CN114295658B - Detection method of solid electrolyte lithium lanthanum zirconium oxygen LLZO material - Google Patents
Detection method of solid electrolyte lithium lanthanum zirconium oxygen LLZO material Download PDFInfo
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Abstract
The embodiment of the invention relates to a detection method of a solid electrolyte lithium lanthanum zirconium oxygen LLZO material. The detection method comprises the following steps: grinding LLZO powder material to be detected, and sieving with 200-400 meshes; taking sieved LLZO powder according to a preset first mass, and soaking the LLZO powder into deionized water of a second mass; soaking for 24-48 hr, filtering with filter paper, collecting filtrate, and testing Li in filtrate with inductively coupled plasma ICP emission spectrometer + Content, measured content m1; in addition, the sieved LLZO powder is taken according to the first mass, put into a mixed acid solution with the second mass, the LLZO powder is digested by microwaves, and Li in the digestion solution is tested by an ICP emission spectrometer + Content, measured content m2; and determining whether tetragonal phase impurities exist in the LLZO powder material to be detected according to the ratio of m1 to m 2.
Description
Technical Field
The invention relates to the technical field of material detection, in particular to a detection method of a solid electrolyte lithium lanthanum zirconium oxygen LLZO material.
Background
Currently, the main current solid electrolyte materials can be divided into three main categories, oxide, sulfide and polymer. Among them, oxides are receiving a great deal of attention because of their stability to air and high ionic conductivity.
Garnet-type oxide solid state electrolyte material Lithium Lanthanum Zirconium Oxide (LLZO) is considered one of the most ideal solid state electrolyte materials for solid state batteries because of its excellent ionic conductivity and readily available raw materials. Since garnet-type LLZO is divided into two phase structures of a cubic phase and a tetragonal phase, wherein the ionic conductivity of the cubic phase can reach 0.1-1ms/m, but the ionic conductivity of the tetragonal phase is extremely low. Therefore, in practical research applications and production processes, the cubic phase of LLZO is mainly used.
In the LLZO sintering process, the phase forming condition is harsh due to the complex composition of the material. In the actual sintering process, tetragonal phase impurity phase also appears, and the influence on the material performance is larger. Phase detection of LLZO becomes necessary.
At present, a commonly adopted detection method for phase detection of LLZO is an X-ray diffraction (XRD) method, and the phase of LLZO is tested by X-ray diffraction, so that the impurity phase composition in the LLZO is analyzed.
However, using XRD as a method for detecting the LLZO phase composition has the following two drawbacks:
1. the sensitivity of XRD to perform phase detection is 1%, and when the content of the impurity phase is lower than 1%, the XRD cannot detect the existence of the impurity phase;
2. when phase analysis is performed by XRD, only the hetero-phase can be qualitatively analyzed, and the specific composition of the cubic phase and the tetragonal phase in LLZO cannot be quantitatively analyzed.
Disclosure of Invention
The invention aims to provide a detection method of a solid electrolyte lithium lanthanum zirconium oxygen LLZO material, which can accurately measure the ratio of the neutral phase to the tetragonal phase in LLZO powder.
Therefore, the embodiment of the invention provides a detection method of a solid electrolyte lithium lanthanum zirconium oxygen LLZO material, which comprises the following steps:
the detection method comprises the following steps:
grinding LLZO powder material to be detected, and sieving with 200-400 meshes;
taking sieved LLZO powder according to a preset first mass, and soaking the LLZO powder into deionized water of a second mass;
soaking for 24-48 hr, filtering with filter paper, collecting filtrate, and testing Li in filtrate with inductively coupled plasma ICP emission spectrometer + Content, measured content m1;
in addition, the sieved LLZO powder is taken according to the first mass, put into a mixed acid solution with the second mass, the LLZO powder is digested by microwaves, and Li in the digestion solution is tested by an ICP emission spectrometer + Content, measured content m2;
and determining whether tetragonal phase impurities exist in the LLZO powder material to be detected according to the ratio of m1 to m 2.
Preferably, the first mass is in the range of 0.1g-10g; the second mass ranges from 100 to 500g.
Preferably, the ratio of the first mass to the second mass is 1:20.
preferably, the mixed acid solution specifically comprises: concentrated nitric acid HNO according to volume ratio 3 Concentrated HCl: mixed acid solution of hf=4:12:1 configuration.
