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Method for preparing samarium-doped strontium borate under high temperature and high pressure by using precursor

A high temperature and high pressure, boron-doped technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of difficult control of experimental conditions, low luminous efficiency, low purity, etc., and achieve the effect of easy control of sintering temperature

Active Publication Date: 2018-01-12
INST OF GEOCHEM CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is to provide a method for preparing samarium-doped strontium borate using a precursor under high temperature and high pressure, so as to solve the problem that the prior art method for preparing samarium-doped strontium borate mainly uses strontium carbonate, boric acid and trioxide Disamarium is used as raw material, using high-temperature solid-state reaction method, hydrothermal synthesis method, etc., but its synthesis process is complex, experimental conditions are difficult to control, and the synthesized samarium-doped strontium borate has low purity, poor crystallization, small particle size, samarium Technical problems such as small doping amount and low luminous efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Using analytically pure boron trioxide and strontium carbonate as raw materials, mixing them in a stoichiometric molar ratio of 1.1:1, sintering in a tube furnace at a high temperature of 900°C for 12 hours to prepare pure matrix phase 147 strontium borate SrB 4 O 7 ; Using analytically pure boron trioxide and samarium oxalate decahydrate as raw materials, after mixing in a stoichiometric molar ratio of 1.3:1, sintering in a tube furnace at 800 ℃ for 12 hours to prepare pure precursor phase 136 samarium borate SmB 3 O 6 ; The parent phase 147 strontium borate SrB prepared in step 2 and step 3 4 O 7 , Precursor phase 136 SmB borate 3 O 6 And B 2 O 3 , Weigh according to the stoichiometric molar ratio (1-x):x:x / 2, where x is the doped amount of samarium, with a value of 0.1, mix the weighed objects uniformly, and press the mixture powder with a tablet press Into a Φ5×3mm cylindrical sample. Use a tablet press to analyze pure zirconia ZrO 2 The powder is pressed into a pair ...

Embodiment 2

[0068] Using analytically pure boron trioxide and strontium carbonate as raw materials, mixing them in a stoichiometric molar ratio of 1.1:1, sintering in a tube furnace at a high temperature of 900°C for 12 hours to prepare pure matrix phase 147 strontium borate SrB 4 O 7 ; Using analytically pure boron trioxide and samarium oxalate decahydrate as raw materials, after mixing in a stoichiometric molar ratio of 1.3:1, sintering in a tube furnace at 800 ℃ for 12 hours to prepare pure precursor phase 136 samarium borate SmB 3 O 6 ; The parent phase 147 strontium borate SrB prepared in step 2 and step 3 4 O 7 , Precursor phase 136 SmB borate 3 O 6 And B 2 O 3 , Weigh according to the stoichiometric molar ratio (1-x):x:x / 2, where x is the doped amount of samarium, with a value of 0.1, mix the weighed objects uniformly, and press the mixture powder with a tablet press Into a Φ5×3mm cylindrical sample. Use a tablet press to analyze pure zirconia ZrO 2 The powder is pressed into a pair ...

Embodiment 3

[0075] Using analytically pure boron trioxide and strontium carbonate as raw materials, mixing them in a stoichiometric molar ratio of 1.1:1, sintering in a tube furnace at a high temperature of 900°C for 12 hours to prepare pure matrix phase 147 strontium borate SrB 4 O 7 ; Using analytically pure boron trioxide and samarium oxalate decahydrate as raw materials, after mixing in a stoichiometric molar ratio of 1.3:1, sintering in a tube furnace at 800 ℃ for 12 hours to prepare pure precursor phase 136 samarium borate SmB 3 O 6 ; The parent phase 147 strontium borate SrB prepared in step 2 and step 3 4 O 7 , Precursor phase 136 SmB borate 3 O 6 And B 2 O 3 , Weigh according to the stoichiometric molar ratio (1-x):x:x / 2, where x is the doped amount of samarium, with a value of 0.1, mix the weighed objects uniformly, and press the mixture powder with a tablet press Into a Φ5×3mm cylindrical sample. Use a tablet press to analyze pure zirconia ZrO 2 The powder is pressed into a pair ...

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Abstract

The invention discloses a method for preparing samarium-doped strontium borate by taking analytically pure diboron trioxide, strontium carbonate and samarium oxalate decahydrate as raw materials and combining precursor preparation under normal pressure and high pressure and a high temperature and high pressure solid phase reaction. The method comprises the following steps: pressing mixture powderto be cylindrical by using a tablet press; respectively pressing zirconia powder and sodium oxalate powder into a pair of wafers by using the tablet press; staking and filling the prepared wafers intoa platinum tube to be sealed in a sandwich form, completing high-pressure assembling, and carrying out the high temperature and high pressure reaction by a large cubic press, thereby obtaining the samarium-doped strontium borate sample. The technical problems in the prior art that synthesis conditions are difficultly controlled in the process of taking strontium carbonate, boric acid and samariumsesquioxide as raw materials and synthesizing the samarium-doped strontium borate by using a high-temperature solid-phase reaction method, a hydrothermal synthesis method and the like and the synthesized samarium-doped strontium borate is low in purity, poor in crystallinity, low in granularity, small in samarium doping amount and low in luminous efficiency and the like are solved.

Description

Technical field: [0001] The invention relates to the field of pressure calibration material synthesis, in particular to a preparation of samarium-doped strontium borate (Sr 1-x Sm x B 4 O 7 )Methods. Background technique: [0002] Among the non-linear optical crystals that have been discovered, borate has a wide range of application prospects and scientific research value. The boron-oxygen bond facilitates the transmission of ultraviolet light, and the group configuration of boron-oxygen compounds is rich and diverse and has strong chemical stability. The borate fluorescent material doped with rare earth ions has the characteristics of good chemical stability, good thermal stability, wide bandwidth and excellent organization. Among many borates, strontium borate type 147 (SrB 4 O 7 ) It has the characteristics of high mechanical strength, high microhardness, and excellent nonlinear optical properties, such as large frequency multiplication factor, short ultraviolet cut-off absorp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/63
Inventor 李和平梁文王燕李泽明
Owner INST OF GEOCHEM CHINESE ACADEMY OF SCI
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