CN108821343B

CN108821343B - Slice Y2W3O12Method of synthesis of

Info

Publication number: CN108821343B
Application number: CN201810750126.9A
Authority: CN
Inventors: 汪元元
Original assignee: Hefei Cuili New Material Technology Co ltd
Current assignee: Hefei Cuili New Material Technology Co ltd
Priority date: 2018-07-02
Filing date: 2018-07-02
Publication date: 2020-07-28
Anticipated expiration: 2038-07-02
Also published as: CN108821343A

Abstract

The invention provides a sheet Y₂W₃O₁₂The synthesis method is characterized by comprising the following steps: dissolving tungstate and yttrium salt in N, N-dimethylAdding oxalic acid and a template agent into dimethylformamide at an atomic ratio of Y to W of 2 to 3, uniformly stirring, transferring the solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, screwing up and sealing, and standing and reacting in a constant-temperature oven at 200-220 ℃ for 8-12 hours; filtering the precipitate after the reaction is finished, and repeatedly cleaning the precipitate with deionized water until the pH value is 7-8; and filtering and separating out precipitates by adopting a centrifuge precipitation or suction filtration device, and drying in a drying oven at 50-70 ℃ to obtain a final product. The invention has the advantages of cheap raw materials, simple process and synthesized flake Y, and the synthesis method adopts a full liquid phase chemical reaction process₂W₃O₁₂The appearance control is stable, and the product can be used as a filler of an electronic packaging metal carrier or a polymer carrier and has the function of compensating thermal expansion.

Description

Slice Y2W3O12Method of synthesis of

Technical Field

The invention belongs to the technical field of material chemistry, and relates to a flaky Y₂W₃O₁₂The method of (1).

Background

With the development of science and technology, various electronic products increasingly show the trend of miniaturization and multi-functionalization, and the requirement on the reliability of the electronic products is higher and higher. The thermal expansion characteristics of the circuit board carrier greatly affect the reliability of the electronic device. Rare earth tungstate Y₂W₃O₁₂The composite packaging material has remarkable negative thermal expansion performance, and can be prepared by matching metal powder metallurgy or blending with a high polymer material according to a proper component ratio. Y is₂W₃O₁₂Common preparation methods of the particles include a solid phase method, a sol-gel method, a combustion method, a coprecipitation method, and the like. Sheet Y₂W₃O₁₂The synthesis of (A) is only rarely reported at present.

Disclosure of Invention

The invention aims to provide a sheet Y₂W₃O₁₂The synthesis method is characterized by comprising the following steps: dissolving tungstate and yttrium salt in N, N-dimethylformamide at an atomic ratio of Y to W of 2 to 3, adding oxalic acid and a template agent, uniformly stirring, transferring the solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, screwing up and sealing, and standing in a constant-temperature oven at 200-220 ℃ for reaction for 8-12 hours; filtering the precipitate after the reaction is finished, and repeatedly cleaning the precipitate with deionized water until the pH value is 7-8; and filtering and separating out precipitates by adopting a centrifuge precipitation or suction filtration device, and drying in a drying oven at 50-70 ℃ to obtain a final product.

The tungstate comprises one or a combination of ammonium tungstate, ammonium metatungstate, sodium tungstate and potassium tungstate, the yttrium salt comprises one or a combination of yttrium nitrate and yttrium chloride, and the concentration of the yttrium salt in the N, N-dimethylformamide is 0.1-0.15 mol/L.

The template agent comprises one or a combination of α -naphthalenesulfonic acid, β -naphthalenesulfonic acid, 1, 5-dinaphthalenesulfonic acid and 2, 4-dinitronaphthol-7-sulfonic acid, the equivalent concentration of the template agent in the mixed solution is 0.15-0.2 mol/L, and the equivalent concentration of oxalic acid in the solution is 1.5-3 mol/L.

The invention has the advantages of cheap raw materials, simple process and synthesized flake Y, and the synthesis method adopts a full liquid phase chemical reaction process₂W₃O₁₂The appearance control is stable, and the product can be used as a filler of an electronic packaging metal carrier or a polymer carrier and has the function of compensating thermal expansion.

While the invention has been disclosed in the foregoing description with reference to specific embodiments thereof, the foregoing description is directed to only certain specific embodiments of the invention and many more specific features of the invention may be employed than as disclosed herein. Therefore, the scope of the present invention should not be limited to the disclosure of the embodiments, but should include all combinations of the contents embodied in different parts, and various substitutions and modifications without departing from the present invention, and are covered by the claims of the present invention.

