CN105778912A - Preparation method of triangular prism-shaped rare earth-activated yttrium oxide nano-luminescence material - Google Patents

Preparation method of triangular prism-shaped rare earth-activated yttrium oxide nano-luminescence material Download PDF

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Publication number
CN105778912A
CN105778912A CN201610352926.6A CN201610352926A CN105778912A CN 105778912 A CN105778912 A CN 105778912A CN 201610352926 A CN201610352926 A CN 201610352926A CN 105778912 A CN105778912 A CN 105778912A
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oxide nano
preparation
rare earth
deionized water
rare
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王金淑
赵冰心
贾新建
董丽然
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Beijing University of Technology
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Beijing University of Technology
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention discloses a preparation method of a triangular prism-shaped rare earth-activated yttrium oxide nano-luminescence material, and belongs to preparation of luminescent nanomaterials.The preparation method comprises the following steps that yttrium nitrate (Y(NO3)3) serving as a yttrium source and rare earth (such as europium, erbium and samarium) nitrate are added into deionized water and triethanolamine (TEOA), full stirring is performed, therefore, the molar concentration of Y<3+> is 0.01 M-1 M, and the molar concentration of rare earth ions accounts for 1%-8% of that of the yttrium ions.Heat preservation is performed for 24-80 h at the temperature of 130 DEG C-200 DEG C through a solvothermal method, and the volume ratio of solvent (TEOA) to the deionized water is (0.1-3):1.

Description

A kind of preparation method of triangle column rare-earth activated yittrium oxide nano luminescent material
Technical field
The preparation method of a kind of rare-earth activated yttrium oxide luminescent material of triangle column, belongs to the preparation of Illuminant nanometer material.
Background technology
Yittrium oxide (Y2O3) have many good qualities: high chemical stability and heat stability, high band gap (energy gap 5.8eV).And Y2O3As the matrix material of excellent luminescent material, known oxide has minimum phonon energy (380cm-1)。
Summary of the invention
Inventive process avoids conventional rare luminescent powder common higher temperature sintering link, and a kind of triangle column provided is dilute The preparation method of soil activated yttria luminescent material.
The preparation method of a kind of triangle column rare-earth activated yittrium oxide nano luminescent material that the present invention provides, its feature exists In, comprise the steps of Yttrium trinitrate (Y (NO3)3) add deionized water and triethanolamine as yttrium source with rare earth nitrate (TEOA) in the mixed solvent formed, and it is sufficiently stirred for so that Y3+Molar concentration be 0.01M-1M, rare earth ion molar concentration 1%-8% for ruthenium ion;Solvent-thermal method is utilized to be incubated 24-80h process through 130-200 DEG C.Solvent TEOA and deionized water Volume ratio be (0.1-3): 1.
Described rare earth is selected from europium, erbium, samarium etc..
The preparation method of the present invention is further preferred, following steps:
It is (0.1-0.6) that Yttrium trinitrate adds triethanolamine (TEOA) with deionized water volume ratio: in the solvent of 1 so that Y3+ Substance withdrawl syndrome be 0.01M-0.5M;Rare earth ion molar concentration is the 1%-5% of ruthenium ion.
The triangle column rare-earth activated yittrium oxide nano material of gained of the present invention, is to be triangle or four limits by multiple cross sections Parallel the combining of column structure of shape and the triangle column that formed.
Compared with prior art, the invention has the beneficial effects as follows:
Compared with existing common higher temperature combustion method (more than 1000 DEG C), it is rear-earth-doped that the present invention uses prepared by solvent-thermal method Y2O3Only need to be through low temperature (less than 200 DEG C) solvent thermal program, and 500 DEG C of heat treatments.Simplified flowsheet, the saving energy.
Accompanying drawing explanation
Fig. 1: Er ions yittrium oxide (embodiment 1) scanning electron microscope (SEM) photograph.
Fig. 2: europium doped yttrium oxide (embodiment 2) EDS energy penetrates scattered spectrogram.
Absorption (250nm) spectrum of Fig. 3: europium doped yttrium oxide and transmitting (610nm) spectrogram.
The emission spectrum figure (excitation wavelength is 980nm) of Fig. 4: Er ions yittrium oxide.
Detailed description of the invention
Combine accompanying drawing below by embodiment and further describe the present invention, its object is to be more fully understood that the present invention's is interior Hold rather than limitation of the present invention.
Embodiment 1:
Take 2.238g TEOA, 43ml deionized water, the Erbium trinitrate of 1.09mM and the Yttrium trinitrate of 0.073M, by this mixed liquor Put in autoclave.It is incubated 40 hours at 140 DEG C, takes out yittrium oxide nano powder after cooling, take out with deionized water rinsing with ethanol Filter, dries.500 degree of heat treatments 2 hours, are cooled to room temperature, prepared by europium doped yttrium oxide nano powder.
Embodiment 2:
Take europium nitrate and the Yttrium trinitrate of 0.08M of 50g TEOA, 600ml deionized water, 0.86mM, this mixed liquor is put into In autoclave.Through two step isothermal holding, be incubated 36 hours at 150 DEG C, after cooling, take out yittrium oxide nano powder, with ethanol with go Ionized water rinses sucking filtration, dries.500 degree of heat treatments 2 hours, are cooled to room temperature, prepared by europium doped yttrium oxide nano powder.
Embodiment 3:
Take europium nitrate and the Yttrium trinitrate of 0.05M of 4g TEOA, 43ml deionized water, 1.1mM, this mixed liquor is put into height In pressure still.It is incubated 50 hours at 140 DEG C, after cooling, takes out yittrium oxide nano powder, with ethanol and deionized water rinsing sucking filtration, dry Dry.500 degree of heat treatments 2 hours, are cooled to room temperature, prepared by europium doped yttrium oxide nano powder.
Embodiment 4:
Take samaric nitrate and the Yttrium trinitrate of 0.05M of 10g TEOA, 200ml deionized water, 0.8mM, this mixed liquor is put into In autoclave.It is incubated 38 hours at 150 DEG C, after cooling, takes out yittrium oxide parcel TiO2Nano powder, rushes with deionized water with ethanol Wash sucking filtration, dry.500 degree of heat treatments 2 hours, are cooled to room temperature, prepared by europium doped yttrium oxide nano powder.
Embodiment 5:
Take europium nitrate and the Yttrium trinitrate of 0.03M of 2g TEOA, 55ml deionized water, 0.5mM, this mixed liquor is put into height In pressure still.It is incubated 60 hours at 130 DEG C, after cooling, takes out yittrium oxide parcel TiO2Nano powder, with ethanol and deionized water rinsing Sucking filtration, dries.500 degree of heat treatments 2 hours, are cooled to room temperature, prepared by europium doped yttrium oxide nano powder.
Table 1 experiment parameter list

