CN102936041A - Synthesizing method of LuVO4 nano-crystals with different morphologies and dimensions - Google Patents
Synthesizing method of LuVO4 nano-crystals with different morphologies and dimensions Download PDFInfo
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- CN102936041A CN102936041A CN2012104028435A CN201210402843A CN102936041A CN 102936041 A CN102936041 A CN 102936041A CN 2012104028435 A CN2012104028435 A CN 2012104028435A CN 201210402843 A CN201210402843 A CN 201210402843A CN 102936041 A CN102936041 A CN 102936041A
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Abstract
The invention relates to a synthesizing method of LuVO4 nano-crystals with different morphologies and dimensions, and relates to a nano-crystal synthesizing method. The method comprises the process that: Na2tar is dissolved in deionized water; a Lu(NO3)3 solution is added; a solution containing Na3VO4.12H2O is added after half an hour of stirring; a pH value is regulated by using NaOH; the mixture is then stirred for 15 minutes, and is transferred to a reaction vessel; the reaction vessel is sealed, and the temperature is maintained at a high value; the material is naturally cooled to room temperature; a supernatant is discarded, and a precipitate is respectively washed with water and ethanol; centrifugation separation is carried out; and the obtained material is subjected to constant-temperature drying under a low temperature, such that the nano-crystals are obtained. The resulting nano-crystal products have unified uniform rhombic leaf shapes. Under room temperature, the obtained nano-crystals respectively emit bright red, yellow-green, orange-red, and green lights. The nano-crystals are valuable nano-grade luminescent materials.
Description
Technical field
The present invention relates to a kind of nanocrystalline synthetic method, particularly relate to a kind of have different-shape and size LuVO
4Nanocrystalline synthetic method.
Background technology
Rare earth luminescent material once played a part milestone in the development of luminescence and luminescent material.The outer electronic structure of rare earth element is basic identical, and internal layer 4f track unpaired electron is many, and magnetic moment of atom is high, and electronic level is abundant, than 3 orders of magnitude of the number l of manying – of every other element transition of electronic energy in the periodictable.Because its unique 4f electron structure, rare earth compound all has a wide range of applications in fields such as optical material, magneticsubstance, electronic material, electronic ceramics, engineering ceramics, catalytic material, energy-accumulating material and biological medicines.The research of rare earth luminescent material also becomes emphasis and the forward position of luminescent material research, and competition both domestic and external is very fierce.China is rare earth resources big country, and the rare earth resources industrial reserves accounts for the world and verified 80% of resource.Yet in the past few decades, China is in the status of cheap export State for a long time.Therefore, for the chemist of China, take full advantage of and develop rare earth resources and more seem particularly important.
Summary of the invention
The object of the present invention is to provide a kind of have different-shape and size LuVO
4Nanocrystalline synthetic method, pH value, the adding Na of present method by changing initial solution
2The amount of tar and the water-heat process in reaction times synthesize the LuVO with different-shape and size
4Nanocrystalline.Under the room temperature under ultraviolet ray and the electron-beam excitation of low pressure nanocrystalline shiny red, yellow-green colour, the orange red and green emitting of presenting respectively, be a kind of valuable nano luminescent material.
The objective of the invention is to be achieved through the following technical solutions:
A kind of have different-shape and a size LuVO
4Nanocrystalline synthetic method, described method comprises following process:
With Na
2Tar is dissolved in the deionized water, adds to contain Lu (NO
3)
3Solution, stir to add after half hour and contain Na
3VO
412H
2The solution of O is used the NaOH adjust pH, then stirs after 15 minutes to change in the reactor, and sealing, constant temperature under the high temperature afterwards, naturally cools to room temperature, abandoning supernatant, precipitation water and ethanol wash respectively, centrifugation, constant temperature drying gets final product under the low temperature.
Described a kind of have different-shape and size LuVO
4Nanocrystalline synthetic method, the nanocrystalline product of gained is unified, uniform rhombus shaped-like leaf.
Described a kind of have different-shape and size LuVO
4Nanocrystalline synthetic method, nanocrystalline shiny red, yellow-green colour, the orange red and green emitting of at room temperature presenting respectively of gained.
Description of drawings
Fig. 1 is LuVO
4: Ln
3+(Ln
3+=Eu
3+, Dy
3+, Sm
3+, Er
3+) nanocrystalline A-D figure photoluminescence spectrogram relatively.
