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Preparation method of barium titanium silicate crystal

A barium silicate and crystal technology is applied in the field of preparation of barium and titanium silicate crystals, which can solve the problems of inability to purchase crystals in the market, high requirements, and difficulty in realization.

Inactive Publication Date: 2011-02-16
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Scientist J.T.Alfors et al first reported barium titanium silicon oxide Ba in 1965 2 TiSi 2 o 8 The existence of compounds; in 1985, S.A.Markgraf et al obtained the Ba used for single crystal structure analysis through the pulling method 2 TiSi 2 o 8 However, this method has high requirements on the growth furnace and is not easy to realize. In addition, to test the basic physical properties of a crystal, the size of the crystal needs to reach several millimeters or even centimeters. Ba for physical property test 2 TiSi 2 o 8 The report of single crystal, more can't buy this crystal on the market, the present invention aims at preparing large size Ba 2 TiSi 2 o 8 single crystal

Method used

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  • Preparation method of barium titanium silicate crystal
  • Preparation method of barium titanium silicate crystal
  • Preparation method of barium titanium silicate crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Take reaction formula (1) as an example: but not limited to reaction formula (1)

[0031] BaO+SiO 2 +TiO 2 →Ba 2 TiSi 2 o 8 Synthesis of Ba 2 TiSi 2 o 8 compound, the specific steps are as follows:

[0032] BaO, SiO 2 、TiO 2 Put it into a mortar with a stoichiometric ratio of 2:2:1, mix it evenly and grind it carefully, then put it into a corundum crucible with an opening of Φ200mm×200mm, press it tightly, put it into a muffle furnace, and slowly heat up to 450°C , constant temperature for 5 hours, try to drive out the gas, take out the crucible after cooling, grind the sample evenly, then put it in the crucible, keep it in the muffle furnace at 720°C for 5 hours, wait until the temperature drops to room temperature, take it out carefully Grind, keep the temperature at 1200°C for 24 hours again, put it into a mortar after cooling, and grind it slightly to get completely sintered barium titanium silicate (Ba 2 TiSi 2 o 8 ) compound, and the product is subjec...

Embodiment 2

[0036] Take reaction formula (3) as an example: but not limited to reaction formula (3)

[0037] Ba(NO 3 ) 2 +SiO2 2 +TiO 2 →Ba 2 TiSi 2 o 8 +NO 2 ↑ Synthesis of Ba 2 TiSi 2 o 8 Compound, specific operation steps are carried out according to embodiment 1:

[0038] The synthesized Ba 2 TiSi 2 o 8 Compounds and Fluxes LiF and B 2 o 3 Massive Ba 2 TiSi 2 o 8 :LiF:B 2 o 3 = 1:4:2 for mixing, put into an open platinum crucible of Φ40mm×30mm, heat up to 1200°C, keep the temperature down to 890°C after 30 hours, and cut the optimized Ba 2 TiSi 2 o 8 The seed crystal is fixed on the lower end of the seed rod with a platinum wire, and the seed crystal is introduced into the crucible from the small hole on the top of the furnace, immersed in the liquid surface, and the seed crystal rotates reversibly at a rate of 50 rpm, and the rotation time in each direction is 7 minutes. The time interval is 0.8 minutes, keep the temperature for 20 minutes, quickly drop to 880°...

Embodiment 3

[0041] Take reaction formula (6) as an example: but not limited to reaction formula (6)

[0042] Ba(OH) 2 +SiO2 2 +TiO 2 →Ba 2 TiSi 2 o 8 +H 2 O ↑ Synthesis of Ba 2 TiSi 2 o 8 Compound, specific operation steps are carried out according to embodiment 1:

[0043] The synthesized Ba 2 TiSi 2 o 8 Compounds and Fluxes LiF and H 3 BO 3 Massive Ba 2 TiSi 2 o 8 :LiF:H 3 BO 3 = 1:5:2 for mixing, put into an open platinum crucible of Φ40mm×30mm, heat up to 1200°C, keep the temperature for 30 hours and then cool down to 870°C, the optimized Ba 2 TiSi 2 o 8 The seed crystal is fixed on the lower end of the seed rod with a platinum wire, and the seed crystal is introduced into the crucible from the small hole on the top of the furnace, immersed in the liquid surface, and the seed crystal rotates reversibly at a rate of 30 rpm, and the rotation time in each direction is 5 minutes. The time interval is 0.6 minutes, keep the temperature for 20 minutes, quickly drop to 8...

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Abstract

The invention relates to a preparation method of a barium titanium silicate crystal, comprising the following steps of: heating the mixed system of the barium titanium silicate and a fluxing agent LiF and H3BO3 or B2O3, making the mixed system at the constant temperature and cooling to obtain a mixed solution; then putting a seed crystal into the mixed solution for cooling to prepare the crystal with the big dimensions of 1-100mm*1-100mm*1-100mm. The crystal prepared by the method belongs to a tetragonal system. The space group of the crystal is P4bm, the chemical formula of the crystal is Ba2TiSi2O8, the cell parameter of the crystal is shown as follows: a=b=8.518+ / -0.002c=5.211+ / -0.002Z=4, and the Moh's hardness of the crystal is 4-5. The method has high preparation speed and low cost and is simple to operate; and the obtained crystal has the advantages of big dimensions, good mechanical behavior, stable physical and chemical properties and the like, is free of deliquescence and is easy to process and store.

Description

technical field [0001] The invention relates to a method for preparing barium titanium silicate crystals, in particular to a method for growing molten salt seed crystals of barium titanium silicate crystals. Background technique [0002] After decades of hard work by scientists from various countries, many crystals have been discovered, and some crystals have been used in practice, such as: KTP, low-temperature phase BBO, LBO, etc. crystals. Based on the above reasons, scientists from all over the world are still paying close attention to the exploration and research of various new crystals, not only focusing on the optical and mechanical properties of crystals, but also paying more and more attention to the preparation characteristics of crystals. It is hoped that new crystal materials can be easily prepared, so that they can be obtained Inexpensive large size high quality crystals. [0003] Scientist J.T.Alfors et al first reported barium titanium silicon oxide Ba in 196...

Claims

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Application Information

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IPC IPC(8): C30B29/34C30B9/12
Inventor 潘世烈赵文武
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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