CN100575451C - A kind of red nano-fluorescent powder and preparation method thereof - Google Patents
A kind of red nano-fluorescent powder and preparation method thereof Download PDFInfo
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- CN100575451C CN100575451C CN200810033027A CN200810033027A CN100575451C CN 100575451 C CN100575451 C CN 100575451C CN 200810033027 A CN200810033027 A CN 200810033027A CN 200810033027 A CN200810033027 A CN 200810033027A CN 100575451 C CN100575451 C CN 100575451C
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Abstract
The invention belongs to the luminescent material technical field, be specifically related to a kind of red light Nano phosphor powder and preparation method thereof.The present invention is from the angle of Molecular Structure Design, at first adopt the method for organic synthesis to obtain having the organic functional molecular part of amphipathic backbone, adopt the liquid phase reaction method that itself and rare-earth ion coordination are obtained amphipathic rare-earth title complex presoma then, again by method for pyrolysis obtain that pattern is controlled, chemistry and thermodynamic property is stable, ultraviolet and near ultraviolet excitated Gd
xY
2-xO
3: Eu
3+Red nano-fluorescent powder.The inventive method workable, favorable reproducibility, the products obtained therefrom steady quality, pattern is regular, and size of microcrystal is controlled in the 80nm scope.
Description
Technical field
The invention belongs to the luminescent material technical field, be specifically related to a kind of red light Nano phosphor powder and preparation method thereof.
Background technology
The performance of material and its dimensional structure have confidential relation, and the research of specific form structure helps the design and development of the novel material of excellent properties.Therefore, research and the synthetic novel structure of exploration to material microstructure caused the great interest of people.The microtexture of control rare earth oxide can be improved the performance of material, and along with the darker understanding to crystal nucleation and process of growth, people more and more pay attention to come synthetic material with superperformance by design and assembling to presoma.Amphipathic molecule is the molecule that contains hydrophilic polar head and hydrophobic fatty afterbody, has unique self-assembly performance, and its solution forms supramolecular ordered aggregate one micella of different shape by self-assembly under suitable composition and temperature condition.Amphipathic molecule has high molecular stickiness and the low molecular surfactivity of increasing concurrently, can be used as molecular surface active agent and uses, and its amphipathic nature has been kept stability of structure.When having a delicate balance between the hydrophobicity of amphipathic molecule and the wetting ability, slight end group not only can adjustment structure microcosmic self-assembly behavior, also can influence the behavior of soft material macroscopic condensed state by regulating its spontaneous physical gelization.
On the other hand; rare-earth luminescent material has purposes widely in many fields such as indicating meter, anti-counterfeiting marks. in recent years; along with spreading unchecked day by day of pseudo-technology for making of modern times; simple fluoroscopic image is false proof to be easy to by imitated; do not reached the purpose of protection product, the nano-luminescent material of controlled preparation then provides the senior false proof means of microcosmic level with size, pattern and the microstructure of its homogeneous.In addition, continuous development along with display technology, the appearance of especially various novel flat-plate indicating meters (as Field Emission Display, plasma display), in order to obtain higher display resolution, improve image resolution ratio, reduce the indicating meter operating voltage, not only require luminescent material to show stronger fluorescence property, and require fluorescent grain itself to have the pattern of regular homogeneous.Therefore, the nano-fluorescent grain with regular pattern of narrow size distribution becomes satisfactory important potential material.
Gd
xY
2-xO
3: Eu
3+Material is the most frequently used rare-earth activated red fluorescence powder, stability is high, and has good luminous efficiency, luminosity, characteristic such as purity of color and light decay, be widely used in cathode ray tube (CRT), color projection TV, fields such as high-color rendering luminescent lamp and trichromatic energy saving fluorescent lamp are used in illumination.A small amount of Gd
3+Adding can effectively play the effect that improves lattice, improves degree of crystallinity, thereby the fluorescence intensity of nano particle is effectively strengthened. and the yttrium price comparison is cheap, becomes certain proportioning to mix with gadolinium and can reduce the more expensive Gd of the required price of maximum fluorescence intensity
3+Consumption helps reducing cost.And relevant experiment shows to have nano-composite fluorescent material Gd
xY
2-xO
3: Eu
3+Have than single Y
2O
3: Eu
3+Or Gd
2O
3: Eu
3+The fluorescent emission that material is stronger. therefore, the Gd that pattern is controlled
xY
2-xO
3: Eu
3+Nano-luminescent material is satisfactory important potential material.
