CN115108585A - Rod-shaped Li 2 Mg 2 (MoO 4 ) 3 Material and method for the production thereof - Google Patents

Rod-shaped Li 2 Mg 2 (MoO 4 ) 3 Material and method for the production thereof Download PDF

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CN115108585A
CN115108585A CN202210666417.6A CN202210666417A CN115108585A CN 115108585 A CN115108585 A CN 115108585A CN 202210666417 A CN202210666417 A CN 202210666417A CN 115108585 A CN115108585 A CN 115108585A
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moo
rod
shaped
preparation
nitrate
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王立秋
陈太
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Dalian University of Technology
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Dalian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/006—Compounds containing, besides molybdenum, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • 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

Abstract

Rod-shaped Li 2 Mg 2 (MoO 4 ) 3 A material and a preparation method thereof belong to the field of preparation of inorganic non-metallic materials. Lithium hydroxide and magnesium and molybdenum metal oxides are used as raw materials, and nitrate is mixed with the raw materials and ground to obtain a precursor. Calcining the obtained precursor at the temperature of 350-550 ℃ for 1-5h, and cooling to room temperature to obtain Li after the treatment is finished 2 Mg 2 (MoO 4 ) 3 -a salt mixture. Washing the obtained mixture with deionized water for 4-6 times, filtering to remove salt components, and drying in oven at 110 deg.C for 2-3 hr to obtain rod-shaped Li 2 Mg 2 (MoO 4 ) 3 A material. The product obtained by the invention has an obvious rod-shaped structure and good dispersibility, the diameter is 0.3-0.65 μm, and the length is 0.5-9 μm. In addition, Li can be reduced 2 Mg 2 (MoO 4 ) 3 The preparation temperature of the material is reduced, the calcination time is shortened, the energy consumption is reduced, and the whole process is simple and convenient and is easy to operate.