Preferably, determining whether the tetragonal phase is present in the LLZO powder material to be measured according to the ratio of m1 to m2 specifically includes:
when the ratio of m1 to m2 is equal to Li in the cubic phase LLZO of the first mass + /H + Exchanged Li + When the ratio of the amount to m2 is determined, determining that LLZO in the LLZO powder material to be detected is in a cubic phase, and no tetragonal phase is present;
when the ratio of m1 to m2 is smaller than Li in the cubic phase LLZO of the first mass + /H + Exchanged Li + And when the ratio of the amount to m2 is determined, determining that tetragonal phase impurities exist in the LLZO powder material to be detected.
Preferably, determining whether the tetragonal phase is present in the LLZO powder material to be measured according to the ratio of m1 to m2 specifically includes:
if m 1/m2=64%, determining that LLZO in the LLZO powder material to be detected is a cubic phase, and no tetragonal phase is present;
if m1/m2 is less than 64%, determining that the LLZO in the LLZO powder material to be detected has tetragonal phase.
Preferably, after determining whether the LLZO powder material to be tested has the tetragonal phase, the method further includes:
when it is determined that tetragonal phase is present in the LLZO powder material to be measured, the ratio of tetragonal phase of the LLZO powder material to be measured is calculated according to [ (0.64 m2-m 1)/(0.64 m 2) ]. Times.100%.
The detection method of the solid electrolyte lithium lanthanum zirconium oxygen LLZO material provided by the embodiment of the invention can accurately measure the occupancy rate of tetragonal phase impurity phases in cubic phase LLZO powder. The method example uses Li in cubic LLZO and tetragonal LLZO + /H + Not only can detect the tetragonal phase proportion of which the impurity phase content is lower than 1 percent, the tetragonal phase impurity content in the cubic phase can be quantified even to the ppm level. The method has high detection precision and can be used for quantification, and a high-precision, simple and feasible scheme is provided for detecting the LLZO phase composition.
Drawings
Fig. 1 is a flowchart of a method for detecting a solid electrolyte Lithium Lanthanum Zirconium Oxide (LLZO) material according to an embodiment of the present invention.
Detailed Description
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
The embodiment of the invention provides a detection method of a solid electrolyte Lithium Lanthanum Zirconium Oxide (LLZO) material, the main steps of which are shown in figure 1, and the detection method can be implemented according to the following steps:
preferably, the first mass is in the range of 0.1g-10g; the second mass ranges from 100 to 500g.
More preferably, the first mass and the second mass are in the above range according to a ratio of 1:20.
preferably, the mixed acid solution is specifically: concentrated nitric acid HNO according to volume ratio 3 Concentrated HCl: mixed acid solution of hf=4:12:1 configuration.
And step 150, determining whether tetragonal phase impurities exist in the LLZO powder material to be detected according to the ratio of m1 to m 2.
Wherein when the ratio of m1 to m2 is equal to Li in the cubic phase LLZO of the first mass + /H + Exchanged Li + When the ratio of the amount to m2 is determined, determining that LLZO in the LLZO powder material to be detected is in a cubic phase, and no tetragonal phase is present; when the ratio of m1 to m2 is smaller than Li in the cubic phase LLZO of the first mass + /H + Exchanged Li + Quantity and mAnd 2, determining that the LLZO in the LLZO powder material to be detected has tetragonal phase.
The method utilizes Li in cubic phase LLZO and tetragonal phase LLZO + /H + The detection is realized by different ion exchange degrees.
Specifically, the garnet-type solid electrolyte material LLZO has two phase structures-a cubic phase and a tetragonal phase. The tetragonal phase space group is No.142I41/acd, and the unit cell parameters are
Space group of cubic phase is No.230Ia3d, unit cell parameter is +.>
The frames of the two crystal structures are identical, 8 coordinated [ LaO8 ]]Hexahedral and 6-coordinated [ ZrO 6]]A framework of octahedra. The difference is that li+ occupies different sites in the crystal structure.
In the tetragonal phase structure, lithium ions are distributed at three positions, namely tetrahedral voids 8a (Li 1), regular octahedral voids 16f (Li 2), and regular octahedral voids 32g (Li 3), with a space occupation ratio of 1. In the cubic phase structure, lithium ions are distributed at two positions, namely tetrahedral voids (24 d) and eccentric octahedral voids (96 h). Wherein the Li1 occupancy of 24d in the [ LiO4] tetrahedral position is 0.94 and the Li2 occupancy of 96h in the [ LiO6] octahedral position is 0.349.
