CN104059652A - Metal nanoparticle-doped columbate luminescent material and preparation method thereof - Google Patents

Metal nanoparticle-doped columbate luminescent material and preparation method thereof Download PDF

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CN104059652A
CN104059652A CN201310089492.1A CN201310089492A CN104059652A CN 104059652 A CN104059652 A CN 104059652A CN 201310089492 A CN201310089492 A CN 201310089492A CN 104059652 A CN104059652 A CN 104059652A
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luminescent material
nano particle
doped
metal nano
preparation
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周明杰
王荣
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention discloses a metal nanoparticle-doped columbate luminescent material and a preparation method thereof, belonging to the field of luminescent materials. The general chemical formula of the luminescent material is Gd2-xScNbO7:Eux,My, wherein M is at least one selected from metal nanoparticles consisting of Ag, Au, Pt, Pd and Cu, x is more than 0 and no more than 1.5, and y is the mol ratio of M to Gd2-xScNbO7:Eux and is more than 0 and no more than 1 * 10<-2>. In the metal nanoparticle-doped columbate luminescent material, the M metal particle is introduced, so the columbate luminescent material has greatly improved luminous efficiency under same excitation conditions, the wavelength of emitted light is not changed, color purity and luminance of light emitted under excitation are high, and the columbate luminescent material can be applied to field emission devices.

Description

Metal nano particle-doped niobate luminescent material and preparation method
Technical field
The present invention relates to field of light emitting materials, relate in particular to a kind of metal nano particle-doped niobate luminescent material and preparation method.
Background technology
Field Emission Display is a kind of New flat panel display, and its principle of work and CRT are similar.One of key factor of preparing premium properties FED is the preparation of fluorescent material.Current most of FED fluorescent material is to use for reference traditional CRT fluorescent material type, and it is improved.The fluorescent material adopting is mainly sulfide and oxide compound.For sulphide fluorescent material, luminosity is higher, and there is certain electroconductibility, but poor stability, under low-voltage, high-current beam bombardment, easily decompose and produce, decompose the sulphur anticathode emission needle producing and have " poisoning " effect, the throw out of generation covers phosphor surface, reduce the luminous efficiency of fluorescent material, shortened the work-ing life of FED.Oxide fluorescent powder good stability, but luminous efficiency is relatively low, and both performances all need to be improved and improve.
Summary of the invention
Problem to be solved by this invention is to provide the metal nano particle-doped niobate luminescent material that a kind of luminous efficiency is higher, can be used for field transmitting.
Technical scheme of the present invention is as follows:
A metal nano particle-doped niobate luminescent material, its chemical general formula is: Gd 2-xscNbO 7: Eu x, M y, wherein, M is metal nano particle-doped, is selected from least one in Ag, Au, Pt, Pd, Cu metal nanoparticle, and x is the mole number that Eu atom replaces Gd atom, and the span of x is 0<x≤1.5, and y is M and Gd 2-xscNbO 7: Eu xmole ratio, the span of y is 0 < y≤1 × 10 -2; Gd 2-xscNbO 7: Eu is luminescent material, and colon ": " is expressed as the doping of Eu.
Described metal nano particle-doped niobate luminescent material, preferably, the span of x is 0.02≤x≤1.0, the span of y is 1 × 10 -5≤ y≤5 × 10 -3.
