Preparation method of large-size lath-shaped artificial ruby crystal

A lath-shaped ruby ​​technology, applied in crystal growth, chemical instruments and methods, single crystal growth, etc., can solve the problems of slow ruby ​​crystal speed, poor uniformity, and high growth cost, and achieve the suppression of Cr3+ ion volatilization , Crystal physical properties are excellent, the effect of improving crystal utilization

Inactive Publication Date: 2020-08-11
CHINA ELECTRONICS TECH GRP NO 26 RES INST
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Problems solved by technology

[0004] At present, the methods for growing red gemstone single crystal mainly include flame method, pulling method, flux method, hydrothermal method, etc. The production cost of flame method is low, but the crystal size is small, the quality is poor, and the uniformity is not good. Larger-sized ruby ​​crystals can be grown, but because the melting point of ruby ​​is 2040°C, expensive iridium

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  • Preparation method of large-size lath-shaped artificial ruby crystal

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preparation example Construction

[0031] The invention provides a method for preparing a large-size lath-shaped artificial ruby ​​crystal, comprising the following steps:

[0032] A: The mixed material of 5N alumina polycrystalline material and chromium oxide powder is used as a raw material and put into a molybdenum boat-shaped crucible;

[0033] B: Put the seed crystal in the seed crystal tank at the middle position on the top of the boat-shaped crucible, put the crucible into the crystal furnace, place a reflective screen around the crucible, close the crystal furnace, and turn on the circulating water cooling system of the crystal furnace;

[0034] C: Turn on the vacuum pump to make the air pressure in the crystal furnace reach 2×10 -4 Below Pa;

[0035] D: Fill hydrogen into the crystal furnace until the air pressure in the crystal furnace reaches 1.4×10 5 Pa~1.6×10 5 Stop hydrogen injection after Pa;

[0036] E: The crystal furnace heating system increases the internal temperature of the crystal furn...

Embodiment 1

[0048] In this example, a piece of ruby ​​crystal with a size of 200×95×32 mm and a color of darker red pigeon’s blood red was prepared, and the preparation method included:

[0049] Select 2156.00g of 5N polycrystalline alumina and 44.00g of 5N chromium oxide powder, and put them into a boat-shaped molybdenum crucible with a size of 200×100×40mm;

[0050] Put the crucible containing the raw materials into the horizontal directional crystal growth furnace, place a heat shield around it, close the crystal furnace, turn on the circulating water, and evacuate to 2×10 -4 Pa, close the vacuum;

[0051] Fill in hydrogen to make the pressure in the crystal furnace reach 1.5×10 5 Pa, stop hydrogen filling, start to heat up;

[0052] Raise the temperature in the crystal furnace to about 2050 °. The power of the crystal furnace used in this embodiment is 31 kilowatts at this time. At this time, it is found that the powder melts, and obvious liquid streamlines appear near the seed crys...

Embodiment 2

[0060] In this embodiment, a light red ruby ​​crystal with a size of 220×120×40 mm and a lighter color is prepared, and the preparation method includes:

[0061] Select 3193.60g of 5N polycrystalline alumina and 6.40g of 5N chromium oxide powder, and put them into a boat-shaped molybdenum crucible with a size of 220×120×40mm;

[0062] Put the crucible containing the raw materials into the horizontal oriented crystal growth furnace, put a heat shield around it, close the crystal furnace, turn on the circulating water, and evacuate to 1×10 -4 Pa, close the vacuum;

[0063] Charge hydrogen to make the pressure in the crystal furnace reach 1.55×10 5 Pa, stop hydrogen filling, start to heat up;

[0064] When the temperature was raised to 31 kW, it was found that the powder melted, and obvious liquid streamlines appeared near the seed crystal. The crucible was moved to bring the seed crystal close to the high temperature area and observed, and it was found that the edge of the see...

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Abstract

The invention belongs to the technical field of artificial single crystal preparation, and particularly relates to a preparation method of large-size lath-shaped artificial ruby crystal. The preparation method comprises the following steps: putting raw materials into a boat-shaped molybdenum crucible, and injecting hydrogen under the condition that the air pressure in a crystal furnace is lower than 2 * 10 <-4 > Pa to enable the air pressure in the crystal furnace to reach about 1.5 * 10 < 5 > Pa; raising the temperature in the crystal furnace to completely melt the raw materials; adjusting the position of the crucible to complete seeding, crystal shouldering growth and crystal equal-width growth; cooling the crystal furnace, and taking out the prepared ruby crystal. A horizontal directional crystallization method is utilized, the advantages of a directional crystallization method and a vertical zone melting method are achieved at the same time, and the method for preparing ruby has the advantages of being low in cost, short in period, large in size, high in crystal quality, good in product uniformity, adjustable in color size and the like.

Description

technical field [0001] The invention belongs to the technical field of artificial single crystal preparation, and in particular relates to a method for preparing large-scale lath-shaped artificial ruby ​​crystals. Background technique [0002] Artificial red gemstones are made of corundum (α-Al 2 o 3 ) doped with a small amount of Cr 2 o 3 The formed single crystal, because the doped Cr3+ ions can absorb part of the visible light band, so that the crystal appears red. [0003] The crystal structure and physical and chemical properties of artificial ruby ​​​​are the same as those of natural ruby. It also has the characteristics of high hardness (second only to diamond), bright color, high refractive index, and large dispersion coefficient. It is a crystal widely used in high-end jewelry. Material. [0004] At present, the methods for growing red gemstone single crystal mainly include flame method, pulling method, flux method, hydrothermal method, etc. The production cost...

Claims

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Application Information

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IPC IPC(8): C30B29/20C30B11/00C30B11/14
CPCC30B11/00C30B11/006C30B11/14C30B29/20
Inventor 顾跃丁雨憧李海林姜磊
Owner CHINA ELECTRONICS TECH GRP NO 26 RES INST
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