CN105219388A - A kind of Er ions lanthanum yttrium oxide luminescent material and preparation method thereof - Google Patents
A kind of Er ions lanthanum yttrium oxide luminescent material and preparation method thereof Download PDFInfo
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- CN105219388A CN105219388A CN201510605072.3A CN201510605072A CN105219388A CN 105219388 A CN105219388 A CN 105219388A CN 201510605072 A CN201510605072 A CN 201510605072A CN 105219388 A CN105219388 A CN 105219388A
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Abstract
The invention discloses a kind of Er ions lanthanum yttrium oxide luminescent material and preparation method thereof.The biomolecule expressions of luminescent material of the present invention is: (Er
xy
1-x-yla
y)
2o
3, wherein, 0 & lt; X≤0.05,0.08≤y≤0.1.The present invention uses low temperature micro-gel flooding to prepare described Er ions lanthanum yttrium oxide luminescent material, comprising: the high-temperature calcination of the polymeric gel of nitrate solution and incendiary material, the low temperature spontaneous combustion of gel, presoma.Er ions lanthanum yttrium oxide luminescent material of the present invention has good optical property, due to La
3+introducing, its green upper conversion and 1.5 ~ 1.6 μm of near infrared emission intensity can be significantly improved simultaneously, and its chemical stability and Heat stability is good, nontoxic, radiationless, be the desired illumination material being applied in the fields such as display, temperature sensor, biomarker, medical monitoring, high-precision measurement.
Description
Technical field
The present invention relates to a kind of Er
3+doped luminescent material and preparation method thereof, belongs to field of light emitting materials.
Background technology
Rare earth luminescent material is the base application material in the fields such as green light source, technique of display, optical communication and Laser Devices, has its own strategic significance to national economy, social development and national defense construction.In numerous rare earth ion, Er
3+research emphasis that is luminous and laser field is become because up-conversion luminescence and 1.5 ~ 1.6 μm of near infrared emissions can be realized.And La
3+due to not luminous, be usually considered to not contribute the luminous intensity of material.Due to Er
3+'s
2h
11/2/
4s
3/2→
4i
15/2transition makes it to excite in lower realization green at ir radiation and changes, therefore Er
3+dopant material has been used to the fields such as display material, up-conversion lasing, temperature sensor and oncotherapy.Meanwhile, Er
3+'s
4i
13/2→
4i
15/2transition can realize the output of 1.5 ~ 1.6 mu m wavebands, this wave band corresponds to the low decay of optical fiber and atmospheric communication and low dispersion window, and to the radiation of visual medium and transmissivity low, not easily injure retina, thus can be applicable to the fields such as high-acruracy survey, high speed wide-band communication and medical science.
Er
3+doped luminescent material has high requirements to choosing of substrate material, Er in different substrates material
3+luminous intensity difference very large.Y
2o
3crystal is T
7 htype cubic system, has good heat conductivity, chemical stability and physical strength, lower phonon energy (the highest about 600cm
-1), wide optical clear region (0.2 ~ 8 μm) and be easy to realize the advantages such as rare earth ion doped.Meanwhile, due to Y
2o
3with Er
2o
3there is identical crystalline structure and lattice parameter, Er
3+very easily replace Y
3+case, be conducive to high density Er
3+the realization of doping.Therefore, Y
2o
3er
3+good matrix.At present, Er
3+: Y
2o
3nano luminescent material becomes study hotspot.
But, due to Er
3+absorption cross section low, this makes Er
3+doped luminescent material ubiquity up-conversion fluorescence and the not high problem of 1.5 ~ 1.6 mu m waveband near infrared light intensity, constrain it and further apply.In research in the past, general by mixing other sensitizer ions altogether, utilize energy transfer process to improve Er
3+luminous intensity.Regrettably, according to Er
3+energy level transition feature, the method cannot be taken into account up-conversion luminescence and 1.5 ~ 1.6 mu m wavebands simultaneously and launch.As, utilize Yb
3+as Er
3+sensitizing agent time, although pass through
2f
5/2(Yb
3+)+
4i
13/2(Er
3+) →
2f
7/2(Yb
3+)+
4f
9/2(Er
3+) homenergic transmittance process can improve Er
3+up-conversion emission intensity, but said process will reduce Er
3+'s
4i
13/2energy level population.Due to Er
3+pass through
4i
13/2→
4i
15/2transition realizes the fluorescent emission of 1.5 ~ 1.6 mu m wavebands, therefore goes up energy level
4i
13/2the reduction of population must weaken Er
3+1.5 ~ 1.6 mu m wavebands launch.As can be seen here, Er
3+the enhancing of Up-conversion emission intensity will weaken its 1.5 ~ 1.6 mu m waveband emissive porwer; Vice versa.Therefore, for Er
3+dopant material, is difficult to take into account its up-conversion luminescence and 1.5 ~ 1.6 mu m waveband near-infrared fluorescents usually, and the emissive porwer both how simultaneously improving is the scientific research difficult problem that material supplier author tries hard to solve.
Summary of the invention
The object of the invention is to overcome all or part of defect of prior art and a kind of Er ions lanthanum yttrium oxide luminescent material and preparation method thereof is provided.
Inventive concept of the present invention is: break through people to La
3+the intrinsic understanding of performance, by Y
2o
3non-luminous La is added in matrix
3+, utilize La
3+to Er
3+local crystal field cut out effect, change Er
3+radiation parameter, improve Er thus simultaneously
3+green Up-conversion emission and 1.5 ~ 1.6 mu m waveband near infrared light intensity.Preparation-obtained material is nano level fluorophor powder, and have the advantage that green is above changed and near-infrared luminous brightness is high, it not only can be used as display, sensor, biological fluorescent labelling material, also can be used for the fields such as high-precision measurement, medical monitoring.