The preparation method who the invention still further relates to a kind of metal nano particle-doped niobate luminescent material, comprises the steps:
By after the auxiliary agent and reductive agent hybrid reaction of the salts solution of M, a dissemination, make M nanometer particle colloid solution;
According to Gd 2-xscNbO 7: Eu x, M yin each element chemistry metering ratio, measure aqueous ethanolic solution, the Nb salts solution of Gd, Sc and Eu salt, then measure described M nanometer particle colloid, then add citric acid complexing agent and polyglycol surfactants, in 60～80 DEG C of stirring 2～6h, obtain precursor sol; Wherein, the mol ratio of citric acid and Gd, Sc, Nb, the total metal ion sum of Eu is 1～5:1, and the concentration of polyoxyethylene glycol is 0.05～0.20g/mL;
Precursor sol is dried to 6～20h in 70～150 DEG C, make solvent evaporates, obtain xerogel, grind xerogel, grinding powder is put in retort furnace in air in 400～800 DEG C of pre-burnings 2～6 hours, grinds again pre-sintered sample after cooling, and then by pre-sintered sample powder in 1300-1600 ° of C calcining 2-12h, be cooled to room temperature, grinding, obtaining chemical general formula is Gd 2-xscNbO 7: Eu x, M ymetal nano particle-doped niobate luminescent material;
In above-mentioned steps, M is at least one in Ag, Au, Pt, Pd, Cu metal nanoparticle, and x is the mol ratio that Eu atom replaces Gd atom, and the span of x is 0<x≤1.5, and y is M and Gd 2-xscNbO 7: Eu xmole ratio, the span of y is 0 < y≤1 × 10 -2.
The preparation method of described metal nano particle-doped niobate luminescent material, preferably, described reductive agent is at least one in hydrazine hydrate, xitix, Trisodium Citrate or sodium borohydride, the mol ratio of described reductive agent and M is 0.5:1～10:1; In actual use, reductive agent need to be configured to the aqueous solution, and its concentration is 1 × 10 -4mol/L～1mol/L; Auxiliary agent is at least one in polyethylene arsenic pyrrolidone (PVP), Trisodium Citrate, cetyl trimethylammonium bromide, sodium lauryl sulphate or sodium laurylsulfonate, and the content of the addition of auxiliary agent in the M nanometer particle colloid solution finally obtaining is 1 × 10 -4g/mL～5 × 10 -2g/mL.
The preparation method of described metal nano particle-doped niobate luminescent material, preferably, the time of salts solution, auxiliary agent and the reductive agent hybrid reaction of M is 10～45min.
The preparation method of described metal nano particle-doped niobate luminescent material, preferably, the molecular weight of described polyoxyethylene glycol is 100-20000, is expressed as polyoxyethylene glycol 100-20000, lower same, more preferably, the molecular weight of described polyoxyethylene glycol is 2000-10000; Polyoxyethylene glycol is tensio-active agent, and the concentration of polyoxyethylene glycol is 0.05～0.30g/mL.
The preparation method of described metal nano particle-doped niobate luminescent material, wherein, Gd, Sc and Eu salt are each self-corresponding nitrate or acetate; Nb salt is Nb 5+oxalic acid solution.
Gd, Sc and Eu salt aqueous ethanolic solution are separately to adopt following methods to make:
Taking the oxide compound of Gd, Sc and Eu and carbonate as raw material, be dissolved in nitric acid respectively, then to add volume ratio be in the second alcohol and water of 3～8:1, obtain respectively the aqueous ethanolic solution of Gd, Sc and Eu salt; Or taking the acetate of Gd, Sc and Eu, nitrate as raw material, being dissolved in volume ratio is in the second alcohol and water of 3～8:1, obtains respectively the aqueous ethanolic solution of Gd, Sc and Eu salt.
Nb salts solution is to adopt following steps to make:
First by Nb 2o 5evenly mix with KOH, at 350 DEG C, calcine 2h and obtain solubility potassium niobate;
Secondly, potassium niobate is dissolved in distilled water, and adding nitric acid to pH value is 2～3, forms cotton-shaped precipitation [Nb (OH) 5nH 2o];
Finally, this precipitation is all dissolved into oxalic acid, fully stirs, form the transparent Nb of light green 5+oxalic acid solution, i.e. solubility niobium salt.
The preparation method of described metal nano particle-doped niobate luminescent material, preferably, the span of x is 0.02≤x≤1.0, the span of y is 1 × 10 -5≤ y≤5 × 10 -3.
