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Bridgman-stockbarger growth method for zirconium titanate crystals

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

Inactive Publication Date: 2014-10-08
上海晶生实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Zirconium titanate crystals have been widely used as a high refractive index film material, but there are almost no research reports on the preparation of zirconium titanate crystals. Therefore, there is a great need for a method that can grow zirconium titanate crystals at a lower cost. in order to facilitate industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach

[0057] The growth method mainly includes the following steps:

[0058] 1. Pretreatment of raw materials: TiO 2 (99.9%) and ZrO 2 (99.9%) are mixed according to the chemical composition of zirconium titanate, and the mixed powder is ground on a mortar or grinder to mix evenly, and pressed into blocks on an isostatic press as required;

[0059] 2. Put the briquetting material obtained in step 1. into the molybdenum crucible, transfer the molybdenum crucible to the high-temperature drop furnace, adjust to a certain height, power on the whole system to heat up after sealing, start the mechanical pump and diffusion pump successively, and evacuate to 10 -3 -10 -4 Pa, when the furnace temperature reaches 1350-1650°C, fill in an inert protective gas, and continue to heat up to the set temperature, and the set temperature is within the range of 1800-1950°C;

[0060] 3. After the furnace temperature reaches the set temperature, keep it warm for 2-6 hours to fully melt the raw materia...

Embodiment 1

[0077] TiO with a purity of 99.9% 2 and 99.9% ZrO 2 Mix the ingredients according to the mass percentage of 15:85, grind the mixed powder on the mortar or grinder and mix evenly, 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 to raise the temperature. The mechanical pump and the diffusion pump are started successively, and the vacuum is evacuated to 10 -3 Pa, when the furnace temperature reaches 1500°C, fill it with 99.99% argon, continue to heat up to 1930°C, keep the temperature for 3 hours to completely melt the raw materials, and maintain the temperature gradient of the growth interface at about 20°C / cm at a rate of 1.5mm / h Lower the crucible, keep warm for 12 hours after the crystal growth is completed, slowly cool down to room temperature at a rate o...

Embodiment 2

[0079] TiO with a purity of 99.9% 2 and 99.9% ZrO 2 Mix the ingredients according to the mass percentage of 5:95, grind the mixed powder on the mortar or grinder and mix evenly, 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 -4Pa, when the furnace temperature reaches 1380°C, fill it with 99.99% argon, continue to heat up, control the furnace temperature at 1950°C, and keep it warm for 4 hours to completely melt the raw materials. Decrease the crucible at a rate of mm / h. After the crystal growth is complete, keep it warm for 18 hours, then slowly cool down to room temperature at a rate of about 40°C / h, and take out the zirconium titanate crystal. According to GB / T7962.12-1987 colorless optical glass test method, t...

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Abstract

The invention provides a bridgman-stockbarger growth method for zirconium titanate crystals. The method comprises the following steps: (1) providing a crucible with a pressing block raw material, wherein the pressing block raw material is prepared by matching 5-90% by mass of TiO2 and 10-95% by mass of ZrO2, uniformly mixing and pressing into blocks; (2) putting the crucible into a high temperature dropping furnace, heating and vacuuming till 10<-3>-10<-4>Pa, introducing an inert protecting gas when the temperature of the furnace is 1350-1650 DEG C, and heating to a set temperature within a range of 1800-1950 DEG C; (3) after the temperature of the furnace achieves the set temperature, keeping the temperature for 2-6 hours to sufficiently melt the raw materials, wherein the temperature gradient of solid-liquid boundary of crystal growth is within the range of 15-60 DEG C / cm, and the crucible dropping velocity is within 0.1-6.0mm / h; and (4) after the crystal growth is completed, keeping the temperature for 12-24 hours, cooling to be the room temperature in the speed of 25-65 DEG C / h, and performing annealing treatment on the grown crystal. The invention provides the bridgman-stockbarger growth method which is simple in operation method, low in growth cost and stable in quality for zirconium titanate crystals, and thus industrial preparation of crystals is achieved.

Description

technical field [0001] The invention relates to a crucible-drop method growth technology for crystals, that is, a crucible-drop method is used to grow zirconium titanate crystals, and belongs to the field of crystal growth. Background technique [0002] Zirconium titanate is an important electronic ceramic material with extremely low dielectric loss, high dielectric constant and quality factor, and good frequency stability. It is ideal for preparing capacitors, piezoelectric sensors and microwave dielectric resonators preferred material. Zirconium titanate material also has good high-temperature performance, and its melting point is about 1820°C, so it can be used as a high-temperature structural material. [0003] At present, zirconium titanate is also widely used as an evaporation material for high refractive index coatings in the manufacture of optoelectronic devices, such as display technology, imaging technology, light output and light integration devices, etc. The zi...

Claims

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Application Information

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IPC IPC(8): C30B29/32C30B11/00
Inventor 吴宪君马军陈灯华
Owner 上海晶生实业有限公司
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