WO2019188750A1 - Procédé d'inspection - Google Patents

Procédé d'inspection Download PDF

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Publication number
WO2019188750A1
WO2019188750A1 PCT/JP2019/011995 JP2019011995W WO2019188750A1 WO 2019188750 A1 WO2019188750 A1 WO 2019188750A1 JP 2019011995 W JP2019011995 W JP 2019011995W WO 2019188750 A1 WO2019188750 A1 WO 2019188750A1
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Prior art keywords
atmosphere
sample
ionization potential
lithium secondary
secondary battery
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PCT/JP2019/011995
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English (en)
Japanese (ja)
Inventor
手嶋　勝弥
信行 是津
山田　哲也
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国立大学法人信州大学
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Priority to KR1020207027760A priority Critical patent/KR102278258B1/ko
Priority to CN201980022094.3A priority patent/CN111902977B/zh
Priority to JP2020509940A priority patent/JP6905292B2/ja
Publication of WO2019188750A1 publication Critical patent/WO2019188750A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/227—Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
    • G01N23/2273—Measuring photoelectron spectrum, e.g. electron spectroscopy for chemical analysis [ESCA] or X-ray photoelectron spectroscopy [XPS]
    • 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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • 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

Definitions

  • the present invention relates to an inspection method for inspecting a surface electronic state of a material for a lithium secondary battery.
  • Patent Document 1 describes a secondary battery inspection method for inspecting an internal short circuit of a secondary battery.
  • Lithium secondary batteries use lithium composite oxides and non-oxide powders as electrode active materials and solid electrolytes.
  • the surface of the lithium composite oxide deteriorates when exposed to the atmosphere.
  • a resistance layer may be formed on the surface by reacting with moisture in the atmosphere.
  • production of such a deterioration phenomenon causes the performance deterioration of a lithium secondary battery.
  • the crystal structure is disturbed due to generation of cation mixing or lattice defects, the battery performance is significantly deteriorated. Therefore, there is a need for an inspection method that accurately predicts the performance of a lithium secondary battery material used as a raw material for a lithium secondary battery in a short time without performing a battery test.
  • the present invention has been made in view of the above circumstances, and has a short effect on the surface electronic states such as generation of a surface resistance layer having a thickness of 10 nm from the atomic layer level and disorder of the crystal structure, which influence the performance of the lithium secondary battery material.
  • the object is to provide a method for accurately checking in time. As a result, the performance of the material for the lithium secondary battery used as the raw material for the lithium secondary battery can be accurately predicted in a short time without performing a battery test.
  • the present invention includes the following [1] to [9].
  • the first aspect of the present invention provides the inspection method described in [1].
  • An inspection method for inspecting a surface electronic state of an electrode material for a lithium secondary battery or a solid electrolyte material under atmospheric pressure, from an ionization potential specific to the electrode material for the lithium secondary battery or the solid electrolyte material An inspection method comprising an inspection step of inspecting a surface electronic state of an electrode material for a lithium secondary battery.
  • the method of the first aspect preferably includes the following features.
  • the ionization potential was judged to be lower than the ionization potential immediately after exposure to the atmosphere, and when it was judged that the ionization potential was lowered, the surface of the electrode material for the lithium secondary battery was deteriorated.
  • the present invention includes the following aspects.
  • [4] The inspection method according to [3], wherein the measurement immediately after exposure to the atmosphere is performed between 0 minutes and 5 minutes after exposure of the material to the atmosphere.
  • [5] A step of preparing an electrode material or a solid electrolyte material for a lithium secondary battery as a first sample, and performing one or more measurements by changing the exposure time of the material to the atmosphere one or more times, Obtaining one or more ionization potential values, storing the values, preparing a second sample comprising a compound having the same chemical composition as the first sample, and ionizing the second sample
  • the surface electronic state of the second sample is determined from the step of measuring the potential, the step of comparing the stored value of the first sample with the measured value of the second sample, and the comparison result.
  • [6] A measurement result of measuring the ionization potential of the lithium secondary battery electrode material or the solid electrolyte material exposed to the atmosphere, and at least one result of STEM-ADF measurement and EELS measurement of the material exposed to the atmosphere And a step of determining a surface electronic state of the material from the comparison result.