The exploitation of current novel fluorescence powder, preparation method thereof becomes numerous scientific and technological investigators' pursuing of goal.But have not yet to see by the controlled preparation Gd of the presoma that adopts amphipathic structure
xY
2-xO
3: Eu
3+The report of red fluorescence material.
Summary of the invention
The object of the present invention is to provide a kind of luminous efficiency height, long service life, stable chemical performance, ultraviolet and near ultraviolet excitated red nano-fluorescent powder and preparation method thereof.
The red fluorescence powder that the present invention proposes, its chemical formula is Gd
xY
2-xO
3: Eu
3+, wherein, x is 0.2,0.6,1.0,1.4 or 1.8, and this fluorescent material pattern is regular, arranges evenly, and median size is below 80nm.
The preparation method of the red nano-fluorescent powder that the present invention proposes, concrete steps are as follows:
(1) preparation of organic ligand:
With anhydrides organic molecule and long-chain alcohol is raw material, and under 110-115 ℃ of oil bath temperature backflow 15-16 hour, products therefrom normal hexane recrystallization obtained white powder, is to have amphipathic long-chain organic functional molecular, as part; Wherein: the proportioning of anhydrides organic molecule and long-chain alcohol amount of substance is 1: 1;
(2) preparation of presoma:
With rare earth oxide yttrium oxide Y
2O
3, gadolinium sesquioxide Gd
2O
3With europium sesquioxide Eu
2O
3Handle by concentrated nitric acid respectively, obtain corresponding nitric hydrate salt compound Y (NO
3)
36H
2O, Gd (NO
3)
36H
2O and Eu (NO
3)
36H
2O joins in the ethanolic soln of the amphipathic organic functions part of step (1) gained then successively, and the pH value of regulator solution is 7-8, stirs, treat that solution evenly after, solvent evaporated obtains thickness exsiccant amphipathic rare-earth organic precursor; Gd (NO
3)
36H
2O, Y (NO
3)
36H
2O and Eu (NO
3)
36H
2The mol ratio of O is 1: 9: 0.5--9: 1: 0.5;
(3) the amphipathic rare-earth organic precursor of step (2) gained is handled through high temperature pyrolysis, promptly got desired product;
Wherein, described sour bar class organic molecule is a MALEIC ANHYDRIDE, and described long-chain alcohol is a stearyl alcohol.
Among the present invention, the anhydrides organic molecule has MALEIC ANHYDRIDE or Tetra hydro Phthalic anhydride etc. described in the step (1).
Among the present invention, long-chain alcohol can use hexadecanol, stearyl alcohol, eicosanol or behenyl alcohol etc. described in the step (1), preferred stearyl alcohol.
Among the present invention, pH value conditioning agent is NaCO described in the step (2)
3Solution.
Among the present invention, churning time is 1.2-2 hour described in the step (2), and the temperature of solvent evaporated is 80-85 ℃.
Among the present invention, pyrolysis temperature is 900-1100 ℃ described in the step (3), and pyrolysis time is 2.5-3.5 hour.
Among the present invention, gained monoesters normal hexane recrystallization 2-3 time in the step (1), purpose is in order to remove impurity.
Among the present invention, the monoesters and the rare-earth ion coordination of step (2) optional step (1) gained anhydrides obtain the amphipathic rare-earth organic precursor.Mainly be divided into two parts: at first with rare earth oxide Y
2O
3, Gd
2O
3, Eu
2O
3, obtain corresponding nitric hydrate salt compound Y (NO by the concentrated nitric acid processing
3)
36H
2O, Gd (NO
3)
36H
2O and Eu (NO
3)
36H
2O; Ethanolic soln with these three kinds of rare earth nitrate compounds joins in the ethanolic soln of the amphipathic organic functions part of step (1) gained successively then, and coordination obtains the amphipathic rare-earth organic precursor.