Fig. 1 is the analysis synoptic diagram of product state, the unintelligible understanding that does not affect technical solution of the present invention of figure Chinese word or image.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
The invention provides a kind of pH value, adding Na by changing reaction parameter such as initial solution
2The amount of tar and the water-heat process in reaction times synthesize the LuVO with different-shape and size
4Nanocrystalline.LuVO to gained
4: Ln
3+(Ln
3+=Eu
3+, Dy
3+, Sm
3+, Er
3+) luminosity be illustrated.The present invention adopts Na
2Tar is organic additive, successfully synthesizes through test of many times to have the lobate LuVO of nanometer unified, uniform rhombus
4Nanocrystalline.Unified, uniform LuVO
4The controlledly synthesis that nanometer is lobate and the LuVO that mixes other rare earth ion
4: Ln
3+(Ln
3+=Eu
3+, Dy
3+, Sm
3+, Er
3+) luminosity.
Specific operation process is with Na
2Tar is dissolved in the deionized water, adds to contain Lu (NO
3)
3Solution, stir to add after half hour and contain Na
3VO
412H
2The solution of O is used the NaOH adjust pH, then stirs to change over to after 15 minutes in the reactor (about 50 mL), and sealing, constant temperature is some hours under the high temperature.Afterwards, naturally cool to room temperature, abandoning supernatant, precipitation water and ethanol wash respectively centrifugation, constant temperature drying under the low temperature.The product of gained characterizes with X-ray diffraction, infrared spectra, scanning electron microscope image, images of transmissive electron microscope, photoelectron spectrum, photoluminescence spectrogram and cathodeluminescence curve, and the result has shown that product is comprised of unification, uniform the nanocrystalline of rhombus shaped-like leaf.In addition, the series of parallel test card understands pH value, the adding Na that answers parameter such as initial solution
2The amount of tar and reaction times pattern and the size for product has important impact.
The LuVO of gained
4: Ln
3+(Ln
3+=Eu
3+, Dy
3+, Sm
3+, Er
3+) nanocrystalline shiny red, yellow-green colour, the orange red and green emitting of at room temperature presenting respectively.
Embodiment:
With Lu (NO
3)
3(0.5-2 mmol), Na
2Tar (0-3 mmol), H
2The mixed solution of O (20 –, 30 mL) is inserted in the reactor (50 mL) and is stirred half an hour, then adds Na
3VO
412H
2O (1-2 mmol) stirred 15 minutes, sealed reactor, and 180 ℃ of constant temperature of hydro-thermal naturally cooled to room temperature after 24-48 hours, precipitation water and the washing with alcohol of gained, 60-80 ℃ of lower oven dry obtains product.
Claims (3)
1. one kind has different-shape and size LuVO
4Nanocrystalline synthetic method is characterized in that, described method comprises following process:
With Na
2Tar is dissolved in the deionized water, adds to contain Lu (NO
3)
3Solution, stir to add after half hour and contain Na
3VO
412H
2The solution of O is used the NaOH adjust pH, then stirs after 15 minutes to change in the reactor, and sealing, constant temperature under the high temperature afterwards, naturally cools to room temperature, abandoning supernatant, precipitation water and ethanol wash respectively, centrifugation, constant temperature drying gets final product under the low temperature.
2. a kind of have different-shape and size LuVO according to claim 1
4Nanocrystalline synthetic method is characterized in that, the nanocrystalline product of gained is unified, uniform rhombus shaped-like leaf.
3. a kind of have different-shape and size LuVO according to claim 1
4Nanocrystalline synthetic method is characterized in that, nanocrystalline shiny red, yellow-green colour, the orange red and green emitting of at room temperature presenting respectively of gained.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110565070A (en) * | 2019-10-14 | 2019-12-13 | 安徽工业大学 | Terbium vanadate nanowire electrode material and preparation method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101774641A (en) * | 2010-01-06 | 2010-07-14 | 哈尔滨工程大学 | Method for preparing yttrium vanadate crystals |
CN102241983A (en) * | 2011-06-22 | 2011-11-16 | 四川大学 | Preparation method of vanadium boric acid gadolinium thulium blue luminescent material with modification of glucose |
-
2012
- 2012-10-22 CN CN2012104028435A patent/CN102936041A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101774641A (en) * | 2010-01-06 | 2010-07-14 | 哈尔滨工程大学 | Method for preparing yttrium vanadate crystals |
CN102241983A (en) * | 2011-06-22 | 2011-11-16 | 四川大学 | Preparation method of vanadium boric acid gadolinium thulium blue luminescent material with modification of glucose |
Non-Patent Citations (1)
Title |
---|
ZHENHE XU等: "Self-assembled growth of LuVO4 nanoleaves: hydrothermal synthesis, morphology evolution, and luminescence properties", 《RSC ADVANCES》, 18 September 2012 (2012-09-18), pages 11067 - 11077 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110565070A (en) * | 2019-10-14 | 2019-12-13 | 安徽工业大学 | Terbium vanadate nanowire electrode material and preparation method thereof |
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Application publication date: 20130220 |