Cubic phase LLZO is essentially a metastable phase of lithium ion disorder, whereas tetragonal phase LLZO is stable. Due to Li in cubic LLZO + And H is + Has strong ion exchange reaction, and at room temperature, cubic LLZO and water in air can generate Li + And H is + Is a function of the exchange of (a). Due to the tetragonal LLZO, li + The occupation ratios of (2) are 1, so Li + /H + Is 0. This difference phenomenon exists mainly due to the crystal structure of the cubic phase and the crystal junction of the tetragonal phaseThe difference in structure results in different degrees of ion exchange reaction of Li+/H+.
In cubic LLZO, li1 sites account for total Li + 36% of the number, li2 sites account for total Li + 25% of the number, li3 sites account for total Li + 39% of the number. According to Li1, li2, li3 different sites Li + The degree of exchange of H+ varies, and Li occurs + /H + During exchange, li of Li2 site and Li3 site + Will be completely replaced by H+, i.e. 64% Li in the cubic LLZO + Is replaced by H + . Whereas tetragonal LLZO is stable in structure and therefore Li + /H + Is 0.
Thus, in the above step, the measured content m1 corresponds to Li2 sites and Li3 sites of the cubic phase LLZO present in the LLZO powder material to be measured of the first mass + Is a combination of the amounts of (a) and (b). I.e. Li in the cubic phase LLZO of the first mass + /H + Exchanged Li + Amount of the components.
In the digestion process in the mixed acid solution, all Li in the LLZO powder material to be measured with the first quality is converted into Li + I.e. the measured content m2 corresponds to Li of all LLZO in the LLZO powder material to be measured of the first quality + Is a combination of the amounts of (a) and (b).
If only cubic LLZO exists in the LLZO powder material to be measured, the content m1 corresponds to 64% of Li + The content m2 is 100% of Li + 。
If not only cubic phase LLZO but also tetragonal phase LLZO exists in the LLZO powder material to be measured, the content m1 is necessarily less than 64% of Li + Li of which the content m2 is still 100% + 。
Therefore, in the above-mentioned determination in step 150, it can be considered that if m 1/m2=64%, it is determined that LLZO in the LLZO powder material to be measured is cubic phase, and there is no tetragonal phase; if m1/m2 is less than 64%, determining that the LLZO in the LLZO powder material to be detected has tetragonal phase.
Further, after determining whether the LLZO powder material to be detected has the tetragonal phase, the detection method of the present invention further includes quantifying the tetragonal phase, which is specifically as follows:
when it is determined that tetragonal phase impurities exist in the LLZO powder material to be measured, the ratio of tetragonal phase of the LLZO powder material to be measured is calculated according to [ (0.64×m2-m 1)/(0.64×m2) ]×100%. The allowable error fluctuation range is 64% ± 0.5%.
This is because 64%. Times.m2 is Li in the intrinsic cubic phase LLZO + /H + Exchanged Li + The amount of Li actually exchanged, however, is due to the presence of tetragonal phase LLZO + The amount of Li is reduced by (0.64×m2-m 1) + The amount is in tetragonal phase LLZO.
The square phase LLZO has a ratio of [ (0.64×m2-m 1)/(0.64×m2) ] ×100%, and the remainder is the ratio of the cubic phase LLZO.
In order to better understand the technical solution of the present invention, the following description will be given with some specific examples.
Example 1
The LLZO powder A to be tested was ground and sieved through a 200 mesh screen.
0.2g of the sieved LLZO powder was taken and immersed in 150g of deionized water. After 24 hours of soaking, the powder was filtered off using filter paper, the filtrate was taken, and Li in the filtrate was tested using ICP + Content m1, m1=49 mg/L was measured.
Then 0.2g of sieved LLZO powder is taken and put into concentrated nitric acid HNO 3 Concentrated HCl: in a mixed acid solution with HF=4:12:1 ratio, the LLZO powder is digested by microwaves. Testing Li in digestion solution using ICP + Content m2, m2=77 mg/L was measured.
Comparing Li+ content of m1 and m2, and m1/m2 is approximately equal to 64%, wherein the tested LLZO materials are considered to be cubic phase LLZO, and tetragonal phase LLZO impurity phases are not generated.
Example 2
The LLZO powder B to be tested was ground and sieved through a 200 mesh screen.