Description

Rod-shaped Li 2 Mg 2 (MoO 4 ) 3 Material and method for the production thereof
Technical Field
The invention belongs to the technical field of preparation of inorganic nonmetallic materials, and particularly relates to a rod-shaped Li 2 Mg 2 (MoO 4 ) 3 Materials and methods for their preparation.
Background
Micro-nano material due to its uniqueExcellent performance, and has been widely applied in the fields of chemical catalysis, photocatalysis, electrochemistry, electronic devices and the like. Since the last century, various micro-nano materials with specific morphologies are developed and researched, and the materials with the specific morphologies often have excellent performance in the fields of catalysis, optics, electric materials and the like. For example, rod-shaped micro-nano ZnO has higher photocatalytic activity; rod-shaped spinel-type LiMn 2 O 4 Shows more excellent electrical cycle performance and rate capability.
Li 2 Mg 2 (MoO 4 ) 3 As an important molybdate material, the molybdate red has important application value in the aspects of laser materials, luminescent materials, microwave dielectric ceramics and the like. Li 2 Mg 2 (MoO 4 ) 3 :Yb 3+ The laser has a wider emission band, and can be used as an alternative material of a tunable laser. The document "Photolutenescence of Orthorhombic Li 2 Mg 2 (MoO 4 ) 3 crystal doped with Yb 3+ ions "report Yb obtained at 750 ℃ 3+ Doped orthorhombic phase Li 2 Mg 2 (MoO 4 ) 3 The material can be used as a potential application material of a tunable laser.
At present, Li is relevant at home and abroad 2 Mg 2 (MoO 4 ) 3 The preparation of the material mostly adopts a solid phase method, and the raw materials need to be ball-milled for a long time and then need to be calcined at high temperature to obtain Li 2 Mg 2 (MoO 4 ) 3 The powder and the prepared powder have irregular micro-morphology. And rod-shaped Li 2 Mg 2 (MoO 4 ) 3 The material has important significance for textured ceramics, and the rod-shaped structure has larger specific surface area, which has positive effects in the fields of catalysis, luminescence and the like. Therefore, the Li with the specific rod-like shape is prepared under the conditions of shorter preparation time and low calcination temperature 2 Mg 2 (MoO 4 ) 3 The material has very important potential value.
The invention adopts nitrate to melt at low temperature to provide liquid-phase ionic environment for reaction, is used for reducing the surface energy of raw materials and can be lowerPreparing the Li with a rod-like shape at a temperature 2 Mg 2 (MoO 4 ) 3 Material, Li prepared by this method 2 Mg 2 (MoO 4 ) 3 The material has regular shape and good dispersibility; the method has the advantages of low preparation temperature and short calcination time, and has great advantages for large-scale production, so the method has good application value.
Disclosure of Invention
The object of the present invention is to provide a rod-like Li 2 Mg 2 (MoO 4 ) 3 The material and the preparation method thereof can solve the problems of irregular preparation shape, high temperature, long calcination time and particle agglomeration in the prior method.
The technical route of the invention is as follows:
rod-shaped Li 2 Mg 2 (MoO 4 ) 3 The material has a remarkable rod-shaped structure, the diameter of the material is 0.3-0.65 μm, and the length of the material is 0.5-9 μm.
Rod-shaped Li 2 Mg 2 (MoO 4 ) 3 The preparation method of the material comprises the following steps:
(1) according to Li 2 Mg 2 (MoO 4 ) 3 Weighing lithium hydroxide, metal oxide of magnesium and metal oxide of molybdenum as raw materials according to a stoichiometric ratio, weighing nitrate, mixing the nitrate with the raw materials, and grinding to obtain a precursor, wherein the molar ratio of the raw materials to the nitrate is 1 (0.5-2.5);
(2) calcining the precursor obtained in the step (1) in an air atmosphere at the temperature of 350-550 ℃ for 1-5h, and after the calcination is finished, cooling to room temperature to obtain a mixture;
(3) washing the mixture obtained in the step (2) with deionized water for 4-6 times, filtering to remove salt components, and drying at the temperature of 110 ℃ for 2-3h to obtain rod-shaped Li 2 Mg 2 (MoO 4 ) 3 And (3) powder.
The nitrate is NaNO 3 。
Compared with the prior art, the invention has the following advantages:
1. the invention prepares the rod-shaped Li 2 Mg 2 (MoO 4 ) 3 Material, expand Li 2 Mg 2 (MoO 4 ) 3 The application field of the material.
2. The invention utilizes nitrate to provide a liquid phase reaction environment to reduce the surface energy of reactants and prepares the rod-shaped Li at low temperature 2 Mg 2 (MoO 4 ) 3 Compared with the traditional solid phase method, the method greatly reduces the energy consumption.
3. Rod-shaped Li prepared by the invention 2 Mg 2 (MoO 4 ) 3 The material has good dispersibility.
4. The preparation method is simple, the conditions are mild and easy to control, and the large-scale production is easy to realize.
Drawings
FIG. 1 is a bar-shaped Li prepared in example 1 2 Mg 2 (MoO 4 ) 3 XRD pattern of the material.
FIG. 2 is a rod-shaped Li prepared in example 1 2 Mg 2 (MoO 4 ) 3 SEM image of material.
FIG. 3 is a bar-shaped Li prepared in examples 2 and 3 at different calcination temperatures 2 Mg 2 (MoO 4 ) 3 SEM pictures of materials, (a)350 ℃; (b) at 550 ℃.
FIG. 4 is a plot of the rod-shaped Li prepared in examples 4 and 5 at different calcination times 2 Mg 2 (MoO 4 ) 3 SEM pictures of the material, (a)1 h; (b) and 5 h.
Detailed Description
For further illustration of the present invention, the salient features of the invention are further illustrated by some embodiments, but not to limit the scope of the invention.
Example 1:
a rod-like Li is described in the present example 2 Mg 2 (MoO 4 ) 3 The preparation method of the material comprises the following steps:
weighing LiOH & H according to stoichiometric ratio 2 O、MgO、MoO 3 Using NaNO as raw material 3 Mixing nitrate with the above raw materials, grinding to obtain precursor, mixing the raw materials with NaNO 3 The molar ratio of the raw material of NaNO 3 1: 1.5. Transferring the precursor into a muffle furnace, calcining for 2h at 450 ℃ in air atmosphere, cooling to room temperature after the calcination time is over, and obtaining Li 2 Mg 2 (MoO 4 ) 3 -a salt mixture. The Li obtained above 2 Mg 2 (MoO 4 ) 3 Washing the salt mixture with deionized water for many times, filtering to remove salt components, and drying at 110 ℃ for 2h to obtain the rod-shaped Li 2 Mg 2 (MoO 4 ) 3 A material.