Claims (4)

1. the preparation method of a triangle column rare-earth activated yittrium oxide nano luminescent material, it is characterised in that comprise following step Rapid: by Yttrium trinitrate (Y (NO3)3) add, with rare earth nitrate, the mixing that deionized water forms with triethanolamine (TEOA) as yttrium source In solvent, and it is sufficiently stirred for so that Y3+Molar concentration be 0.01M-1M, rare earth ion molar concentration is the 1%-of ruthenium ion 8%;Utilizing solvent-thermal method to be incubated 24-80h process through 130-200 DEG C, solvent TEOA is (0.1-with the volume ratio of deionized water 3): 1.
2. according to the preparation method of a kind of triangle column rare-earth activated yittrium oxide nano luminescent material described in claim 1, its Being characterised by, it is (0.1-0.6) that Yttrium trinitrate adds triethanolamine (TEOA) with deionized water volume ratio: in the solvent of 1 so that Y3+ Substance withdrawl syndrome be 0.01M-0.5M;Rare earth ion molar concentration is the 1%-5% of ruthenium ion.
The triangle column rare-earth activated yittrium oxide nano luminescent material prepared the most in accordance with the method for claim 1.
The triangle column rare-earth activated yittrium oxide nano luminescent material prepared the most in accordance with the method for claim 1, its It is characterised by, is to be combined, by the column structure that multiple cross sections are triangle or tetragon is parallel, the triangular prism formed Shape.
CN201610352926.6A 2016-05-25 2016-05-25 Preparation method of triangular prism-shaped rare earth-activated yttrium oxide nano-luminescence material Pending CN105778912A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102226084A (en) * 2011-04-28 2011-10-26 北京科技大学 Synthesis method of flower-like Y2O3:Eu<3+> microspheres
CN104319106A (en) * 2014-09-26 2015-01-28 北京工业大学 Preparation method of yttrium oxide enveloped titanium dioxide nano-powder for dye-sensitized solar cells

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102226084A (en) * 2011-04-28 2011-10-26 北京科技大学 Synthesis method of flower-like Y2O3:Eu<3+> microspheres
CN104319106A (en) * 2014-09-26 2015-01-28 北京工业大学 Preparation method of yttrium oxide enveloped titanium dioxide nano-powder for dye-sensitized solar cells

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
BINGXIN ZHAO等: "Rare Earth - Activated Y2O3 Phosphors with Novel Morphology for Dye-Sensitized Solar Cells", 《CHEMISTRYSELECT》 *
QI ZHAO 等: "Dendritic Y4O(OH)9NO3:Eu3+/Y2O3:Eu3+ hierarchical structures: controlled synthesis, growth mechanism,and luminescence properties", 《CRYSTENGCOMM》 *

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Application publication date: 20160720