  • [7] A step of comparing the ionization potential value of the first sample exposed to the atmosphere with at least one result of the STEM-ADF measurement and the EELS measurement of the material exposed to the atmosphere. And a step of determining a surface electronic state of the material.
  • the inspection method according to [1] including a step of performing and a step of determining a surface electronic state of the material from a comparison result.
  • the second sample is a separately stored material, and the step of comparing the stored value of the first sample with the measured value of the second sample includes the second sample.
  • the inspection method according to [5] which is a step of determining whether or not the sample is usable for battery production.
  • the present invention it is possible to provide a method for accurately inspecting a surface electronic state closely related to the performance of a material for a lithium secondary battery used for a lithium secondary battery or a solid electrolyte material in a short time.
  • LiNi 0.82 Co 0.15 Al 0.03 O 2 immediately after the particles exposed to the atmosphere, and is a diagram showing the subsequent powder X-ray diffraction measurement results measured at every predetermined time.
  • LiNi 0.82 Co 0.15 Al 0.03 O 2 immediately after the particles exposed to the atmosphere, and is a view showing the measurement results of the subsequent ionization potential measured every predetermined time.
  • the present invention is an inspection method for inspecting the surface electronic state of an electrode material or a solid electrolyte material for a lithium secondary battery in the atmosphere.
  • ionization potential measurement is performed on an electrode material or a solid electrolyte material for a lithium secondary battery.
  • the ionization potential inherent to the electrode material for a lithium secondary battery or the solid electrolyte material, that is, the material itself, is measured.
  • the intrinsic ionization potential may be, for example, an ionization potential under a condition where the exposure time to the atmosphere is very short.
  • lithium secondary battery materials such as electrodes and electrolytes are inspected in a relatively short time in the atmosphere, for example, within 5 minutes per sample, without any special pretreatment. Can do.
  • “under atmospheric pressure” may mean standard atmospheric pressure, but may mean a state where no special apparatus is used for depressurization or pressurization.
  • Under air may mean under atmospheric air.
  • the ionization potential is preferably measured with an atmospheric ultraviolet photoelectron spectrometer.
  • examples of the “electrode material for a lithium secondary battery” include a positive electrode active material for a lithium secondary battery and a negative electrode active material for a lithium secondary battery.
  • a lithium composite metal oxide mainly containing one element selected from the group consisting of cobalt, nickel, manganese, and aluminum and lithium can be given. More specific examples of lithium composite metal oxides include lithium nickel cobalt aluminum composite oxide and lithium nickel manganese composite oxide.
  • the “solid electrolyte material” is a material used for the electrolyte material of an all-solid battery.
  • sulfide solid electrolyte an oxide solid electrolyte, a lithium-containing sulfide, a lithium-containing metal oxide, a lithium-containing nitride, and lithium phosphate.
  • the shape and size of the electrode material or solid electrolyte material are not particularly limited, but may be particles or lumps.
  • the ionization potential of the electrode material for a lithium secondary battery or the solid electrolyte material is measured using an atmospheric ultraviolet photoelectron spectrometer.
  • the ionization potential of the material immediately after exposure to the atmosphere is also measured in advance, and it is determined by comparing whether or not the measured ionization potential is lower than the ionization potential immediately after exposure to the atmosphere. And when it falls, it determines with deterioration having been seen on the surface of the electrode material for lithium secondary batteries.
  • the length of the exposure time can be arbitrarily set each time.
  • the exposure may be performed continuously or intermittently using one sample, and the evaluation may be performed each time a predetermined time elapses.
  • one or more samples of the same type or different types may be prepared, and evaluation may be performed by changing the conditions.
  • These data may be stored and used for comparison.
  • ionization potential data for a specific compound product when the length of exposure time is different may be measured and stored in advance for reference. Thereafter, when there is a product of the same type of compound that it is desired to determine for degradation, the ionization potential of this product may be measured and compared to the stored data.
  • an electrode material or a solid electrolyte material for a lithium secondary battery is prepared as a first sample, and the material is exposed to the atmosphere for one or more times by changing the exposure time to one or more times.
  • preparing a second sample made of a compound having the same chemical composition and / or other characteristics as the first sample measuring the ionization potential of the second sample, the stored value of the first sample, The measured values of the second sample may be compared, and the surface electronic state of the second sample may be determined from the result.
  • the sample is irradiated with ultraviolet rays while changing the energy of ultraviolet rays.