Step (2) relates to selects for use amphipathic anhydrides monoester rare earth organic functional molecular as presoma, is because the amphipathic nature of this presoma has regulating and controlling effect preferably to the microtexture and the luminescent properties of gained phosphor material powder.
Among the present invention, the pH value has bigger influence to speed of response and productive rate, adds NaCO
3The solution unnecessary acid that not only can neutralize, and the weak base conditions favouring carries out in reaction.
Among the present invention, the alcoholic acid boiling point is 78.5 ℃, so at 80 ℃ of left and right sides evaporating solvents.
Among the present invention, the high temperature pyrolysis that step (3) relates to, purpose is for organic composition in the system of removing and other impurity, obtains having of one's own the luminescent material of microparticle system.
Gd by the inventive method production
xY
2-xO
3: Eu
3+The phosphor material powder photon absorbing intensity is big and transformation efficiency is high, and microscopic appearance is regular, size distribution evenly and particle diameter be effectively controlled within 80nm; In addition, its favorable dispersity.At last, the inventive method workable, favorable reproducibility, and products obtained therefrom steady quality.
Description of drawings
Fig. 1 is the embodiment of the invention 3 gained Gd
xY
2-xO
3: Eu
3+The X ray diffracting spectrum of nano-phosphor.
Fig. 2 is the embodiment of the invention 3 gained Gd
xY
2-xO
3: Eu
3+The scanning electron microscope diagram of nano-phosphor.
Fig. 3 is the embodiment of the invention 3 gained Gd
xY
2-xO
3: Eu
3+The transmission electron microscope figure of nano-phosphor.
Fig. 4 is the embodiment of the invention 3 gained Gd
xY
2-xO
3: Eu
3+The uv drs spectrogram of nano-phosphor.
Fig. 5 is the embodiment of the invention 3 gained Gd
xY
2-xO
3: Eu
3+The nano-phosphor excitation spectrum.
Fig. 6 is the embodiment of the invention 3 gained Gd
xY
2-xO
3: Eu
3+The nano-phosphor emmission spectrum.
Embodiment
The present invention below will be described in more detail by reference example, but protection scope of the present invention is not limited to these embodiment.Raw material in the embodiment of the invention is analytical pure available from Shanghai traditional Chinese medicines group.
Embodiment 1
Take by weighing the stearyl alcohol (about 5.41g) of 20mmol (about 1.96g) MALEIC ANHYDRIDE and amount of substance such as grade respectively, place round-bottomed flask, regulate oil bath temperature between 110-115 ℃, refluxed 16 hours, product normal hexane recrystallization 2-3 time, obtain white powder, be MALEIC ANHYDRIDE stearyl alcohol monoesters (MAO).
Get excessive slightly MAO (3.1mmol) and join in 95% ethanolic soln, use NaCO after waiting to dissolve
3Solution is regulated the pH value to 7-8, then to wherein slowly adding Gd (NO
3)
36H
2O (0.1mmol), Y (NO
3)
36H
2O (0.9mmol) and Eu (NO
3)
36H
2O (0.05mmol) (nGd: Y: Eu=0.1: 0.9: 0.05) ethanolic soln places on the constant temperature blender with magnetic force and stirs, and treats to use NaCO after solution evenly
3Solution is transferred to 7-8 with pH value, stirs once more, after about 1.5 hours, slowly is warming up to 80 ℃, evaporates excessive solvent, obtains the heavy-gravity dry precursor.Again presoma is placed retort furnace,, treat that organo-functional group decomposes in the system to finish, obtain target product at last, i.e. Gd about 3 hours of 1000 ℃ of roasting temperatures
xY
2-xO
3: Eu
3+Nano red fluorescent material, diameter of particle is about 40-60nm.Its chemical equation can be expressed as follows:
0.1Gd(NO
3)
3+0.9Y(NO
3)
3+0.05Eu(NO
3)
3+3.10MAO+xNH
3·H
2O
→[Ln(MAO)
3]complex+x’NH
3·H
2O
→Gd
xY
2-xO
3:Eu
3++CO
2↑+H
2O↑+NH
3↑+NO
2↑
Take by weighing the hexadecanol (about 4.85g) of 20mmol (about 1.96g) MALEIC ANHYDRIDE and amount of substance such as grade respectively, place round-bottomed flask, regulate oil bath temperature between 110-115 ℃, refluxed 16 hours, product normal hexane recrystallization 2-3 time, obtain white powder, be MALEIC ANHYDRIDE hexadecanol monoesters (MAH).
