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A (la 1 - x ln x ) 2 (moo 4 ) 3 Direct method for the preparation of thin films

A thin film and direct technology, applied in the field of materials science, can solve the problems of high synthesis temperature, high synthesis conditions, and insufficient powder particle size, and achieve the effect of simplifying the preparation method, good film quality, and avoiding influence.

Active Publication Date: 2019-07-23
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The principle of the sol-gel method is that an alkoxide or an ester compound is dissolved in an organic solvent, and undergoes a hydrolysis reaction to form an active monomer. The monomer is then polymerized to form a sol, and the sol is polymerized to form a gel with a certain spatial structure, and then dried. And heat treatment to remove the organic matter, sintering and solidification to form the required nanomaterials. The nanomaterials of the molybdate system prepared by this method are mostly nanorods with uneven surfaces, and are prone to agglomeration. Materials with this shape are not suitable for making Film formation; the hydrothermal method is to create a high temperature and high pressure environment to dissolve the insoluble or insoluble substances under atmospheric conditions, or to react to form the dissolved products of the substances, and to convect the reactants by controlling the temperature difference of the solution in the autoclave. A supersaturated state is formed to precipitate growth crystals. The nanomaterials of the molybdate system prepared by this method are mostly in the shape of flowers, and each flower is composed of multiple nanosheets, and these nanosheets are stable enough and not easy to disperse. The similar morphology is also not suitable for making thin films; solid-phase method generally refers to a method that uses solid-phase substances to participate and produce powders through phase changes. The powders prepared by this method are not fine enough and not uniform, so It is also impossible to obtain the ideal morphology for preparing high-quality thin films; microwave synthesis is widely used in nano During the synthesis process of the material, the morphology of the product prepared by the microwave method is prone to agglomeration, so the obtained product is still not ideal for the preparation of high-quality thin films
[0003] In summary, the synthesis conditions of the above methods are relatively high, which is reflected in the high synthesis temperature and high requirements on the reaction vessel; except for the microwave method, the synthesis process of other methods takes a long time; the most important thing is to use the above The morphology of the nanomaterials obtained by the method is not suitable for the preparation of high-quality light-emitting films, which greatly limits its application

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  • A (la  <sub>1</sub> -  <sub>x</sub> ln  <sub>x</sub> )  <sub>2</sub> (moo  <sub>4</sub> )  <sub>3</sub> Direct method for the preparation of thin films
  • A (la  <sub>1</sub> -  <sub>x</sub> ln  <sub>x</sub> )  <sub>2</sub> (moo  <sub>4</sub> )  <sub>3</sub> Direct method for the preparation of thin films
  • A (la  <sub>1</sub> -  <sub>x</sub> ln  <sub>x</sub> )  <sub>2</sub> (moo  <sub>4</sub> )  <sub>3</sub> Direct method for the preparation of thin films

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Lanthanum (La) nitric acid compound, rare earth element (Ln) nitric acid compound, ethylenediaminetetraacetic acid (EDTA), NaOH, Na 2 MoO 4 2H 2 O, KCl, HNO 3 All commercially available analytical pure chemical reagents.

[0024] Concrete preparation steps are as follows:

[0025] (1) La(NO 3 ) 3 ·6H 2 O was dissolved in deionized water to prepare a rare earth ion solution with a total concentration of rare earth ions of 0.01mol / L, and then ethylenediaminetetraacetic acid (EDTA) was added to the above In the rare earth ion solution, add 0.5mol / L NaOH solution dropwise until the pH value of the mixed solution reaches 12.5, and finally add NaOH solution 2 MoO 4 2H 2 O, KCl and HNO 3 , where Na 2 MoO 4 2H 2 The molar ratio of the amount of O added to the total amount of rare earth ions is 2:1, the molar ratio of KCl to the total amount of rare earth ions is 25:1, and the molar ratio of HNO 3 The added amount is used to adjust the pH value of the mixed solutio...

Embodiment 2

[0033] Lanthanum (La) nitric acid compound, rare earth element (Ln) nitric acid compound, ethylenediaminetetraacetic acid (EDTA), NaOH, Na 2 MoO 4 2H 2 O, KCl, HNO 3 All commercially available analytical pure chemical reagents.

