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Method for preparing beta-phase trititanium pentoxide crystal sheet

A technology of titanium pentoxide and crystal flakes is applied in the field of preparation of flake titanium pentoxide crystals, which can solve the problems of inability to meet the requirements of high-precision coating materials, poor phase stability, and difference in refractive index, and shorten the pre-melting time. , good phase stability, low equipment requirements

Inactive Publication Date: 2019-05-03
XUZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The experimental data show that the encapsulation of phenolic resin is good after carbonization, and the reduction performance is stable, but the reaction intermediate products are λ phase and γ phase Ti 3 o 5 , its phase stability is poor, and the temperature changes significantly, resulting in a difference in refractive index, which cannot meet the requirements of high-precision coating materials

Method used

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  • Method for preparing beta-phase trititanium pentoxide crystal sheet
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  • Method for preparing beta-phase trititanium pentoxide crystal sheet

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step 1: According to the mass ratio of phenolic resin: titanium dioxide = 1:10.5, weigh the raw materials of phenolic resin and titanium dioxide respectively. The phenolic resin is pre-dissolved in anhydrous ethanol first, and after fully dissolving, add titanium dioxide and mix it by ball milling for 24 hours. The speed of ball milling is 200r / min. The mass ratio of absolute ethanol to mixed powder is 1.5:1; after ball milling, take out the material and dry it in a drying oven at 60°C, take out the mixed material after drying, pass through a 100-mesh sieve after mechanical grinding; adopt dry pressing, the pressure is 1.5MPa, the time is 60s, and the mixture is pressed into tablets;

[0033] Step 2: Put the mixed material tablet obtained in step 1 into a crucible and place it in a muffle furnace, and pass argon gas into the furnace cavity for 20 minutes to exhaust the air in the furnace cavity;

[0034] Step 3: Sintering in stages, and continuously feed argon gas throu...

Embodiment 2

[0044] Step 1: According to the mass ratio of phenolic resin: titanium dioxide = 1:9.5, weigh the raw materials of phenolic resin and titanium dioxide respectively. The phenolic resin is pre-dissolved in anhydrous ethanol first, and after fully dissolving, add titanium dioxide and mix for 28 hours by ball milling. The speed of ball milling is 60r / min. The mass ratio of absolute ethanol to the mixed powder is 3.5:1; after ball milling, the material is taken out and dried in a 60°C drying oven. After drying, the mixed material is taken out and passed through a 100-mesh sieve after mechanical grinding; it is formed by dry pressing at a pressure of 4MPa, the time is 15s, and the mixture is pressed into tablets;

[0045] Step 2: Put the mixed material tablet obtained in step 1 into a crucible and place it in a muffle furnace, and pass argon gas into the furnace cavity for 20 minutes to exhaust the air in the furnace cavity;

[0046] Step 3: Sintering in stages, and continuously fee...

Embodiment 3

[0055] Step 1: According to the mass ratio of phenolic resin: titanium dioxide = 1:10, weigh the raw materials of phenolic resin and titanium dioxide respectively. The phenolic resin is pre-dissolved in anhydrous ethanol, and after fully dissolving, add titanium dioxide, mix for 24 hours by ball milling, and the ball milling speed is 200r / min. The mass ratio of absolute ethanol to mixed powder is 2:1; after ball milling, take out the material and dry it in a drying oven at 100°C, take out the mixed material after complete drying, pass through a 100-mesh sieve after mechanical grinding; adopt dry pressing, the pressure is 2MPa, the time is 20s, followed by cold isostatic pressing, the parameter is 300MPa, the time is 150s, and the mixed material is obtained;

[0056] Step 2: Put the mixed material tablet obtained in step 1 into a crucible and place it in a muffle furnace, and pass nitrogen into the furnace cavity for 20 minutes to exhaust the air in the furnace cavity;

[0057]...

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Abstract

The invention discloses a method for preparing a beta-phase trititanium pentoxide crystal sheet, which includes the steps of: according to mass ratio of phenolic resin to TiO2 = 1:8.5-10, weighing rawmaterials phenolic resin and TiO2, pre-dissolving the phenolic resin in an organic solvent completely, and adding the TiO2 to perform ball-milling and mixing, drying, grinding, sieving and tablettingoperations; stepwise sintering the mixture in inert atmosphere and cooling the mixture to obtain the crystal sheet. The method can be used for preparing the sheet-like trititanium pentoxide, whereinthe crystalline phase is beta phase, purity reaches 99.99% and yield is 83-85%. The sheet-like trititanium pentoxide crystal can shorten the pre-melting time of film plating and improve film plating efficiency. By means of the physical ball-milling and mixing operation, the product is directly prepared by sintering the raw materials at the temperature zone nearby 1300 DEG C in one step without useof a vacuum environment. The method is low in equipment requirement, is greatly improved in controllability and safety, and is also greatly reduced in production cost.

Description

technical field [0001] The invention relates to the fields of coating materials, catalytic chemical materials, data storage and new energy, in particular to a preparation method of flaky trititanium pentoxide crystals. Background technique [0002] Titanium pentoxide is a blue-black non-stoichiometric compound with metallic luster. Its density is about 4.29g / cm 3 , melting point 2180°C, oxygen-titanium atomic ratio between 1.66 and 1.70, has five crystal phases (ɑ, β, λ, γ, δ), has both semiconductor and metal properties, acid and alkali corrosion resistance, and can replace noble metals as electrodes Material. And because of its small temperature resistance coefficient, but the resistance can change with the change of atmosphere, it is also a potential oxygen sensitive material. [0003] Titanium dioxide thin film has excellent mechanical, chemical, optical and electrical properties, and is the most important dielectric thin film material in optical and electronic applic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/46C04B35/622C04B35/626
Inventor 张乐杨顺顺魏帅陈浩
Owner XUZHOU NORMAL UNIVERSITY
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