Get excessive slightly MAH (3.1mmol) and join in 95% ethanolic soln, use NaCO after waiting to dissolve
3Solution is regulated the pH value to 7-8, then to wherein slowly adding Gd (NO
3)
36H
2O (0.3mmol), Y (NO
3)
36H
2O (0.7mmol) and Eu (NO
3)
36H
2O (0.05mmol) (nGd: Y: Eu=0.3: 0.7: 0.05) ethanolic soln places on the constant temperature blender with magnetic force and stirs, and treats to use NaCO after solution evenly
3Solution is transferred to 7-8 with pH value, stirs once more, after about 1.2 hours, slowly is warming up to 85 ℃, evaporates excessive solvent, obtains the heavy-gravity dry precursor.Again presoma is placed retort furnace,, treat that organo-functional group decomposes in the system to finish, obtain target product at last, i.e. Gd about 3.5 hours of 900 ℃ of roasting temperatures
xY
2-xO
3: Eu
3+Nano red fluorescent material, diameter of particle is about 45-65nm.Its chemical equation can be expressed as follows:
0.3Gd(NO
3)
3+0.7Y(NO
3)
3+0.05Eu(NO
3)
3+3.10MAH+xNH
3·H
2O
→[Ln(MAH)
3]complex+x’NH
3·H
2O
→Gd
xY
2-xO
3:Eu
3++CO
2↑+H
2O↑+NH
3↑+NO
2↑
Embodiment 3
Take by weighing the stearyl alcohol (about 5.41g) of 20mmol (about 1.96g) MALEIC ANHYDRIDE and amount of substance such as grade respectively, place round-bottomed flask, regulate oil bath temperature between 110-115 ℃, refluxed 16 hours, product normal hexane recrystallization 2-3 time, obtain white powder, be MALEIC ANHYDRIDE stearyl alcohol monoesters (MAO).
Get excessive slightly MAO (3.1mmol) and join in 95% ethanolic soln, use NaCO after waiting to dissolve
3Solution is regulated the pH value to 7-8, then to wherein slowly adding Gd (NO
3)
36H
2O (0.5mmol), Y (NO
3)
36H
2O (0.5mmol) and Eu (NO
3)
36H
2O (0.05mmol) (nGd: Y: Eu=0.5: 0.5: 0.05) ethanolic soln places on the constant temperature blender with magnetic force and stirs, and treats to use NaCO after solution evenly
3Solution is transferred to 7-8 with the pH value, stirs once more, after 1.2 hours, slowly is warming up to 85 ℃, evaporates excessive solvent, obtains the heavy-gravity dry precursor.Again presoma is placed retort furnace,, treat that organo-functional group decomposes in the system to finish, obtain target product at last, i.e. Gd 1000 ℃ of roasting temperatures 3 hours
xY
2-xO
3: Eu
3+Nano red fluorescent material, diameter of particle is about 40-70nm.Its chemical equation can be expressed as follows:
0.5Gd(NO
3)
3+0.5Y(NO
3)
3+0.05Eu(NO
3)
3+3.10MAO+xNH
3·H
2O
→[Ln(MAO)
3]complex+x’NH
3·H
2O
→Gd
xY
2-xO
3:Eu
3++CO
2↑+H
2O↑+NH
3↑+NO
2↑
The X-ray diffractogram of this nano fluorescent powder, scanning electron microscope diagram, transmission electron microscope figure, uv drs spectrogram, excitation spectrum and emmission spectrum are respectively as Fig. 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5 and shown in Figure 6.X-ray diffractogram shows, Gd
xY
2-xO
3: Eu
3+Material is a crystallization phases, has body-centered cubic structure and degree of crystallinity preferably, and size of microcrystal is about 70nm; Scanning electron microscope diagram and transmission electron microscope figure show, Gd
xY
2-xO
3: Eu
3+The pattern of material is regular, even particle distribution; Uv drs spectrogram, excitation spectrum and emmission spectrum figure illustrate Gd
xY
2-xO
3: Eu
3+Material has sent Eu
3+The emission of ionic ruddiness feature, light intensity is higher, is a kind of ultraviolet and near ultraviolet excitated good red nano-fluorescent powder.
