Method for preparing Nano/micro crystal of rare earth vanadate from oxide as precursor body under low temperature

A rare earth vanadate and oxide technology, applied in the field of materials, can solve the problems of unfavorable environmental protection, rational application of resources, high equipment performance requirements, large energy consumption, etc., and achieves convenient industrial transformation, convenient operation and simple equipment. Effect

Inactive Publication Date: 2006-12-06
TONGJI UNIV
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Problems solved by technology

[0003] Although the above-mentioned methods provide some ways to synthesize rare earth vanadates, there are still deficiencies, such as high-temperature ball milling, which requires high equipment performance, high energy consumption, and high noise
The hydrothermal method uses soluble salts as reaction precursors, the production cost is higher than that of oxides, and it also produces a large amount of waste liquid, which is not conducive to environmental protection and rational application of resources

Method used

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  • Method for preparing Nano/micro crystal of rare earth vanadate from oxide as precursor body under low temperature
  • Method for preparing Nano/micro crystal of rare earth vanadate from oxide as precursor body under low temperature
  • Method for preparing Nano/micro crystal of rare earth vanadate from oxide as precursor body under low temperature

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Experimental program
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Effect test

Embodiment 1

[0036] Embodiment 1: prepare yttrium vanadate

[0037] Add 1.0×10 -4 mol of Y 2 o 3 , 1.2×10 -4 mol of V 2 o 5 , 7ml of deionized water, and then add additives, the addition of additives is (a) 0.05mL of 1M nitric acid and 0.5×10 -4 mol EDTA, (b) without any additives, (c) 0.05mL of 1M hydrochloric acid, (d) 0.05mL of 1M hydrochloric acid, 0.5×10 -4 mol EDTA, (e) add 1M sulfuric acid 0.05mL and 0.25×10 -4 mol of EDTA, sealed reactor; transferred the reactor to an ultrasonic generator, ultrasonicated for 10 minutes, then transferred the reactor to a constant temperature drying oven, and controlled the reaction temperature to 130°C and 170°C at a heating rate of 10°C / min. ℃, 170℃, 170℃, 200℃, and heated at constant temperature for 48 hours, 24 hours, 24 hours, 24 hours, 24 hours respectively.

[0038] Step 5: After the reaction is completed, take out the reactor and let it cool down to room temperature naturally.

[0039] Step 6: Take out the precipitate obtained from t...

Embodiment 2

[0041] Embodiment 2: Preparation of monoclinic lanthanum vanadate

[0042] Take 1.0×10 respectively -4 mol of La 2 o 3 and V 2 o 5 As raw material, 6 mL of deionized water, 0.05 mL of 1M hydrochloric acid and 0.05×10 -4 mol KCN, according to the steps described in Example 1, the reaction temperature was 170° C., and the reaction time was 24 hours to obtain the desired product. figure 2 The X-ray diffraction pattern of the obtained product given in, finds by retrieval, the product is the LaVO of pure monoclinic system 4 . There is obvious broadening phenomenon in the spectrogram, indicating that the product is a nanoscale particle. The TEM of the product further confirms that it is a rod-shaped single crystal at the nanoscale.

Embodiment 3

[0043] Embodiment 3: Preparation of tetragonal lanthanum vanadate

[0044] Take 1.0×10 respectively -4 mol of La 2 o 3 and V 2 o 5 As raw material, deionized water 6mL, additive EDTA0.5×10 -4 mol and 0.05mL1M nitric acid, according to the steps described in Example 1, the reaction temperature is 170 ° C, and the reaction times is 24 hours to obtain the desired product. From image 3 The X-ray diffraction spectrum of the obtained product given in , found by retrieval, the product is the LaVO of tetragonal crystal system 4 . There is obvious broadening phenomenon in the spectrogram, indicating that the product is a nanoscale particle.

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Abstract

This invention relates to a method for preparing rare earth vanadate nano- and micro-crystals from oxide precursors at a low temperature. The method uses insoluble rare earth oxide and V2O5 as the precursors to directly synthesize rare earth vanadate nano- and micro-crystals by hydrothermal reaction at 120-240 deg.C for a certain time. Besides, the morphology and crystal structure and the product can be controlled by changing the reaction temperature and time as well as adding the additive.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a method for preparing rare earth vanadate nano / micron crystals with oxides as precursors at low temperatures. Background technique [0002] Rare earth vanadyl compounds are a class of functional materials with broad application prospects. It has attracted much attention because of its many special physical and chemical properties. For example, yttrium vanadate crystal is not only a good birefringent crystal, but also a good matrix material, which is widely used in luminescent materials, electromagnetic materials, photoelectric materials and piezoelectric materials. At present, the methods for synthesizing such materials mainly include solid-phase method and liquid-phase method: (1) solid-phase method usually uses vanadium pentoxide and rare earth oxide or carbonate as precursors, through high-temperature calcination (sintering ) method to obtain the corresponding...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C01G31/00
Inventor 吴庆生马杰
Owner TONGJI UNIV
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