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Growing method by Ti3O5 by bridgman method

A crucible descending method, a technology of titanium pentoxide, applied in the directions of crystal growth, single crystal growth, single crystal growth, etc.

Active Publication Date: 2010-06-02
苏州晶生新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ti 3 o 5 Crystal has been widely used as a high refractive index film material, but about Ti 3 o 5 There are almost no research reports on crystal preparation. Therefore, there is a great need for a method that can grow Ti at a lower cost. 3 o 5 Method of crystallization for advantageous industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] TiO with a purity of 99.9% 2 and 99.99% Ti by Ti 3 o 5 The chemical composition ingredients are mixed, and the mixed powder is ground and mixed evenly on a mortar or grinder, at 2t / cm 2 Press into pellets under isostatic pressure; then place the pellets in a cylindrical molybdenum crucible. The molybdenum crucible is placed in the lowering furnace and adjusted to the high temperature zone. After the whole system is sealed, it is powered on and heated up. The mechanical pump and the diffusion pump are started successively to vacuumize to 10-3Pa. When the furnace temperature reaches 1500°C, it is filled with 99.99% argon. , continue to heat up to 1850°C, keep the temperature for 3 hours to completely melt the raw materials, maintain the temperature gradient of the growth interface at about 30°C / cm, lower the crucible at a rate of 1.0mm / h, and grow Ti 3 o 5 Crystal, according to GB / T 7962.12-1987 test method for colorless optical glass, the Ti 3 o 5 The refractive in...

Embodiment 2

[0042] TiO with a purity of 99.9% 2 and 99.99% Ti by Ti 3 o 5 The chemical composition ingredients are mixed, and the mixed powder is ground and mixed evenly on a mortar or grinder, at 3t / cm 2 Press into pellets under isostatic pressure; then place the pellets in a cylindrical molybdenum crucible. The molybdenum crucible is placed in the descending furnace and adjusted to the high temperature zone. After the whole system is sealed, it is energized and heated, and the vacuum is pumped to 10 -4 Pa, when the furnace temperature reaches 1600°C, fill it with 99.99% argon, continue to heat up, control the furnace temperature at 1800°C, and keep it warm for 4 hours to completely melt the raw materials. The rate of mm / h drops the crucible and grows Ti 3 o 5 crystals. According to GB / T 7962.12-1987 colorless optical glass test method, the Ti 3 o 5 The refractive index (n) of the crystal at a wavelength of 560nm (λ) is 2.308.

Embodiment 3

[0044] TiO with a purity of 99.9% 2 and 99.99% Ti by Ti 3 o 5 The chemical composition ingredients are mixed, the mixed powder is ground and mixed evenly on a mortar or grinder, and pressed into a round block; respectively put into three molybdenum crucibles with a diameter of 70mm, and then placed in a high-temperature drop furnace with three crucible positions, Adjust to the position of the high temperature zone. After the whole system is sealed, it is energized and heated up, and the vacuum is pumped to 10 -3 Pa, when the furnace temperature reaches 1700°C, fill it with 99.99% argon, continue to raise the temperature, and control the furnace temperature at 1900°C. Adjust the positions of the three crucibles into the furnace respectively, and keep them warm for 3 hours to completely melt the raw materials. The temperature gradient of the growth interface is about 60°C / cm, and the crucible descending rate is 3.0mm / h. Three crucibles Ti can be obtained at the same time. 3 o...

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Abstract

The invention provides the bridgman growing method for the growth of Ti3O5 crystal, which includes that (1) the raw materials TiO2 and Ti are in proportioning according to Ti3O5 and mixed evenly, pressed. (2) The raw briquetting is loaded in a crucible that then transferred to the inside of a high-temperature decreasing furnace, and the whole system is heated and pumped to 10-3-10-4Pa. When the furnace temperature reaches 1400 to 1700 DEG C, the furnace is charged with an insert protection gas and continuously heated to 1800 to 1900 DEG C. (3) When the temperature reaches the set temperature,the heat is preserved for 3 to 6 hours so that the raw materials can be fully melted. The temperature gradient of solid-liquid interface for the crystal growth is within a framework of 20 to 60 DEG C / cm, and the crucible decline rate is between 0.1 to 5.0mm / h. (4) After the end of the crystal growth, in an appropriate position inside the growing furnace, the heat is preserved for 10 to 24 hours. Afterwards, the furnace temperature is reduced to a room temperature with the speed of 25 to 80 DEG C / h. The annealing treatment is implemented for the growing crystals.

Description

technical field [0001] The invention relates to a crystal growth technology by a crucible drop method, that is, a crucible drop method is used to grow trititanium pentoxide crystals, and belongs to the field of crystal growth. Background technique [0002] Titanium pentoxide (Ti 3 o 5 ) crystals belong to the orthorhombic system, with a density of ~4.60g / cm3 and a melting point of ~1760°C. Ti 3 o 5 It is a relatively stable compound in the low-priced series of titanium oxides. It has metal-like properties and high conductivity at room temperature. Compared with noble metal electrode materials, it is cheap and has strong acid and alkali corrosion resistance, so it can be used As an electrode material to replace noble metals. Ti 3 o 5 It is a non-stoichiometric compound, O / Ti can vary between 1.66-1.70, it contains a large number of oxygen vacancies, the concentration of quasi-free electrons is high, and its resistance can change with the change of the atmosphere, so it...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/16C30B11/00
Inventor 李新华吴宪君
Owner 苏州晶生新材料有限公司
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