Example 2:
the present embodiment is different from embodiment 1 in that: the calcination temperature was 350 ℃. The preparation method comprises the following steps:
weighing LiOH & H according to stoichiometric ratio 2 O、MgO、MoO 3 Using NaNO as raw material 3 Mixing nitrate with the above raw materials, grinding to obtain precursor, mixing with NaNO 3 The molar ratio of the raw material of NaNO 3 1: 1.5. Transferring the precursor into a muffle furnace, calcining for 2h at 350 ℃ in air atmosphere, cooling to room temperature after the calcination time is over, and obtaining Li 2 Mg 2 (MoO 4 ) 3 -a salt mixture. The Li obtained above 2 Mg 2 (MoO 4 ) 3 Washing the salt mixture with deionized water for multiple times, filtering to remove salt components, and drying at 110 deg.C for 2h to obtain rod-shaped Li 2 Mg 2 (MoO 4 ) 3 A material.
Example 3:
the present embodiment is mainly different from embodiment 1 in that: the calcination temperature was 550 ℃. The preparation method comprises the following steps:
weighing LiOH & H according to stoichiometric ratio 2 O、MgO、MoO 3 Using NaNO as raw material 3 Mixing nitrate with the above raw materials, grinding to obtain precursor, mixing with NaNO 3 The molar ratio of the raw material of NaNO 3 1: 1.5. Transferring the precursor into a muffle furnace, calcining for 2h at 550 ℃ in air atmosphere, cooling to room temperature after the calcination time is over, and obtaining Li 2 Mg 2 (MoO 4 ) 3 -a salt mixture.The Li obtained above 2 Mg 2 (MoO 4 ) 3 Washing the salt mixture with deionized water for many times, filtering to remove salt components, and drying at 110 ℃ for 2h to obtain the rod-shaped Li 2 Mg 2 (MoO 4 ) 3 A material.
Example 4:
the present embodiment is mainly different from embodiment 1 in that: the calcination time was 1 h. The preparation method comprises the following steps:
weighing LiOH & H according to stoichiometric ratio 2 O、MgO、MoO 3 Using NaNO as raw material 3 Mixing nitrate with the above raw materials, grinding to obtain precursor, mixing with NaNO 3 The molar ratio of the raw material of NaNO 3 1: 1.5. Transferring the precursor into a muffle furnace, calcining for 1h at 450 ℃ in air atmosphere, cooling to room temperature after the calcination time is over, and obtaining Li 2 Mg 2 (MoO 4 ) 3 -a salt mixture. The Li obtained above 2 Mg 2 (MoO 4 ) 3 Washing the salt mixture with deionized water for many times, filtering to remove salt components, and drying at 110 ℃ for 2h to obtain the rod-shaped Li 2 Mg 2 (MoO 4 ) 3 A material.
Example 5:
the present embodiment is mainly different from embodiment 1 in that: the calcination time was 5 h. The preparation method comprises the following steps:
weighing LiOH & H according to stoichiometric ratio 2 O、MgO、MoO 3 Using NaNO as raw material 3 Mixing nitrate with the above raw materials, grinding to obtain precursor, mixing with NaNO 3 The molar ratio of the raw material of NaNO 3 1: 1.5. Transferring the precursor into a muffle furnace, calcining for 5h at 450 ℃ in air atmosphere, cooling to room temperature after the calcination time is over, and obtaining Li 2 Mg 2 (MoO 4 ) 3 -a salt mixture. The Li obtained above 2 Mg 2 (MoO 4 ) 3 Washing the salt mixture with deionized water for multiple times, filtering to remove salt components, and drying at 110 deg.C for 2h to obtain rod-shaped Li 2 Mg 2 (MoO 4 ) 3 A material.
Example 6:
the present embodiment is mainly different from embodiment 1 in that: the molar ratio of the raw material to the molten salt is NaNO 3 1: 0.5. The preparation method comprises the following steps:
weighing LiOH & H according to stoichiometric ratio 2 O、MgO、MoO 3 Using NaNO as raw material 3 Mixing nitrate with the above raw materials, grinding to obtain precursor, mixing with NaNO 3 The molar ratio of the raw material of NaNO 3 1: 0.5. Transferring the precursor into a muffle furnace, calcining for 2h at 450 ℃ in air atmosphere, cooling to room temperature after the calcination time is over, and obtaining Li 2 Mg 2 (MoO 4 ) 3 -a salt mixture. The Li obtained above 2 Mg 2 (MoO 4 ) 3 Washing the salt mixture with deionized water for many times, filtering to remove salt components, and drying at 110 ℃ for 2h to obtain the rod-shaped Li 2 Mg 2 (MoO 4 ) 3 A material.
Example 7:
the present embodiment is mainly different from embodiment 1 in that: the molar ratio of the raw material to the molten salt is NaNO 3 1: 2.5. The preparation method comprises the following steps:
weighing LiOH & H according to stoichiometric ratio 2 O、MgO、MoO 3 Using NaNO as raw material 3 Mixing nitrate with the above raw materials, grinding to obtain precursor, mixing with NaNO 3 The molar ratio of the raw material of NaNO 3 1: 2.5. Transferring the precursor into a muffle furnace, calcining for 2h at 450 ℃ in air atmosphere, cooling to room temperature after the calcination time is over, and obtaining Li 2 Mg 2 (MoO 4 ) 3 -a salt mixture. The Li obtained above 2 Mg 2 (MoO 4 ) 3 Washing the salt mixture with deionized water for many times, filtering to remove salt components, and drying at 110 ℃ for 2h to obtain the rod-shaped Li 2 Mg 2 (MoO 4 ) 3 A material.
FIG. 1 shows Li prepared in example 1 2 Mg 2 (MoO 4 ) 3 The XRD spectrum of the material shows that no impurity peak appears in the diffraction peak, and the table shows thatClearly produce high purity Li 2 Mg 2 (MoO 4 ) 3 A material.
FIGS. 2 to 4 are Li prepared in examples 1 to 5, respectively 2 Mg 2 (MoO 4 ) 3 SEM image of the material, from which it can be seen that rod-like Li was obtained in each example 2 Mg 2 (MoO 4 ) 3 A material.
The foregoing illustrates and describes the general principles and features of the present invention. However, the above embodiments are only examples of the present invention, and the technical features of the present invention are not limited thereto, and all changes and modifications made within the claims of the present invention should be included in the scope of the present invention.