The preparation method of metal nano particle-doped niobate luminescent material provided by the invention, adopts sol-gel method to prepare the Gd that contains metal nanoparticle 2-xscNbO 7: Eu xluminescent material, by the metal nano particle-doped light-emitting phosphor that strengthens.The luminous efficiency of niobate luminescent material under same shooting conditions is greatly improved, and radiative wavelength does not change.
In above-mentioned metal nano particle-doped niobate luminescent material, introduce M metallics, the luminous efficiency of niobate luminescent material under same shooting conditions is greatly improved, and radiative wavelength does not change, purity of color and the brightness of after being stimulated, launching bright dipping are all higher, can be applied to feds.
The preparation method of metal nano particle-doped niobate luminescent material of the present invention, processing step is few, relatively simple; Processing condition are not harsh, easily reach, and cost is low; Do not introduce other impurity, the luminescent material quality obtaining is high, can be widely used in the preparation of luminescent material.
Brief description of the drawings
Fig. 1 is that luminescent material and the comparative example luminescent material that the embodiment of the present invention 2 makes is the luminescent spectrum comparison diagram under the cathode-ray exciting under 1.5KV at acceleration voltage; Wherein, curve 1 is the Gd that is mixed with metal nanoparticle Ag prepared by the present embodiment 2 1.9scNbO 7: Eu 0.1, Ag 2.5 × 10the luminescent spectrum of-4 luminescent materials, curve 2 is Gd that comparative example is not mixed with metal nanoparticle Ag 1.9scNbO 7: Eu 0.1the luminescent spectrum of luminescent material.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
Sol-gel method is prepared Gd 1.98scNbO 7: Eu 0.02, Pd 1 × 10-5
Preparation containing Pd nanoparticle sol: take 0.22mg Palladous chloride (PdCl 22H 2o) be dissolved in the deionized water of 10mL; Under the condition of magnetic agitation, 11.0mg Trisodium Citrate and 4.0mg sodium lauryl sulphate are dissolved in above-mentioned palladium chloride solution; Take 0.38mg sodium borohydride and be dissolved in 100mL deionized water, obtaining concentration is 1 × 10 -4the sodium borohydride solution of mol/L; Under the condition of magnetic agitation, in above-mentioned palladium chloride solution, add fast the above-mentioned sodium borohydride solution of 10mL, reaction 20min, obtaining 20mL Pd nanoparticle concentration is 5 × 10 -5the colloidal sol of mol/L.
Take 33.2263gNb 2o 5evenly mix with 14.0275g KOH, at 350 DEG C, calcine 2h and obtain solubility potassium niobate.Potassium niobate is dissolved in distilled water, and adding nitric acid to pH value is 2～3, forms cotton-shaped precipitation [Nb (OH) 5nH 2o].This resolution of precipitate, in 150mL4.5mol/L oxalic acid, is fully stirred, be settled to 250mL, form the transparent Nb of light green 5+oxalic acid solution, i.e. 1mol/L solubility niobium salt.
Take 2.6478g Gd (CH 3cOO) 3, 0.884g Sc (CH 3cOO) 3, 0.0263g Eu (CH 3cOO) 3with the above-mentioned Nb preparing of 4mL1mol/L 5+oxalic acid solution is placed in container, and then adding 50mL volume ratio is the mixing solutions of the second alcohol and water of 4:1, and under 80 DEG C of stirring in water bath conditions, adding 0.8mL concentration is 5 × 10 -5pd nano particle colloidal sol, 3.0742g citric acid and the 9g polyoxyethylene glycol 100 of mol/L, stir the precursor sol that obtains homogeneous transparent for 2 hours.
Precursor sol dry 20h solvent flashing at 70 DEG C is obtained to xerogel, then by the xerogel grind into powder obtaining, put into high temperature box furnace calcining at constant temperature 2h at 800 DEG C, then in 1300 DEG C of calcining 10h, be cooled to room temperature and obtain Gd 1.98scNbO 7: Eu 0.02, Pd 1 × 10-5 niobate luminescent materials.
