Low temperature process of preparing RE borate crystal with oxide as precursor

A technology of oxide and borate, which is applied in the field of micro/nano material preparation technology and hydrothermal synthesis, can solve the problems of high production cost, waste of organic matter, unfavorable environmental protection and rational application of resources, etc., and achieves simple operation, simple process, The effect of facilitating industrial transformation

Inactive Publication Date: 2007-06-06
TONGJI UNIV
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  • Application Information

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Problems solved by technology

[0003] Though above-mentioned these methods have provided the approach of some synthetic rare-earth borates, there are still deficiencies, as solid-phase reaction will pass through high temperature, excessive boron and complex procedure just can obtain nanoscale borate; And sol-gel can cause A large amount of organic matter is wasted, the production cost is high, and a large amount of waste gas is also generated, which is not conducive to environmental protection and rational use of resources

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  • Low temperature process of preparing RE borate crystal with oxide as precursor
  • Low temperature process of preparing RE borate crystal with oxide as precursor
  • Low temperature process of preparing RE borate crystal with oxide as precursor

Examples

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Embodiment 1

[0035] Embodiment 1: prepare lanthanum borate

[0036] Add 2.0×10 -4 mol of La 2 o 3 , 2.0-2.2×10 -4 mol of B 2 o 3 , 7ml of deionized water, and then close the reactor, transfer the two reactors to an ultrasonic generator, ultrasonically vibrate for 10 minutes, then transfer the reactors containing the mixed solution to a temperature-controlled furnace for roasting at 10°C / According to the heating rate, the reaction temperature in the furnace is controlled to be 200°C and 240°C respectively, and the constant temperature heating time is 24 hours. The reaction kettle is taken out and naturally cooled to room temperature. Washed three times with water and ethanol respectively to obtain the desired product.

[0037] LaBO in Figure 1 3 The curve of LaBO3 X-ray powder diffraction pattern. The obtained product is consistent with the standard spectrogram of the orthorhombic lanthanum borate, and there are different degrees of broadening, indicating that the product is a nano...

Embodiment 2

[0039] Embodiment 2: prepare the borate of Sm, Gd, Dy

[0040] Add 2.0×10 -4 mol of Sm 2 o 3 、Gd 2 o 3 、Dy 2 o 3 and 2.0-2.2×10 -4 mol B 2 o 3 -3H 2 O is the raw material, 6-7mL of deionized water is used to seal the reactor, mix evenly, and then transfer the three reactors containing the mixed solution to a temperature-controlled furnace for roasting, control the reaction temperature in the furnace to 200°C, and heat at a constant temperature The time is 24 hours, take out the reaction kettle, cool naturally to room temperature, take out the precipitate obtained in the reaction kettle, and wash with deionized water and absolute ethanol alternately for 4-5 times respectively to obtain the desired product.

[0041] SmBO given in Figure 1 3 The curve is the resulting product SmBO 3 The X-ray diffraction pattern was found to be consistent with the standard pattern through retrieval. There is obvious broadening phenomenon in the spectrogram, indicating that the produc...

Embodiment 3

[0044] Embodiment 3: prepare the orthoborate of Er and Y

[0045] Add 2.0×10 -4 mol of Er 2 o 3 , Y 2 o 3 , 2.0-2.2×10 -4 mol B 2 o 3 As raw material, deionized water 7-8mL, additive o-phenanthroline 0.02 g, seal the reactor, mix evenly, then transfer the two reactors containing the mixed solution to a temperature-controlled furnace for roasting, and control the reaction in the furnace The temperature is 280°C, and the reaction time is 24 hours. Take out the reactor, let it cool down to room temperature naturally, take out the precipitates in the reactor, wash with deionized water and absolute ethanol alternately for 5-6 times respectively, and obtain the desired product.

[0046] Figure 2 shows the ErBO 3 The curve for ErBO 3 The X-ray diffraction pattern of X-ray diffraction pattern, found that product is consistent with erbium borate standard pattern pattern through retrieval, and pattern pattern appears obvious broadening phenomenon, and ErBO given in Fig. 7 (A) ...

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Abstract

The present invention belongs to the field of micron/nanometer material preparing technology and hydrothermal synthesis technology, and is especially low temperature process of preparing RE borate crystal with oxide as precursor. In the hydrothermal system, insoluble RE oxide and hydrated boron trioxide or boron trioxide as the boron source and precursor are reacted at 190-280 deg.c for 12-48 hr, and through further washing, the required RE borate crystal is obtained. The present invention provides one inorganic synthesis way, and the production process has no any pollution. The present invention has simple technological process, easy-to-constitute reaction system, high product purity and other advantages, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of micro / nano material preparation technology and hydrothermal synthesis, and in particular relates to a method for preparing rare earth borate crystals with oxides as precursors at low temperature. Background technique [0002] Rare earth elements are favored in phosphors because of their unique 4f-layer electronic structure and the excellent performance of excitation light in line spectrum or narrow band spectrum. Rare earth phosphors will replace zinc, strontium, and sulfide phosphors for higher brightness and clarity. Rare earth borate series phosphors are a new type of rare earth phosphors being researched and developed in the late 1990s in order to adapt to the development of large-screen high-definition color projection TVs and computer terminal display technologies. At the same time, rare earth borates are also widely used in the preparation of various optical materials such as luminescent glass, light-emitti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/22C30B7/10C09K11/78
Inventor 吴庆生马杰
Owner TONGJI UNIV
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