Drawings

FIG. 1 shows the synthesis of sheet Y according to the invention (example 1)₂W₃O₁₂SEM photograph of (a).

Detailed Description

Example 1

Dissolving 0.225 mol/L ammonium tungstate and 0.1-0.15 mol/L yttrium nitrate in N, N-dimethylformamide, adding 3 mol/L oxalic acid and 0.2 mol/Lα -naphthalenesulfonic acid, stirring uniformly, transferring the solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, screwing, sealing, placing into a constant-temperature oven at 220 ℃ for standing reaction for 8 hours, filtering and precipitating after the reaction is finished, repeatedly washing with deionized water until the pH value is 7-8, filtering and separating out precipitate by using a centrifuge or suction filtration equipment, placing into an oven at 70 ℃ for drying to obtain the final product sheet-shaped Y shown in figure 1₂W₃O₁₂。

Example 2

Will be 0.225Dissolving ammonium metatungstate in mol/L and yttrium nitrate in 0.15 mol/L in N, N-dimethylformamide, adding oxalic acid in 2 mol/L and naphthalenesulfonic acid in 0.15 mol/Lβ, stirring, transferring the solution into a hydrothermal reaction kettle with a polytetrafluoroethylene liner, screwing and sealing, standing and reacting in a constant-temperature oven at 200 ℃ for 12 hours, filtering and precipitating after the reaction is finished, repeatedly cleaning with deionized water until the pH value is 7-8, filtering and separating out precipitate by using a centrifuge precipitation or suction filtration device, and drying in an oven at 70 ℃ to obtain the final product, namely the flaky Y₂W₃O₁₂。

Example 3

Dissolving 0.15 mol/L sodium tungstate and 0.1 mol/L yttrium chloride in N, N-dimethylformamide, adding 1.5 mol/L oxalic acid and 0.15 mol/L1, 5-dinaphthalenesulfonic acid, uniformly stirring, transferring the solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, screwing and sealing, placing the hydrothermal reaction kettle into a constant-temperature oven at 220 ℃ for standing reaction for 10 hours, filtering and precipitating after the reaction is finished, repeatedly washing the solution with deionized water until the pH value is 7-8, filtering and separating the precipitate by using a centrifuge precipitation or suction filtration equipment, placing the precipitate into an oven at 60 ℃ for drying to obtain the final product of flaky Y₂W₃O₁₂。

Example 4

Dissolving 0.15 mol/L potassium tungstate and 0.1 mol/L yttrium chloride in N, N-dimethylformamide, adding 2 mol/L oxalic acid and 0.2 mol/L2, 4-dinitronaphthol-7-sulfonic acid, uniformly stirring, transferring the solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, screwing, sealing, placing into a constant-temperature oven at 200 ℃ for standing reaction for 10 hours, filtering and precipitating after the reaction is finished, repeatedly washing with deionized water until the pH value is 7-8, filtering and separating out precipitate by using a centrifugal machine or a suction filtration device, placing into an oven at 60 ℃ for drying to obtain the final product of flaky Y₂W₃O₁₂。

Claims

1. Slice Y₂W₃O₁₂The synthesis method is characterized by comprising the following steps: dissolving tungstate and yttrium salt in N, N-dimethylformamide at an atomic ratio of Y to W of 2 to 3, adding oxalic acid and a template agent, and uniformly stirringTransferring the solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, screwing up and sealing, and putting the hydrothermal reaction kettle into a constant-temperature oven at 200-220 ℃ for standing reaction for 8-12 hours; filtering the precipitate after the reaction is finished, and repeatedly cleaning the precipitate with deionized water until the pH value is 7-8; filtering and separating out precipitate by adopting a centrifuge precipitation or suction filtration device, drying in a drying oven at 50-70 ℃ to obtain a final product,

2. Sheet Y according to claim 1₂W₃O₁₂The synthesis method is characterized in that the tungstate comprises one or a combination of ammonium tungstate, ammonium metatungstate, sodium tungstate and potassium tungstate, the yttrium salt comprises one or a combination of yttrium nitrate and yttrium chloride, and the concentration of the yttrium salt in the N, N-dimethylformamide is 0.1-0.15 mol/L.

3. The sheet Y of any one of claims 1 to 2₂W₃O₁₂The synthetic method of (2) prepared flake Y₂W₃O₁₂。