Embodiment 2
Sol-gel method is prepared Gd 1.9scNbO 7: Eu 0.1, Ag 2.5 × 10-4:
Preparation containing Ag nanoparticle sol: take 3.4mg Silver Nitrate (AgNO 3) be dissolved in the deionized water of 18.4mL; Under the condition of magnetic agitation, 42mg Trisodium Citrate is dissolved in above-mentioned silver nitrate solution; Take 5.7mg sodium borohydride and be dissolved in 10mL deionized water, obtaining concentration is 1.5 × 10 -2the sodium borohydride solution of mol/L; Under the condition of magnetic agitation, to the disposable above-mentioned sodium borohydride solution of 1.6mL that adds in above-mentioned silver nitrate solution, continue reaction 10min, obtaining 20mL Ag nanoparticle concentration is 1 × 10 -3the colloidal sol of mol/L.
Nb 5+the preparation of oxalic acid solution is identical with embodiment 1.
Take 2.6088g Gd (NO 3) 3, 0.9238g Sc (NO 3) 3, 0.1352g Eu (NO 3) 3the Nb preparing with 4mL1mol/L 5+oxalic acid solution is placed in container, and then adding 50mL volume ratio is the mixing solutions of the second alcohol and water of 8:1, and under 70 DEG C of stirring in water bath conditions, adding 1mL concentration is 1 × 10 -3ag nano particle colloidal sol, 6.1484g citric acid and the 5.4g PEG20000 of mol/L, stir the precursor sol that obtains homogeneous transparent for 4 hours.
Precursor sol dry 8h solvent flashing at 120 DEG C is obtained to xerogel, then by the xerogel grind into powder obtaining, put into high temperature box furnace calcining at constant temperature 4h at 600 DEG C, then in 1400 DEG C of calcining 5h, be cooled to room temperature and obtain Gd 1.9scNbO 7: Eu 0.1, Ag 2.5 × 10-4 niobate luminescent materials.
Fig. 1 is that luminescent material and the comparative example luminescent material that the embodiment of the present invention 2 makes is the luminescent spectrum comparison diagram under the cathode-ray exciting under 1.5KV at acceleration voltage; Wherein, curve 1 is the Gd that is mixed with metal nanoparticle Ag prepared by the present embodiment 2 1.9scNbO 7: Eu 0.1, Ag 2.5 × 10the luminescent spectrum of-4 luminescent materials, curve 2 is the Gd that are not mixed with metal nanoparticle Ag 1.9scNbO 7: Eu 0.1the luminescent spectrum of luminescent material.
As can be seen from Figure 1,, at the emission peak at 613nm place, the luminous intensity of metal nano particle-doped rear luminescent material has strengthened 20% before not adulterating.
Embodiment 3
Sol-gel method is prepared Gd 1.5scNbO 7: Eu 0.5, Pt 5 × 10-3
Preparation containing Pt nanoparticle sol: take 25.9mg Platinic chloride (H 2ptCl 66H 2o) be dissolved in the deionized water of 17mL; Under the condition of magnetic agitation, 400mg Trisodium Citrate and 600mg sodium laurylsulfonate are dissolved in above-mentioned platinum acid chloride solution; Take 1.9mg sodium borohydride and be dissolved in 10mL deionized water, obtaining concentration is 5 × 10 -3the sodium borohydride solution of mol/L; Prepare 10mL concentration is 5 × 10 simultaneously -2the hydrazine hydrate solution of mol/L; Under the condition of magnetic agitation, first in above-mentioned platinum acid chloride solution, drip the above-mentioned sodium borohydride solution of 0.4mL, after reaction 5min, then add the above-mentioned hydrazine hydrate solution of 2.6mL in above-mentioned platinum acid chloride solution, continue reaction 40min, obtaining 20mL Pt nanoparticle concentration is 2.5 × 10 -3the colloidal sol of mol/L.
Nb 5+the preparation of oxalic acid solution is identical with embodiment 1.
