CN115207454B - Solid ion conductor material and preparation method thereof - Google Patents

Solid ion conductor material and preparation method thereof

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CN115207454B
CN115207454B CN202210735666.6A CN202210735666A CN115207454B CN 115207454 B CN115207454 B CN 115207454B CN 202210735666 A CN202210735666 A CN 202210735666A CN 115207454 B CN115207454 B CN 115207454B
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atoms
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CN115207454A (en
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张晓琨
向勇
宫勇吉
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University of Electronic Science and Technology of China
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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
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
    • H01M50/497—Ionic conductivity
    • 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
    • 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

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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
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  • Conductive Materials (AREA)
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Abstract

本发明涉及离子导体技术领域，特别涉及一种固态离子导体材料及其制备方法。一种固态离子导体材料的制备方法，以二维层状结构材料为原料掺杂一定比例原子，将完成掺杂后的二维层状结构材料进行自组装，以获得自组装完的二维材料；将自组装完的二维材料浸泡在传导离子的饱和水溶液中，以输运所述传导离子至所述自组装完的二维材料的层间形成层间离子的密堆积，即可得到所需的固态离子导体材料；所掺杂的原子为非金属原子；所述传导离子为金属离子。通过该固态离子导体材料的制备方法能得到高离子电导率的固态离子导体材料。

The present invention relates to the field of ion conductor technology, and more particularly to a solid-state ion conductor material and a method for preparing the same. A method for preparing a solid-state ion conductor material comprises doping a two-dimensional layered structure material with a certain proportion of atoms as a raw material, self-assembling the doped two-dimensional layered structure material to obtain a self-assembled two-dimensional material; immersing the self-assembled two-dimensional material in a saturated aqueous solution of conductive ions to transport the conductive ions between the layers of the self-assembled two-dimensional material to form a dense stack of interlayer ions, thereby obtaining the desired solid-state ion conductor material; the doped atoms are non-metallic atoms; and the conductive ions are metal ions. This method for preparing a solid-state ion conductor material can produce a solid-state ion conductor material with high ionic conductivity.