  • the range of the ultraviolet energy used for the measurement can be arbitrarily selected.
  • the number of photoelectrons emitted from the material is measured with an open counter capable of measuring electrons in the atmosphere. As a result, the ionization potential can be measured in the atmosphere.
  • the time immediately after exposing the electrode material for lithium secondary battery or the solid electrolyte material to the atmosphere is defined as 0 hour.
  • ionization potential measurement is implemented for every time set arbitrarily, for example for every hour.
  • the electrode material for the lithium secondary battery and the solid electrolyte material before the measurement can be stored so as not to be exposed to the atmosphere.
  • the ionization potential at 0 hour increases by 0.1 eV or more, it is determined that the surface of the electrode material for the lithium secondary battery or the solid electrolyte material has deteriorated.
  • “immediately after exposure to the atmosphere” may be an arbitrarily selected time.
  • the ionization potential may be taken out into the atmosphere and may be from 0 minutes to 15 minutes, from 0 minutes to 10 minutes, from 0 minutes to 5 minutes, or from 0 minutes to 3 minutes.
  • changes from the ideal structure such as whether or not a resistance layer is formed on the surface of the lithium secondary battery material, especially surface electronic state changes that are closely related to battery characteristics, can be quickly determined. can do.
  • the separately stored material is compared with the ionization potential data of the same type of material that has been previously measured and stored, so that the stored material is It can be easily determined whether it can be used or not.
  • the results of the obtained ionization potential include the results of the second embodiment described below, the results of STEM-ADF measurement and EELS measurement, the results of the discharge capacity actually obtained by using the battery material for the battery, etc. Judgment may be made in combination.
  • Second Embodiment when a lithium secondary battery electrode material is synthesized, the ionization potential of the synthesized lithium secondary battery electrode material is measured. Then, a comparison is made to determine whether or not the measured ionization potential has increased more than that of a standard lithium secondary battery electrode material having the same composition and measured separately. And when it increases, it is an inspection method that determines that a disorder of the crystal structure is observed on the surface of the electrode material for a lithium secondary battery, such as occurrence of some change, for example, whether cation mixing has occurred. For example, while using the same material and material composition, the ionization potential values of a plurality of battery materials obtained by changing the manufacturing conditions and the manufacturing method conditions may be measured and compared.
  • the obtained material may be evaluated for an ionization potential value according to a difference in exposure time to the atmosphere and used for judgment.
  • the determination may be made in combination with the result of STEM-ADF measurement or EELS measurement, or the result of the discharge capacity actually obtained by using the battery material for the battery.
  • the STEM-ADF measurement and the EELS measurement may be used in combination with the measurement of the first embodiment or the second embodiment.
  • the STEM-ADF (Annual Dark Field Scanning Transmission Electron Microscope) measurement method may be performed as follows.
  • the electrode material for a lithium secondary battery is processed into a thin film for cross-sectional measurement using CP (cross section polisher), FIB (focused ion beam), or the like.
  • CP cross section polisher
  • FIB focused ion beam
  • an electron beam is applied so as to pass through the cross section of the sample, the scattered electrons are measured, and the intensity is displayed as an image.
  • the EELS measurement is a method for measuring the energy that electrons passing through the same sample plane lose due to the interaction with atoms.
  • Detecting in X-ray diffraction measurement by combining the measurement values obtained by the first embodiment and the second embodiment with the surface observation result by one or both of STEM-ADF measurement method and EELS measurement It is possible to better predict the change in the electronic state in the outermost surface layer, which is difficult to perform, from the result of ionization potential measurement. By collecting and accumulating such data, the surface electronic state of the lithium secondary battery material can be inspected in detail based on a short-time inspection result.
  • Example 1 LiNi 0.82 Co 0.15 Al 0.03 O 2 Prediction of performance degradation due to generation of resistance layer on particle surface LiNi 0 synthesized by reacting a precursor synthesized by a coprecipitation method with lithium hydroxide .82 Co 0.15 Al 0.03 O 2 particles were exposed to air. Immediately after this and thereafter every predetermined time, powder X-ray diffraction measurement and ionization potential measurement were performed. Changes in peak position and relative intensity, and changes in ionization potential in the obtained X-ray diffraction results were examined.
  • Ionization potential change was measured using an atmospheric photoelectron spectrometer (AC-3, manufactured by Riken Keiki Co., Ltd.).