Take 1.4835g Gd 2(CO 3) 3, 0.5398g Sc 2(CO 3) 3with 0.4839g Eu 2(CO 3) 3, by 6mL rare nitric acid heating for dissolving in container, the Nb that adds 4mL1mol/L to prepare after cooling 5+oxalic acid solution, after stirring, adding 50mL volume ratio is the mixing solutions of the second alcohol and water of 3:1, under 65 DEG C of stirring in water bath conditions, adding 2.5mL concentration is 1 × 10 -2pt nano particle colloidal sol, 9.2226g citric acid and the 12.5g Macrogol 200 of mol/L, stir the precursor sol that obtains homogeneous transparent for 4 hours.
Precursor sol dry 8h solvent flashing at 100 DEG C is obtained to xerogel, then by the xerogel grind into powder obtaining, put into high temperature box furnace calcining at constant temperature 3h at 700 DEG C, then in 1500 DEG C of calcining 12h, be cooled to room temperature and obtain Gd 1.5scNbO 7: Eu 0.5, Pt 5 × 10-3 niobate luminescent materials.
Embodiment 4
Sol-gel method is prepared Gd 1.2scNbO 7: Eu 0.8, Au 1 × 10-2
Preparation containing Au nanoparticle sol: take 48.4mg hydrochloro-auric acid (AuCl 3hCl4H 2o) be dissolved in the deionized water of 10mL; Under the condition of magnetic agitation, 14mg Trisodium Citrate and 6mg cetyl trimethylammonium bromide are dissolved in above-mentioned chlorauric acid solution; Take 1.9mg sodium borohydride and be dissolved in 10mL deionized water, obtaining concentration is 5 × 10 -3the sodium borohydride solution of mol/L; Take 17.6mg dissolution of ascorbic acid in 10mL deionized water, obtaining concentration is 1 × 10 -2the ascorbic acid solution of mol/L; Under the condition of magnetic agitation, first in above-mentioned chlorauric acid solution, add the above-mentioned sodium borohydride solution of 5mL, after reaction 5min, then add the above-mentioned ascorbic acid solution of 5mL in above-mentioned chlorauric acid solution, continue reaction 20min, obtaining 20mLAu nanoparticle concentration is 5 × 10 -3the colloidal sol of mol/L.
Nb 5+the preparation of oxalic acid solution is identical with embodiment 1.
Take 0.8699g Gd 2o 3, 0.2764g Sc 2o 3with 0.5630g Eu 2o 3, by 2mL concentrated nitric acid and 4mL deionized water heating for dissolving in container, the Nb that adds 4mL1mol/L to prepare after cooling 5+oxalic acid solution, after stirring, adding 50mL volume ratio is the mixing solutions of the second alcohol and water of 3:1, under 60 DEG C of stirring in water bath conditions, adding 0.6mL concentration is 5 × 10 -4au nano particle colloidal sol, 15.3725g citric acid and the 6g Macrogol 2000 of mol/L, stir the precursor sol that obtains homogeneous transparent for 4 hours.
Precursor sol dry 6h solvent flashing at 150 DEG C is obtained to xerogel, then by the xerogel grind into powder obtaining, put into high temperature box furnace calcining at constant temperature 6h at 500 DEG C, then in 1600 DEG C of calcining 2h, be cooled to room temperature and obtain Gd 1.2scNbO 7: Eu 0.8, Au 1 × 10-2 niobate luminescent materials.
Embodiment 5
Sol-gel method is prepared Gd 0.5scNbO 7: Eu 1.5, Cu 1 × 10-4
Preparation containing Cu nanoparticle sol: take 1.6mg cupric nitrate (Cu (NO 3) 2) be dissolved in the deionized water of 16mL; Under the condition of magnetic agitation, 2mg polyethylene arsenic pyrrolidone (PVP) is dissolved in above-mentioned copper nitrate solution; Take 0.4mg sodium borohydride and be dissolved in 10mL ethanol, obtaining concentration is 1 × 10 -3the sodium borohydride alcoholic solution of mol/L; Under the condition of magnetic agitation, in above-mentioned copper nitrate solution, slowly splash into the above-mentioned sodium borohydride alcoholic solution of 4mL, continue reaction 10min, obtaining 20mL Cu nanoparticle concentration is 4 × 10 -4the colloidal sol of mol/L.