Description

Solid ion conductor material and preparation method thereof
[ Field of technology ]
[1] The invention relates to the technical field of ion conductors, in particular to a solid ion conductor material and a preparation method thereof.
[ Background Art ]
[2] Solid ion conductor materials are important foundation for constructing low-power consumption information devices and high-performance energy devices in the future. For example, the basic components of the nerve morphology computing system such as conductive bridge resistive switching devices and energy coupling devices, and the energy devices such as high specific property all-solid-state batteries need to be supported by solid ion conductor materials with high ion conductivity and high electronic insulation.
[3] Currently, the level of ionic conductivity of alkaline earth metal ion conductor materials commonly used in devices is generally limited, wherein the ionic conductivity of liquid ion conductors is substantially below 10 -2 S/cm, while the ionic conductivity of solid ion conductors is below 10 -3 S/cm. The liquid ion conductor has remarkable restriction on the integration level of information devices, the safety of energy devices and the like. The lower level of ionic conductivity of the solid state ionic conductor results in low information device frequency characteristics and low energy device power characteristics.
[ Invention ]
[4] In order to solve the problem of low ionic conductivity level of a solid ion conductor, the invention provides a solid ion conductor material and a preparation method thereof.
[5] The invention provides a preparation method of a solid ion conductor material, which comprises the steps of taking a two-dimensional layered structure material as a raw material, doping atoms in a certain proportion, self-assembling the doped two-dimensional layered structure material to obtain a self-assembled two-dimensional material, immersing the self-assembled two-dimensional material in a saturated aqueous solution of conductive ions to transport the conductive ions to the interlayer of the self-assembled two-dimensional material to form close packing of interlayer ions, and obtaining the required solid ion conductor material, wherein the doped atoms are non-metal atoms, and the conductive ions are metal ions.
[6] Preferably, the doping atoms are fluorine atoms, nitrogen atoms, sulfur atoms or oxygen atoms, and the doping proportion is 2-20%.
[7] The conductive ions are lithium ions, sodium ions, potassium ions, magnesium ions or zinc ions.
[8] Preferably, the self-assembly is performed by a template method or a suction filtration method.
[9] Preferably, the doping is achieved by N doping at 1000 degrees celsius in an atmosphere of NH 3.
[10] Preferably, the two-dimensional layered structure material is graphene oxide.
[11] Preferably, the self-assembly is to dissolve the doped two-dimensional layered structure material in water to prepare an aqueous solution and then vacuum-filter the aqueous solution.
[12] Preferably, the vacuum filtration is carried out by taking anodic aluminum oxide as a filter membrane under the vacuum degree of 0-100 ℃ and 0-50Kpa, and the concentration of the aqueous solution is 1-50mg/ml.
[13] Preferably, the preparation method of the solid ion conductor material further comprises the steps of intercalation before or after doping atoms in a certain proportion, and self-assembly after doping and intercalation, wherein the intercalation is to insert atoms, ions or small molecules between two-dimensional lamellar structure material layers.
[14] The invention also provides a solid ion conductor material, which is prepared according to the preparation method of the solid ion conductor material.
[15] Preferably, the interlayer spacing of the solid ion conductor material is 0.5-2nm, and the ion conductivity is 10 -2-10- 1 S/cm.
[16] Compared with the prior art, the preparation method of the solid ion conductor material provided by the invention has the advantages that the electron cloud structure of the two-dimensional layered structure material is regulated and controlled through element doping, the acting force on ions is reduced, namely the resistance of the surrounding environment of an ion channel to ion transportation is effectively reduced, the self-assembly can well realize the high order of the two-dimensional material, and the effective regulation and control on the interlayer spacing of the two-dimensional material can be realized through the introduction of the precursor hetero atoms, so that the solid ion conductor material with high ion conductivity can be obtained.
[17] The invention also provides a solid ion conductor material, and the ion conductivity of the solid ion conductor material can reach 10 -2-10-1 S/cm.
[ Description of the drawings ]
[18] Fig. 1 is a schematic structural diagram of a solid ion conductor material provided by the present invention.
[ Detailed description ] of the invention
[19] For the purpose of making the technical solution and advantages of the present invention more apparent, the present invention will be further described in detail below with reference to the accompanying drawings and examples of implementation. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