  • the atmospheric photoelectron spectrometer is an atmospheric ultraviolet photoelectron spectrometer. Specifically, about 100 mg of a powder sample of LiNi 0.82 Co 0.15 Al 0.03 O 2 particles was prepared on a dedicated sample stage and measured in the energy range of 4.2 to 7.0 eV. Until immediately before the measurement, the sample was stored under a dew point-controlled argon atmosphere and in a pouch filled with dry argon gas. Samples were exposed to the atmosphere only during exposure processing and measurements. The time taken to measure one sample was within 5 minutes.
  • the ionization potential was estimated from the intersection of the extrapolated line obtained by the least square method and the ground level.
  • the ionization potential obtained as a result of the ionization potential of the sample immediately after exposure and after 3 hours passed is the horizontal axis (unit: eV), and the normalized intensity is the vertical axis (described as “Count (%)” in FIG. 2). As shown in FIG.
  • Powder X-ray diffraction measurement Generally, in a lithium nickel-containing composite oxide represented by LiNi 0.82 Co 0.15 Al 0.03 O 2 , Cu—K ⁇ rays are used as an X-ray source in a layered rock salt type crystal structure.
  • the ratio of the diffraction line peak intensity attributed to the (003) plane and the (104) plane obtained from the powder X-ray diffraction used is 1.2 or more.
  • the disorder of the crystal structure was judged from this peak intensity ratio.
  • the X-ray diffraction intensity attributed to the (003) plane becomes small. Therefore, it means that the larger the ratio of the peak intensities is, the less the layered rock salt structure is.
  • FIG. 1 shows the powder X-ray diffraction measurement results obtained by measuring LiNi 0.82 Co 0.15 Al 0.03 O 2 particles immediately after being exposed to the atmosphere and thereafter by exposing for 5 hours every hour. Show. As is clear from FIG. 1, the lines indicating the results overlap, and no change was observed in the position of the diffraction lines or the ratio of the diffraction line peak intensities belonging to the (003) plane and the (104) plane. . No changes could be detected by powder X-ray diffraction measurement.
  • FIG. 2 shows the measurement result of the change in ionization potential, measured immediately after exposure of LiNi 0.82 Co 0.15 Al 0.03 O 2 particles to the atmosphere and every predetermined time thereafter.
  • the ionization potential significantly increased from the intersection of the extrapolated line obtained by the least square method and the ground level after 3 hours from exposure to the atmosphere.
  • FIG. 3 shows the result of EELS measurement measured after the LiNi 0.82 Co 0.15 Al 0.03 O 2 particles were exposed to the atmosphere for 3 hours.
  • FIG. 4 shows the result of STEM-ADF observation, which was measured after LiNi 0.82 Co 0.15 Al 0.03 O 2 particles were exposed to the atmosphere for 3 hours. In these, measurement of one sample required measurement time of 2 days or more. From the STEM-ADF observation photograph, formation of a layer having a pattern different from the checkered pattern was observed, suggesting the formation of a different phase in the surface layer. In addition, from the EELS spectrum, a shift in Ni-derived peak was observed in a layer having a thickness of about 10 nm from the surface. This suggests the formation of a rock salt layer (resistance layer) in the surface layer. These results correspond to the measurement results of the ionization potential.
  • Example 2 LiCoO 2 the ionization potential of the synthesized eight LiCoO 2 single crystal grains in the single crystal grain surface different performance deterioration prediction by cation mixing techniques, atmospheric photoelectron spectrometer (Riken Keiki Co., AC- 3). About 100 mg of a powder sample of isolated LiCoO 2 single crystal particles was prepared on a dedicated sample stage and measured in the energy range of 4.2 to 7.0 eV. Until immediately before the measurement, the sample was stored in a dew point-controlled argon atmosphere and in a pouch filled with dry argon gas. Exposure to air only during measurement. The time taken to measure one sample was within 5 minutes. In the determination method of the present invention, the determination can be made based on the level of the obtained ionization potential value.
  • Table 1 shows the ionization potential and the initial discharge capacity for eight samples. Specifically, eight R2032-type half cells each using LiCoO 2 single crystal particles as electrode active materials were manufactured, and after these, the open circuit voltage was stabilized, the temperature became 4.2 at 25 ° C. and 0.5 C. Then, a charge / discharge test was performed to measure the discharge capacity when discharged as 10C until 2.8V. Table 1 shows the initial discharge capacity and the ionization potential corresponding to the LiCoO 2 particles.
  • the eight samples had the same particle morphology, composition, and X-ray diffraction pattern as in the experiment of Example 1. Nevertheless, only the secondary battery using the LiCoO 2 single crystal particles as the positive electrode active material for the positive electrode having an ionization potential of 5.75 eV or less showed a good initial discharge capacity of 130 mAh / g or more (Sample 1). 3, 5, 7, 8). The difference in these physical property values can be attributed to cation mixing on the surface of the LiCoO 2 crystal particles. This result shows that the superiority of the present invention is remarkably exhibited. As described above, according to the present invention, it is possible to provide a method for accurately inspecting the performance of an electrode material for a lithium secondary battery used as a raw material for a lithium secondary battery in a short time.