Nb 5+the preparation of oxalic acid solution is identical with embodiment 1.
Take 0.6865g Gd (NO 3) 3, 0.9238g Sc (NO 3) 3, 2.0278g Eu (NO 3) 3the Nb preparing with 4mL1mol/L 5+oxalic acid solution is placed in container, and then adding 50mL volume ratio is the mixing solutions of the second alcohol and water of 4:1, and under 60 DEG C of stirring in water bath conditions, adding 1.5mL concentration is the Mn (NO of 0.01mol/L 3) 2cu nanometer particle colloid solution, 8.6454g citric acid and 2.775g PEG 20000 that solution, 2.5mL concentration are 6 × 10-4mol/L, stir the precursor sol that obtains homogeneous transparent for 6 hours.
Precursor sol dry 15h solvent flashing at 80 DEG C is obtained to xerogel, then by the xerogel grind into powder obtaining, put into high temperature box furnace calcining at constant temperature 3h at 600 DEG C, then in 1450 DEG C of calcining 8h, be cooled to room temperature and obtain Gd 0.5scNbO 7: Eu 1.5, Cu 1 × 10-4 niobate luminescent materials.
Embodiment 6
Sol-gel method is prepared Gd 1.8scNbO 7: Eu 0.2, (Ag 0.5/ Au 0.5) 1.25 × 10-3
Preparation containing Ag and Au nanoparticle sol: take 6.2mg hydrochloro-auric acid (AuCl 3hCl4H 2and 2.5mg Silver Nitrate (AgNO O) 3) be dissolved in the deionized water of 28mL, obtain mixing solutions; Under the condition of magnetic agitation, 22mg Trisodium Citrate and 20mg polyethylene arsenic pyrrolidone (PVP) are dissolved in above-mentioned mixing solutions; Take 380mg sodium borohydride and be dissolved in 10mL deionization, obtain the sodium borohydride solution that concentration is 1mol/L; Under the condition of magnetic agitation, to the disposable above-mentioned sodium borohydride solution of 0.3mL that adds in above-mentioned mixing solutions, continue reaction 20min, obtain 30mL Ag and Au nanoparticle concentration sum is 1 × 10 -3the colloidal sol of mol/L.
Nb 5+the preparation of oxalic acid solution is identical with embodiment 1.
Take 1.3049g Gd 2o 3, 0.2764g Sc 2o 3with 0.1407g Eu 2o 3after wetting, by 1mL concentrated nitric acid and 1mL deionized water heating for dissolving in container, the Nb that adds 4mL1mol/L to prepare after cooling 5+oxalic acid solution, after stirring, adding 50mL volume ratio is the mixing solutions of the second alcohol and water of 3:1, under 70 DEG C of stirring in water bath conditions, adding 6.25mL concentration is 1 × 10 -3ag/Au nano particle colloidal sol, 12.2968g citric acid and the 10.8g Macrogol 4000 of mol/L, stir the precursor sol that obtains homogeneous transparent for 4 hours.
Precursor sol dry 12h solvent flashing at 100 DEG C is obtained to xerogel, then by the xerogel grind into powder obtaining, put into high temperature box furnace calcining at constant temperature 6h at 400 DEG C, then in 1350 DEG C of calcining 6h, be cooled to room temperature and obtain Gd 1.8scNbO 7: Eu 0.2, (Ag 0.5/ Au 0.5) 1.25 × 10-3 niobate luminescent materials.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.

Claims (10)

1. a metal nano particle-doped niobate luminescent material, is characterized in that, its chemical general formula is Gd 2-xscNbO 7: Eu x, M y, wherein, M is metal nano particle-doped, is selected from least one in Ag, Au, Pt, Pd, Cu metal nanoparticle, and x is the mole number that Eu atom replaces Gd atom, and the span of x is 0<x≤1.5, and y is M and Gd 2-xscNbO 7: Eu xmole ratio, the span of y is 0 < y≤1 × 10 -2.