[20] Referring to fig. 1, a first embodiment of the present invention provides a method for preparing a solid ion conductor material, which comprises doping a two-dimensional layered structure material with atoms in a certain proportion, self-assembling the doped two-dimensional layered structure material to obtain a self-assembled two-dimensional material, immersing the self-assembled two-dimensional material in a saturated aqueous solution of conductive ions to transport the conductive ions to the interlayer of the self-assembled two-dimensional material to form close packing of interlayer ions, wherein the doped atoms are non-metal atoms, and the conductive ions are metal ions.
[21] The preparation method of the solid ion conductor material reduces the acting force of the element doping to ions by regulating and controlling the electron cloud structure of the two-dimensional layered structure material, namely effectively reduces the resistance of the surrounding environment of the ion channel to ion transportation, can well realize the high order of the two-dimensional material by self-assembly, can realize the effective regulation and control of the interlayer spacing of the two-dimensional material by introducing the precursor heteroatom, and can obtain the solid ion conductor material with high ion conductivity.
[22] It will be appreciated that the present invention is based on a two-dimensional layered structure of materials, between which ion-conducting channels are formed. Whereas the ionic conductivity of solid ion conductor materials is primarily determined by two factors. The ion transport channel is characterized in that the size of the ion transport channel, and the resistance of the ion transport environment around the ion channel is essentially the acting force of electron clouds of atoms/molecules/crystals forming the ion channel on the ions. In the invention, the two factors are well solved, so that the solid ion conductor material with high ion conductivity is prepared.
[23] The doping atoms are preferably fluorine atoms, nitrogen atoms, sulfur atoms or oxygen atoms, more preferably nitrogen atoms, and the doping ratio thereof is preferably 2 to 20%, more preferably 3 to 5%. And by confirming the doping elements and the doping proportion, the effect of regulating and controlling the electron cloud structure and the interlayer spacing of the two-dimensional layered structure material is ensured.
[24] Preferably, the doping is accomplished by a high temperature reaction or a liquid phase reaction. In some specific embodiments, N doping is achieved by an atmosphere of NH 3 at 1000 degrees celsius.
[25] The conductive ions are preferably lithium ions, sodium ions, potassium ions, magnesium ions or zinc ions.
[26] The self-assembly can be carried out by a template method or a suction filtration method, for example, the self-assembly can be completed by suction filtration of an aqueous solution of the two-dimensional layered structure material.
[27] The transport conductive ions can be soaked or electric field regulated. Further, the transportation of the conductive ions is completed by immersing the self-assembled two-dimensional material in a saturated aqueous solution of the conductive ions. Specifically, the self-assembled two-dimensional material can be soaked in an aqueous solution of LiCl, so that spontaneous diffusion among ion layers can be realized, and close packing of conductive ions among the two-dimensional material layers can be realized. The electric field regulation and control rule can be that grid voltage is applied to the two-dimensional material to regulate the interlayer spacing and the charge state of the two-dimensional material, so that the spontaneous entry of the conductive ions is realized.
[28] The two-dimensional layered structure material may be graphene oxide, boron nitride, MXene or a hybrid structure thereof, and preferably, the two-dimensional layered structure material is graphene oxide. The two-dimensional layered structure material can be directly purchased or prepared. For example, the two-dimensional layered structure material nanoflakes may be synthesized by an oxidative exfoliation method, a solvent exfoliation method, a direct synthesis method, or the like. In some embodiments, the nanoflakes of graphene may be obtained by a Hummer oxidation process.
[29] When the two-dimensional layered structure material is graphene oxide, preferably, the self-assembly is to perform vacuum filtration after the doped two-dimensional layered structure material is dissolved in water to prepare an aqueous solution. Further, the vacuum filtration is carried out by taking anodic aluminum oxide as a filter membrane under the vacuum degree of 0-100 ℃ and 0-50Kpa, and the concentration of the aqueous solution is 1-50mg/ml.
[30] In some preferred embodiments, the preparation method of the solid ion conductor material further comprises intercalation before or after doping a certain proportion of atoms, and the self-assembly is performed after doping and intercalation, wherein the intercalation is to insert atoms, ions or small molecules between two-dimensional layered structure material layers. By inserting atoms, ions or small molecules between two-dimensional layered structure material layers, the interlayer spacing of graphene oxide and the electron cloud structure can be further regulated and controlled, so that the conductivity of the solid ion conductor material is improved. Wherein, the intercalation atoms can be sulfur atoms, the ions can be sodium ions and potassium ions, and the small molecules can be water.
[31] Further, intercalation of the two-dimensional layered structure material is achieved by gas phase, electrochemical method or liquid phase method. The introduction of potassium ions between graphene layers can be realized by an electrochemical method, and the interlayer spacing of the graphene layers is changed.