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Abstract

Le présent procédé d'inspection permet d'inspecter, sous pression atmosphérique, l'état d'électrons de surface de matériaux d'électrode ou de matériaux d'électrolyte solide de batteries secondaires au lithium. Selon ce procédé d'inspection, l'état d'électrons de surface d'un matériau d'électrode de batteries secondaires au lithium est inspecté à partir du potentiel d'ionisation spécifique au matériau d'électrode de batteries secondaires au lithium ou au matériau d'électrolyte solide.
PCT/JP2019/011995 2018-03-30 2019-03-22 Procédé d'inspection WO2019188750A1 (fr)

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KR1020207027760A KR102278258B1 (ko) 2018-03-30 2019-03-22 검사 방법
CN201980022094.3A CN111902977B (zh) 2018-03-30 2019-03-22 检测方法
JP2020509940A JP6905292B2 (ja) 2018-03-30 2019-03-22 検査方法

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002305028A (ja) * 2001-04-04 2002-10-18 Nissan Motor Co Ltd 固体高分子電解質型電池および固体高分子電解質の製造方法
JP2003257677A (ja) * 2002-03-04 2003-09-12 Honda Motor Co Ltd 有機エレクトロルミネッセンス素子及びその製造方法
JP2004259650A (ja) * 2003-02-27 2004-09-16 Kanegafuchi Chem Ind Co Ltd マグネシウム二次電池
US20100230632A1 (en) * 2005-09-20 2010-09-16 Virtic, Llc High energy battery materials
JP2015032425A (ja) * 2013-08-01 2015-02-16 日立金属株式会社 負極活物質及びそれを用いた二次電池

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012104276A (ja) 2010-11-08 2012-05-31 Toyota Motor Corp 二次電池の検査方法
JP6523113B2 (ja) * 2015-09-14 2019-05-29 株式会社東芝 電極、非水電解質電池、電池パック、および自動車

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002305028A (ja) * 2001-04-04 2002-10-18 Nissan Motor Co Ltd 固体高分子電解質型電池および固体高分子電解質の製造方法
JP2003257677A (ja) * 2002-03-04 2003-09-12 Honda Motor Co Ltd 有機エレクトロルミネッセンス素子及びその製造方法
JP2004259650A (ja) * 2003-02-27 2004-09-16 Kanegafuchi Chem Ind Co Ltd マグネシウム二次電池
US20100230632A1 (en) * 2005-09-20 2010-09-16 Virtic, Llc High energy battery materials
JP2015032425A (ja) * 2013-08-01 2015-02-16 日立金属株式会社 負極活物質及びそれを用いた二次電池

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JPWO2019188750A1 (ja) 2021-02-12
KR20200117036A (ko) 2020-10-13
CN111902977B (zh) 2021-09-24
CN111902977A (zh) 2020-11-06
KR102278258B1 (ko) 2021-07-15

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