Embodiment 4
Take by weighing the stearyl alcohol (about 5.41g) of 20mmol Tetra hydro Phthalic anhydride (about 2.96g) and amount of substance such as grade respectively, place round-bottomed flask, regulate oil bath temperature between 110-115 ℃, refluxed 16 hours, product normal hexane recrystallization 2-3 time, obtain white powder, be Tetra hydro Phthalic anhydride stearyl alcohol monoesters (Phth-O).
Get excessive slightly (Phth-O) and (3.1mmol) join in 95% ethanolic soln, use NaCO after waiting to dissolve
3Solution is regulated the pH value to 7-8, then to wherein slowly adding Gd (NO
3)
36H
2O (0.7mmol), Y (NO
3)
36H
2O (0.3mmol) and Eu (NO
3)
36H
2O (0.05mmol) (nGd: Y: Eu=0.7: 0.3: 0.05) ethanolic soln places on the constant temperature blender with magnetic force and stirs, and treats to use NaCO after solution evenly
3Solution is transferred to 7-8 with pH value, stirs once more, after 2 hours, slowly is warming up to 80 ℃, evaporates excessive solvent, obtains the heavy-gravity dry precursor.Again presoma is placed retort furnace,, treat that organo-functional group decomposes in the system to finish, obtain target product at last, i.e. Gd 1100 ℃ of roasting temperatures 2.5 hours
xY
2-xO
3: Eu
3+Nano red fluorescent material, diameter of particle is about 45-65nm.Its chemical equation can be expressed as follows:
0.7Gd(NO
3)
3+0.3Y(NO
3)
3+0.05Eu(NO
3)
3+3.10Phth-O+xNH
3·H
2O
→[Ln(Phth-O)
3]complex+x’NH
3·H
2O
→Gd
xY
2-xO
3:Eu
3++CO
2↑+H
2O↑+NH
3↑+NO
2↑
Embodiment 5
Take by weighing the eicosanol (about 5.96g) of 20mmol Tetra hydro Phthalic anhydride (about 2.96g) and amount of substance such as grade respectively, place round-bottomed flask, regulate oil bath temperature between 110-115 ℃, refluxed 16 hours, product normal hexane recrystallization 2-3 time, obtain white powder, be Tetra hydro Phthalic anhydride eicosanol monoesters (Phth-E).