[32] It is understood that the present invention is based on doping atoms to alter the interlayer spacing of a two-dimensional layered structure material such that the resulting solid ion conductor material has an interlayer spacing of 0.5-2nm. Further, atoms, ions or small molecules can be inserted between two-dimensional lamellar structure material layers through intercalation for regulation and control.
[33] Referring to fig. 1, a second embodiment of the present invention provides a solid ion conductor material, which is prepared according to the preparation method of the solid ion conductor material in the first embodiment. Preferably, the interlayer spacing of the solid ion conductor material is 0.5-2nm, and the ion conductivity is 10 -2-10-1 S/cm.
[34] It should be appreciated that reference throughout this specification to "one embodiment" or "an embodiment" means that a particular feature, structure or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention. Thus, the appearances of the phrases "in one embodiment" or "in an embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. Those skilled in the art will also appreciate that the embodiments described in the specification are alternative embodiments and that the acts and modules referred to are not necessarily required for the present invention.
[35] The above embodiments are provided to assist in understanding the method and core ideas of the present invention, and meanwhile, to those skilled in the art, according to the ideas of the present invention, there are changes in the specific embodiments and application scope, and in summary, the present disclosure should not be construed as limiting the invention, and any modification, equivalent replacement, improvement etc. made within the principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1.一种固态离子导体材料的制备方法，其特征在于：以二维层状结构材料为原料掺杂一定比例原子，将完成掺杂后的二维层状结构材料进行自组装，以获得自组装完的二维材料；1. A method for preparing a solid-state ion conductor material, characterized by: using a two-dimensional layered structure material as a raw material, doping a certain proportion of atoms, and self-assembling the doped two-dimensional layered structure material to obtain a self-assembled two-dimensional material; 将自组装完的二维材料浸泡在传导离子的饱和水溶液中，以输运所述传导离子至所述自组装完的二维材料的层间形成层间离子的密堆积，即可得到所需的固态离子导体材料；The self-assembled two-dimensional material is immersed in a saturated aqueous solution of conductive ions to transport the conductive ions to the interlayers of the self-assembled two-dimensional material to form a dense stacking of interlayer ions, thereby obtaining the desired solid-state ion conductor material; 所掺杂的原子为非金属原子；所述传导离子为金属离子。The doped atoms are non-metal atoms; and the conductive ions are metal ions. 2.如权利要求1所述的固态离子导体材料的制备方法，其特征在于：所述掺杂的原子为氟原子、氮原子、硫原子或氧原子，其掺杂比例为2-20%；2. The method for preparing a solid ion conductor material according to claim 1, wherein the doping atoms are fluorine atoms, nitrogen atoms, sulfur atoms or oxygen atoms, and the doping ratio thereof is 2-20%; 所述传导离子为锂离子、钠离子、钾离子、镁离子或锌离子。The conductive ions are lithium ions, sodium ions, potassium ions, magnesium ions or zinc ions. 3.如权利要求1所述的固态离子导体材料的制备方法，其特征在于：所述自组装采用模板法或抽滤法。3. The method for preparing a solid ion conductor material according to claim 1, wherein the self-assembly is performed by a template method or a filtration method. 4.如权利要求1所述的固态离子导体材料的制备方法，其特征在于：所述掺杂通过在1000摄氏度、NH3的气氛下实现N掺杂。4. The method for preparing a solid ion conductor material according to claim 1, wherein the doping is performed by N-doping at 1000 degrees Celsius in an NH3 atmosphere. 5.如权利要求1所述的固态离子导体材料的制备方法，其特征在于：所述二维层状结构材料为氧化石墨烯。5 . The method for preparing a solid ion conductor material according to claim 1 , wherein the two-dimensional layered structure material is graphene oxide. 6.如权利要求5所述的固态离子导体材料的制备方法，其特征在于：所述自组装为将完成掺杂后的二维层状结构材料溶于水中制得水溶液后进行真空抽滤。6. The method for preparing a solid ion conductor material according to claim 5, wherein the self-assembly comprises dissolving the doped two-dimensional layered structure material in water to prepare an aqueous solution and then vacuum filtering the solution. 7.如权利要求6所述的固态离子导体材料的制备方法，其特征在于：所述真空抽滤以阳极氧化铝为滤膜，在0-100℃、0-50Kpa真空度下进行；所述水溶液浓度为1-50mg/ml。7. The method for preparing a solid ion conductor material according to claim 6, wherein the vacuum filtration is performed using anodized aluminum oxide as a filter membrane at a temperature of 0-100°C and a vacuum degree of 0-50 kPa; and the concentration of the aqueous solution is 1-50 mg/ml. 8.如权利要求5所述的固态离子导体材料的制备方法，其特征在于：还包括在掺杂一定比例原子之前或之后进行插层，完成掺杂和插层之后再进行所述自组装；所述插层为将原子、离子或小分子插入二维层状结构材料层间。8. The method for preparing a solid-state ion conductor material according to claim 5, further comprising performing intercalation before or after doping a certain proportion of atoms, and performing the self-assembly after completing the doping and intercalation; the intercalation is to insert atoms, ions or small molecules into the interlayers of the two-dimensional layered structure material. 9.一种固态离子导体材料，其特征在于：根据权利要求1-8任一项中所述固态离子导体材料的制备方法制备得到。9. A solid ion conductor material, characterized in that it is prepared according to the method for preparing a solid ion conductor material according to any one of claims 1 to 8. 10.如权利要求9所述的固态离子导体材料，其特征在于：其层间距为0.5-2nm，离子电导率为10-2-10-1S/cm。10. The solid ion conductor material according to claim 9, wherein the interlayer distance is 0.5-2 nm and the ionic conductivity is 10 <-2> -10 <-1> S/cm.
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