0.2g of the sieved LLZO powder was taken and immersed in 150g of deionized water. After 24 hours of soaking, the powder was filtered off using filter paper, the filtrate was taken, and Li in the filtrate was tested using ICP + Content m1, m1=30 mg/L was measured.
0.2g of sieved L is taken againLZO powder is put into concentrated nitric acid HNO 3 Concentrated HCl: in a mixed acid solution with HF=4:12:1 ratio, the LLZO powder is digested by microwaves. Testing Li in digestion solution using ICP + Content m2, m2=77 mg/L was measured.
Comparing the li+ content of m1 to m2, m1/m2= 38.96% < 64%, it is considered that part of tetragonal phase LLZO impurity exists in the tested LLZO material, and the amount of tetragonal phase impurity is 39.1234% according to calculation.
Example 3
The LLZO powder to be tested was ground and screened through a 200 mesh screen.
0.1g of the sieved LLZO powder was taken and immersed in 100g of deionized water. After 28 hours of soaking, the powder was filtered off using filter paper, the filtrate was taken, and the li+ content m1 in the filtrate was tested using ICP, to measure m1=22 mg/L.
Then 0.1g of sieved LLZO powder is taken and put into concentrated nitric acid HNO 3 Concentrated HCl: in a mixed acid solution with HF=4:12:1 ratio, the LLZO powder is digested by microwaves. Testing Li in digestion solution using ICP + Content m2, m2=39 mg/L was measured.
Comparing Li+ content of m1 and m2, and considering that m1/m2 is approximately equal to 56.41 percent and less than 64 percent, partial tetragonal phase LLZO impurity phase exists in the tested LLZO material, and according to calculation, the content of the tetragonal phase impurity is 11.8590 percent
The detection method of the solid electrolyte lithium lanthanum zirconium oxygen LLZO material provided by the embodiment of the invention can accurately measure the occupancy rate of tetragonal phase impurity phases in cubic phase LLZO powder. The method example uses Li in cubic LLZO and tetragonal LLZO + /H + Not only can detect the tetragonal phase proportion of which the impurity phase content is lower than 1 percent, the tetragonal phase impurity content in the cubic phase can be quantified even to the ppm level. The method has high detection precision and can be used for quantification, and a high-precision, simple and feasible scheme is provided for detecting the LLZO phase composition.
Those of skill would further appreciate that the various illustrative elements and algorithm steps described in connection with the embodiments disclosed herein may be implemented as electronic hardware, computer software, or combinations of both, and that the various illustrative elements and steps are described above generally in terms of function in order to clearly illustrate the interchangeability of hardware and software. Whether such functionality is implemented as hardware or software depends upon the particular application and design constraints imposed on the solution. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present invention.
The steps of a method or algorithm described in connection with the embodiments disclosed herein may be embodied in hardware, in a software module executed by a processor, or in a combination of the two. The software modules may be disposed in Random Access Memory (RAM), memory, read Only Memory (ROM), electrically programmable ROM, electrically erasable programmable ROM, registers, hard disk, a removable disk, a CD-ROM, or any other form of storage medium known in the art.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (7)
1. A method for detecting a solid electrolyte lithium lanthanum zirconium oxygen LLZO material, which is characterized by comprising the following steps:
grinding the LLZO powder material to be detected and sieving the LLZO powder material with a 200-400-mesh sieve;
taking sieved LLZO powder according to a preset first mass, and soaking the LLZO powder into deionized water of a second mass;
soaking for 24-48 hr, filtering with filter paper, collecting filtrate, and testing Li in filtrate with inductively coupled plasma ICP emission spectrometer + Content, measured content m1;
in addition, the sieved LLZO powder is taken according to the first mass and put into a mixed acid solution with the second mass for microwave digestionLLZO powder and Li in digestion solution was tested by ICP emission spectrometer + Content, measured content m2;
and determining whether tetragonal phase impurities exist in the LLZO powder material to be detected according to the ratio of m1 to m 2.
2. The method of claim 1, wherein the first mass is in the range of 0.1g-10g; the second mass ranges from 100 to 500g.
3. The method of claim 2, wherein the ratio of the first mass to the second mass is 1:20.
4. the detection method according to claim 1, wherein the mixed acid solution specifically comprises: concentrated nitric acid HNO according to volume ratio 3 Concentrated HCl: mixed acid solution of hf=4:12:1 configuration.