Claims (3)

1. Rod-shaped Li 2 Mg 2 (MoO 4 ) 3 The material being characterized in that the Li 2 Mg 2 (MoO 4 ) 3 The material has a remarkable rod-shaped structure, the diameter of the material is 0.3-0.65 μm, and the length of the material is 0.5-9 μm.
2. The rod-like Li of claim 1 2 Mg 2 (MoO 4 ) 3 The preparation method of the material is characterized by comprising the following steps:
(1) according to Li 2 Mg 2 (MoO 4 ) 3 Weighing lithium hydroxide, metal oxide of magnesium and metal oxide of molybdenum as raw materials according to a stoichiometric ratio, weighing nitrate, mixing the nitrate with the raw materials, and grinding to obtain a precursor, wherein the molar ratio of the raw materials to the nitrate is 1 (0.5-2.5);
(2) calcining the precursor obtained in the step (1) in an air atmosphere at the temperature of 350-550 ℃ for 1-5h, and after the calcination is finished, cooling to room temperature to obtain a mixture;
(3) washing the mixture obtained in the step (2) with deionized water for 4-6 times, filtering to remove salt components, and drying at the temperature of 110 ℃ for 2-3h to obtain rod-shaped Li 2 Mg 2 (MoO 4 ) 3 And (3) powder.
3. The method of claim 2The preparation method is characterized in that the nitrate is NaNO 3 。
CN202210666417.6A 2022-06-14 2022-06-14 Rod-shaped Li 2 Mg 2 (MoO 4 ) 3 Material and method for the production thereof Pending CN115108585A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116216786A (en) * 2023-01-19 2023-06-06 大连理工大学 Ca with cube structure 5 Co 4 (VO4) 6 Method for producing materials

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2830960A (en) * 1953-08-19 1958-04-15 Peter Spence & Sons Ltd Cobalt molybdate catalysts
CN108640152A (en) * 2018-06-01 2018-10-12 大连理工大学 One kind having one-dimensional micro-nanometer stick LiMgVO4Material and preparation method
CN112830515A (en) * 2021-01-19 2021-05-25 大连理工大学 NaMg with octahedral structure4V3O12Method for producing a material
CN114162869A (en) * 2022-01-05 2022-03-11 大连理工大学 Li with micro-nano rod-shaped structure2Zn2Mo3O12Material and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2830960A (en) * 1953-08-19 1958-04-15 Peter Spence & Sons Ltd Cobalt molybdate catalysts
CN108640152A (en) * 2018-06-01 2018-10-12 大连理工大学 One kind having one-dimensional micro-nanometer stick LiMgVO4Material and preparation method
CN112830515A (en) * 2021-01-19 2021-05-25 大连理工大学 NaMg with octahedral structure4V3O12Method for producing a material
CN114162869A (en) * 2022-01-05 2022-03-11 大连理工大学 Li with micro-nano rod-shaped structure2Zn2Mo3O12Material and preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
F.A. DANEVICH ET AL.: "Growth and characterization of a Li2Mg2(MoO4)3 scintillating bolometer", NUCLEAR INST. AND METHODS IN PHYSICS RESEARCH, A, no. 889, pages 89 - 96 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116216786A (en) * 2023-01-19 2023-06-06 大连理工大学 Ca with cube structure 5 Co 4 (VO4) 6 Method for producing materials
CN116216786B (en) * 2023-01-19 2023-11-03 大连理工大学 Ca with cube structure 5 Co 4 (VO 4 ) 6 Method for producing materials

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