Get excessive slightly Phth-E (3.1mmol) and join in 95% ethanolic soln, use NaCO after waiting to dissolve
3Solution is regulated the pH value to 7-8, then to wherein slowly adding Gd (NO
3)
36H
2O (0.9mmol), Y (NO
3)
36H
2O (0.1mmol) and Eu (NO
3)
36H
2O (0.05mmol) (nGd: Y: Eu=0.9: 0.1: 0.05) ethanolic soln places on the constant temperature blender with magnetic force and stirs, and treats to use NaCO after solution evenly
3Solution is transferred to 7-8 with the pH value, stirs once more, after about 1.5 hours, slowly is warming up to 80 ℃, evaporates excessive solvent, obtains the heavy-gravity dry precursor.Again presoma is placed retort furnace,, treat that organo-functional group decomposes in the system to finish, obtain target product at last, i.e. Gd about 3 hours of 1000 ℃ of roasting temperatures
xY
2-xO
3: Eu
3+Nano red fluorescent material, diameter of particle is about 45-70nm.Its chemical equation can be expressed as follows:
0.9Gd(NO
3)
3+0.1Y(NO
3)
3+0.05Eu(NO
3)
3+3.10Phth-E+xNH
3·H
2O
→[Ln(Phth-E)
3]complex+x’NH
3·H
2O
→Gd
xY
2-xO
3:Eu
3++CO
2↑+H
2O↑+NH
3↑+NO
2↑
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (5)
1, a kind of red fluorescence powder is characterized in that this fluorescent material chemical formula is Gd
xY
2-xO
3: Eu
3+, wherein, x is 0.2,0.6,1.0,1.4 or 1.8, and this fluorescent material pattern is regular, arranges evenly, and median size is below 80nm.
2, a kind of preparation method of red nano-fluorescent powder as claimed in claim 1 is characterized in that concrete steps are as follows:
(1) preparation of organic ligand:
With anhydrides organic molecule and long-chain alcohol is raw material, and under 110-115 ℃ of oil bath temperature backflow 15-16 hour, products therefrom normal hexane recrystallization obtained white powder, is to have amphipathic long-chain organic functional molecular, as part; Wherein: the proportioning of anhydrides organic molecule and long-chain alcohol amount of substance is 1: 1;
(2) preparation of presoma:
With rare earth oxide yttrium oxide Y
2O
3, gadolinium sesquioxide Gd
2O
3With europium sesquioxide Eu
2O
3Handle by concentrated nitric acid respectively, obtain corresponding nitric hydrate salt compound Y (NO
3)
36H
2O, Gd (NO
3)
36H
2O and Eu (NO
3)
36H
2O joins in the ethanolic soln of the amphipathic organic functions part of step (1) gained then successively, and the pH value of regulator solution is 7-8, stirs, treat that solution evenly after, solvent evaporated obtains thickness exsiccant amphipathic rare-earth organic precursor; Wherein: Gd (NO
3)
3.6H
2O, Y (NO
3)
36H
2O and Eu (NO
3)
36H
2The mol ratio of O is 1: 9: 0.5--9: 1: 0.5;
(3) the amphipathic rare-earth organic precursor of step (2) gained is handled through high temperature pyrolysis, promptly got desired product;
Wherein, the anhydrides organic molecule is MALEIC ANHYDRIDE or Tetra hydro Phthalic anhydride described in the step (1), long-chain alcohol described in the step (1) be in hexadecanol, stearyl alcohol, eicosanol or the behenyl alcohol any.
3, the preparation method of red nano-fluorescent powder according to claim 2 is characterized in that pH value conditioning agent is NaCO described in the step (2)
3Solution.
4, the preparation method of red nano-fluorescent powder according to claim 2 is characterized in that churning time is 1.2-2 hour described in the step (2), and the temperature of solvent evaporated is 80-85 ℃.
5, the preparation method of red nano-fluorescent powder according to claim 2 is characterized in that pyrolysis temperature is 900-1100 ℃ described in the step (3), and pyrolysis time is 2.5-3.5 hour.
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| CN1506439A (en) * | 2002-12-07 | 2004-06-23 | 中国科学院长春光学精密机械与物理研 | Red RE oxide luminophor and its prepn |
| CN1635048A (en) * | 2003-12-30 | 2005-07-06 | 北京方正稀土科技研究所有限公司 | Rare earth red fluorescent powder and method for making same |
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| CN1506439A (en) * | 2002-12-07 | 2004-06-23 | 中国科学院长春光学精密机械与物理研 | Red RE oxide luminophor and its prepn |
| CN1635048A (en) * | 2003-12-30 | 2005-07-06 | 北京方正稀土科技研究所有限公司 | Rare earth red fluorescent powder and method for making same |
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