5. The detection method according to claim 1, wherein determining whether the LLZO powder material to be detected has a tetragonal phase according to the ratio of m1 to m2 specifically includes:
when the ratio of m1 to m2 is equal to Li in the cubic phase LLZO of the first mass + /H + Exchanged Li + When the ratio of the amount to m2 is determined, determining that LLZO in the LLZO powder material to be detected is in a cubic phase, and no tetragonal phase is present;
when the ratio of m1 to m2 is smaller than Li in the cubic phase LLZO of the first mass + /H + Exchanged Li + And when the ratio of the amount to m2 is determined, determining that tetragonal phase impurities exist in the LLZO powder material to be detected.
6. The detection method according to claim 1, wherein determining whether the LLZO powder material to be detected has a tetragonal phase according to the ratio of m1 to m2 specifically includes:
if m 1/m2=64%, determining that LLZO in the LLZO powder material to be detected is a cubic phase, and no tetragonal phase is present;
if m1/m2 is less than 64%, determining that the LLZO in the LLZO powder material to be detected has tetragonal phase.
7. The method of claim 1, 5 or 6, wherein after said determining whether tetragonal phase is present in the LLZO powder material to be tested, the method further comprises:
when it is determined that tetragonal phase is present in the LLZO powder material to be measured, the ratio of tetragonal phase of the LLZO powder material to be measured is calculated according to [ (0.64 m2-m 1)/(0.64 m 2) ]. Times.100%.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010143785A (en) * | 2008-12-18 | 2010-07-01 | National Institute Of Advanced Industrial Science & Technology | Lithium ion conductive oxide, producing method of the same and solid electrolyte constituted by the oxide |
| CN104628381A (en) * | 2013-11-12 | 2015-05-20 | 现代自动车株式会社 | Method for preparing aluminum substituted garnet |
| CN105742699A (en) * | 2014-12-30 | 2016-07-06 | 现代自动车株式会社 | Garnet solid electrolyte and method for preparing the same |
| CN109540874A (en) * | 2018-12-14 | 2019-03-29 | 蜂巢能源科技有限公司 | The method for detecting inorganic element content in the sample of lithium lanthanum zirconium oxygen type solid electrolyte |
| CN110128140A (en) * | 2019-04-29 | 2019-08-16 | 内蒙古工业大学 | A kind of ytterbium aluminium codope carbuncle type Li7La3Zr2O12Lithium Ionic Conducting Materials and preparation method thereof |
| CN111732432A (en) * | 2020-06-30 | 2020-10-02 | 上海国瓷新材料技术有限公司 | Spherical lithium lanthanum zirconium oxygen powder material and composite solid electrolyte prepared from same |
| CN113130976A (en) * | 2019-12-30 | 2021-07-16 | 天津国安盟固利新材料科技股份有限公司 | Garnet type solid electrolyte and preparation method thereof |
-
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- 2021-12-10 CN CN202111508587.3A patent/CN114295658B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010143785A (en) * | 2008-12-18 | 2010-07-01 | National Institute Of Advanced Industrial Science & Technology | Lithium ion conductive oxide, producing method of the same and solid electrolyte constituted by the oxide |
| CN104628381A (en) * | 2013-11-12 | 2015-05-20 | 现代自动车株式会社 | Method for preparing aluminum substituted garnet |
| CN105742699A (en) * | 2014-12-30 | 2016-07-06 | 现代自动车株式会社 | Garnet solid electrolyte and method for preparing the same |
| CN109540874A (en) * | 2018-12-14 | 2019-03-29 | 蜂巢能源科技有限公司 | The method for detecting inorganic element content in the sample of lithium lanthanum zirconium oxygen type solid electrolyte |
| CN110128140A (en) * | 2019-04-29 | 2019-08-16 | 内蒙古工业大学 | A kind of ytterbium aluminium codope carbuncle type Li7La3Zr2O12Lithium Ionic Conducting Materials and preparation method thereof |
| CN113130976A (en) * | 2019-12-30 | 2021-07-16 | 天津国安盟固利新材料科技股份有限公司 | Garnet type solid electrolyte and preparation method thereof |
| CN111732432A (en) * | 2020-06-30 | 2020-10-02 | 上海国瓷新材料技术有限公司 | Spherical lithium lanthanum zirconium oxygen powder material and composite solid electrolyte prepared from same |
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