[0034] Concrete preparation steps are as follows:

[0035] (1) La(NO 3 ) 3 ·6H 2 O and Eu(NO 3 ) 3 ·6H 2 O is dissolved in deionized water according to the molar ratio of La / Eu=19 / 1 to prepare a rare earth ion solution with a total concentration of rare earth ions of 0.05mol / L, and then add ethylenediaminetetraacetic acid according to the molar ratio of the total amount of rare earth ions Add it to the above rare earth ion solution at a ratio of 1:1, then add 1mol / L NaOH solution dropwise until the pH value of the mixed solution reaches 12.5, and finally add NaOH 2 MoO 4 2H 2 O, KCl and HNO 3 , where Na 2 MoO 4 2H 2 The molar ratio of the amount of O added to the total amount of rare earth ions is 3:1, the molar ratio of KCl to the tot...

Embodiment 3

[0043] Lanthanum (La) nitric acid compound, rare earth element (Ln) nitric acid compound, citric acid, NaOH, Na 2 MoO 4 2H 2 O, KCl, HNO 3 All commercially available analytical pure chemical reagents.

[0044] Concrete preparation steps are as follows:

[0045] (1) La(NO 3 ) 3 ·6H 2 O and Tb(NO 3 ) 3 ·6H 2 O is dissolved in deionized water according to the molar ratio of La / Tb=97 / 3 to prepare a rare earth ion solution with a total concentration of rare earth ions of 0.5mol / L, and then citric acid is 1 according to the molar ratio of the total amount of rare earth ions. :1 ratio into the above-mentioned rare earth ion solution, then dropwise add 1mol / L NaOH solution until the pH value of the mixed solution reaches 12.7, and finally add NaOH solution 2 MoO 4 2H 2 O, KCl and HNO 3 , where Na 2 MoO 4 2H 2 The molar ratio of the amount of O added to the total amount of rare earth ions is 1:1, the molar ratio of KCl to the total amount of rare earth ions is 10:1, and...

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Abstract

The invention discloses a (La 1‑x ln x ) 2 (MoO 4 ) 3 A direct method for the preparation of thin films. La(NO 3 ) 3 ·6H 2 O or La(NO 3 ) 3 ·6H 2 O and Ln(NO 3 ) 3 ·6H 2 O was dissolved in deionized water to prepare a solution with a total concentration of rare earth ions of 0.005~1mol / L, and EDTA or citric acid, NaOH solution, Na 2 MoO 4 2H 2 O, KCl and HNO 3 After mixing evenly, the electrodeposition solution is obtained, placed in a water bath, and its temperature reaches the required temperature; a three-electrode system is inserted in the electrodeposition solution, and a thin film is deposited on the conductive glass through the electrodeposition reaction, and the thin film is respectively used Rinse with deionized water and absolute ethanol, then place in a blast drying oven to dry, then place the dried electrodeposited film in a tube furnace for heat treatment, and obtain (La 1‑x ln x ) 2 (MoO 4 ) 3 film. The invention is simple to operate, and compared with the traditional method of making powder first and then forming a film, it greatly simplifies the film preparation method, and at the same time avoids the influence of the powder shape on the quality of the film; and the method provided by the invention is simple to operate and time-consuming Short, good film quality.

Description

technical field [0001] The invention belongs to the technical field of materials science, in particular to a kind of (La 1-x Ln x ) 2 (MoO 4 ) 3 A direct method for the preparation of thin films. Background technique [0002] Rare earth luminescent materials of the molybdate system are used as fluorescent materials in the fields of solid-state lighting, flat panel displays, lasers, etc. due to their good chemical stability and high fluorescence quantum efficiency, and the preparation of fluorescent materials into corresponding thin films is An important prerequisite for the deviceization of luminescent materials. At present, there are many methods to prepare rare earth molybdate materials with different morphologies, such as sol-gel method, hydrothermal method, solid phase method, microwave method and so on. The principle of the sol-gel method is that an alkoxide or an ester compound is dissolved in an organic solvent, and undergoes a hydrolysis reaction to form an act...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D9/06
Inventor 武晓鹂张铁龙飞郑国源邹正光
Owner GUILIN UNIVERSITY OF TECHNOLOGY