2. metal nano particle-doped niobate luminescent material according to claim 1, is characterized in that, the span of x is 0.02≤x≤1.0, and the span of y is 1 × 10 -5≤ y≤5 × 10 -3.
3. a preparation method for metal nano particle-doped niobate luminescent material, is characterized in that, comprises the steps:
By after the auxiliary agent and reductive agent hybrid reaction of the salts solution containing M, a dissemination, make M nanometer particle colloid solution;
According to Gd 2-xscNbO 7: Eu x, M yin each element chemistry metering ratio, measure aqueous ethanolic solution, the Nb salts solution of Gd, Sc and Eu salt, then measure described M nanometer particle colloid, then add citric acid complexing agent and polyoxyethylene glycol table promoting agent, stir 2～6h in 60～80 DEG C, obtain precursor sol; Wherein, the mol ratio of citric acid and Gd, Sc, Nb, the total metal ion sum of Eu is 1～5:1; The concentration of polyoxyethylene glycol is 0.05～0.20g/mL;
Precursor sol is dried to 6～20h in 70～150 DEG C, make solvent evaporates, obtain xerogel, grind xerogel, grinding powder is put in retort furnace in air in 400～800 DEG C of pre-burnings 2～6 hours, grinds again pre-sintered sample after cooling, and then by pre-sintered sample powder in 1300-1600 ° of C calcining 2-12h, be cooled to room temperature, grinding, obtaining chemical general formula is Gd 2-xscNbO 7: Eu x, M ymetal nano particle-doped niobate luminescent material;
In above-mentioned steps, M is metal nano particle-doped, is selected from least one in Ag, Au, Pt, Pd, Cu metal nanoparticle, and x is the mole number that Eu atom replaces Gd atom, and the span of x is 0<x≤1.5, and y is M and Gd 2-xscNbO 7: Eu xmole ratio, the span of y is 0 < y≤1 × 10 -2.
4. the preparation method of metal nano particle-doped niobate luminescent material according to claim 3, it is characterized in that, described auxiliary agent is at least one in polyethylene arsenic pyrrolidone, Trisodium Citrate, cetyl trimethylammonium bromide, sodium lauryl sulphate or sodium laurylsulfonate; Described reductive agent is at least one in hydrazine hydrate, xitix, Trisodium Citrate or sodium borohydride; The content of the addition of described auxiliary agent in the M nanometer particle colloid solution finally obtaining is 1 × 10 -4g/mL～5 × 10 -2g/mL, the mol ratio of described reductive agent and M is 0.5:1～10:1.
5. the preparation method of metal nano particle-doped niobate luminescent material according to claim 3, is characterized in that, the time that contains salts solution, auxiliary agent and the reductive agent hybrid reaction of M is 10～45min.
6. the preparation method of metal nano particle-doped niobate luminescent material according to claim 3, is characterized in that, the molecular weight of described polyoxyethylene glycol is 100-20000.
7. the preparation method of metal nano particle-doped niobate luminescent material according to claim 6, is characterized in that, the molecular weight of described polyoxyethylene glycol is 2000-10000.
8. the preparation method of metal nano particle-doped niobate luminescent material according to claim 3, is characterized in that, Gd, Sc and Eu salt are each self-corresponding nitrate or acetate; Nb salt is Nb 5+oxalic acid solution.
9. the preparation method of metal nano particle-doped niobate luminescent material according to claim 3, is characterized in that, in described aqueous ethanolic solution, the volume ratio of ethanol and water is 3～8:1.
10. the preparation method of metal nano particle-doped niobate luminescent material according to claim 3, is characterized in that, the span of x is 0.02≤x≤1.0, and the span of y is 1 × 10 -5≤ y≤5 × 10 -3.
CN201310089492.1A 2013-03-20 2013-03-20 Metal nanoparticle-doped columbate luminescent material and preparation method thereof Pending CN104059652A (en)

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Application publication date: 20140924