Lanthanum (III) nitrate; Described solvent is isopropanol; Described dispersant at least one in ethyl acetate, acetylacetone,2,4-pentanedione, ethyl acetoacetate.
6. method according to claim 3, it is characterised in that the time of ageing described in step b) is 1��48 hour.
7. method according to claim 3, it is characterised in that temperature dry described in step c) is 50 DEG C��150 DEG C.
8. method according to claim 3, it is characterised in that the temperature of sintering curing described in step c) is 300 DEG C��1000 DEG C, the time no less than hour.
9. method according to claim 3, it is characterised in that the temperature of sintering curing described in step c) is 300 DEG C��650 DEG C, and the time is 1��24 hour.
10. a lithium ion battery, it is characterised in that containing nanometer lithium lanthanum titanium oxide material that nanometer lithium lanthanum titanium oxide material described in any one of claim 1��2 and/or method according to any one of claim 3��9 prepare.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107579276A (en) * | 2017-07-25 | 2018-01-12 | 华南理工大学 | A kind of solid polymer electrolyte membrane and preparation method thereof and the application as lithium ion battery barrier film |
| CN108808109A (en) * | 2018-08-21 | 2018-11-13 | 电子科技大学 | All-solid lithium-ion battery film and preparation method thereof |
| CN109056194A (en) * | 2018-07-12 | 2018-12-21 | 东华大学 | A kind of flexibility Li-La-Ti oxygen ceramic nanofibers membrane material and preparation method thereof |
| CN109103505A (en) * | 2018-08-21 | 2018-12-28 | 电子科技大学 | Stratiform all-solid lithium-ion battery and preparation method thereof |
| CN110330050A (en) * | 2019-03-25 | 2019-10-15 | 郑州大学 | A kind of Li-La-Ti oxygen material and preparation method thereof, H2S gas sensor |
| CN111463477A (en) * | 2020-03-13 | 2020-07-28 | 深圳大学 | Composite solid electrolyte with enhanced stability of fluorinated additive and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107579276A (en) * | 2017-07-25 | 2018-01-12 | 华南理工大学 | A kind of solid polymer electrolyte membrane and preparation method thereof and the application as lithium ion battery barrier film |
| CN109056194A (en) * | 2018-07-12 | 2018-12-21 | 东华大学 | A kind of flexibility Li-La-Ti oxygen ceramic nanofibers membrane material and preparation method thereof |
| CN108808109A (en) * | 2018-08-21 | 2018-11-13 | 电子科技大学 | All-solid lithium-ion battery film and preparation method thereof |
| CN109103505A (en) * | 2018-08-21 | 2018-12-28 | 电子科技大学 | Stratiform all-solid lithium-ion battery and preparation method thereof |
| CN108808109B (en) * | 2018-08-21 | 2021-06-04 | 电子科技大学 | All-solid-state lithium ion battery membrane and preparation method thereof |
| CN110330050A (en) * | 2019-03-25 | 2019-10-15 | 郑州大学 | A kind of Li-La-Ti oxygen material and preparation method thereof, H2S gas sensor |
| CN111463477A (en) * | 2020-03-13 | 2020-07-28 | 深圳大学 | Composite solid electrolyte with enhanced stability of fluorinated additive and preparation method thereof |
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Application publication date: 20160601 |