For achieving the above object, the technical solution used in the present invention is: the chemical expression of Er ions lanthanum yttrium oxide luminescent material of the present invention is (Er
xy
1-x-yla
y)
2o
3, wherein, 0<x≤0.05,0.08≤y≤0.1.
The preparation method of Er ions lanthanum yttrium oxide luminescent material of the present invention comprises the following steps:
(1) with the Er (NO of analytical pure purity
3)
3, Y (NO
3)
3, La (NO
3)
3solution as raw material, by chemical formula (Er
xy
1-x-yla
y)
2o
3stoichiometric ratio mixing after stir, obtain mixing solutions;
(2) in described mixing solutions, incendiary material is added, Er (NO
3)
3, Y (NO
3)
3with La (NO
3)
3total amount and the mol ratio of incendiary material be 1 ︰ 2 ~ 4, carry out stirring and incendiary material being dissolved completely at 60 ~ 80 DEG C; Then solution is placed in the constant temperature oven heat drying being preheating to 80 ~ 120 DEG C, obtains transparent wet gel;
(3) described transparent wet gel is placed in the retort furnace that furnace temperature is 300 ~ 400 DEG C, is incubated under air atmosphere, wet gel generation spontaneous combustion, obtains presoma after combustion reactions terminates;
(4) by after described presoma grinding evenly, put into the flat-temperature zone of high temperature sintering furnace, calcine 1 ~ 3 hour at 900 ~ 1200 DEG C, obtain Er ions lanthanum yttrium oxide luminescent material.
Further, the present invention, in described step (4), rises to calcining temperature with the temperature rise rate of 10 ~ 20 DEG C/min.
Further, the median size of Er ions lanthanum yttrium oxide luminescent material that the present invention obtains is 20 ~ 40 nanometers.
Further, incendiary material of the present invention is glycine, urea or citric acid.
Compared with prior art, the present invention has following beneficial effect:
(1) Emission in Cubic Y
2o
3the visible Fig. 1 of crystalline structure figure, a Y
2o
3y in unit cell
3+there is C in case
2and C
3itwo kinds of different case environment, Mo&4&ssbauer spectrum proves, trivalent rare earth ions does not have refusal, therefore Er on these two cases
3+with La
3+the probability occupying these two kinds of cases is consistent.Due to Er
3+(
r er 3+=0.088nm) and Y
3+(
r y 3+=0.089nm) ionic radius is suitable, therefore Er
3+displacement Y
3+to Y
2o
3lattice does not affect.And La
3+(
r la 3+=0.103nm) ionic radius is greater than Y
3+ionic radius, therefore when the present invention introduces La
3+after, La
3+displacement Y
3+case, although now can not Y be changed
2o
3the macrostructure of crystal, but can Y be caused
2o
3matrix local lattice expands, thus reduces Er
3+the symmetry of local crystal field around.This Er
3+around the increase of local environment asymmetry, will improve Er
3+ion 4
fthe possibility of shell transition between the energy levels, makes Er
3+oscillator strength
fincrease, Er
3+ground state absorption cross section increase corresponding to uptake rate, therefore can significantly improve Er simultaneously
3+green Up-conversion emission and near infrared light intensity.
(2) the low temperature micro-gel flooding of the present invention's employing, sol-gel method is effectively combined with combustion method, utilize the complexing function that glycine, citric acid, urea etc. have, the atomic level Homogeneous phase mixing between each composition is ensure that by sol-gel process, make use of again the redox reaction of reaction system self, make wet gel under lesser temps (being less than 400 DEG C), reaction can be completed in several minutes, more at moderate temperatures the short period of time calcining after can obtain nanoscale powder.Whole preparation process technique is simple, safety, production temperature are lower, saves the energy.
(3) luminescent material powder that preparation method of the present invention obtains belongs to nano level, crystallization degree is high, crystal formation is complete, luminescent properties is excellent, and it is chemical stability and Heat stability is good, nontoxic, radiationless, belonging to environmental type luminescent material, is the desired illumination material being applied in the fields such as display, temperature sensor, biomarker, medical monitoring, high-precision measurement.
Accompanying drawing explanation
Fig. 1: be Emission in Cubic Y
2o
3crystalline structure figure.
Fig. 2: (the Er prepared for embodiment 1 and comparative example 1
0.02y
0.88la
0.1)
2o
3with (Er
0.02y
0.98)
2o
3the XRD figure spectrum of nano luminescent material after 1200 DEG C of calcinings, illustration is wherein the enlarged view of (222) diffraction peak.
Fig. 3 (a): (Er prepared for embodiment 1 and comparative example 1
0.02y
0.88la
0.1)
2o
3with (Er
0.02y
0.98)
2o
3the green Up-conversion emission spectrum of sample under 980nm laser diode excites.
Fig. 3 (b): (Er prepared for embodiment 1 and comparative example 1
0.02y
0.88la
0.1)
2o
3with (Er
0.02y
0.98)
2o
3the Near-infrared luminescence of sample under 980nm laser diode excites.
Fig. 4 (a): (Er prepared for embodiment 2 and comparative example 2
0.05y
0.87la
0.08)
2o
3with (Er
0.05y
0.95)
2o
3the green Up-conversion emission spectrum of sample under 980nm laser diode excites.
Fig. 4 (b): (Er prepared for embodiment 2 and comparative example 2
0.05y
0.87la
0.08)
2o
3with (Er
0.05y
0.95)
2o
3the Near-infrared luminescence of sample under 980nm laser diode excites.
Fig. 5 (a): (Er prepared for embodiment 3 and comparative example 3
0.01y
0.89la
0.1)
2o
3with (Er
0.01y
0.99)
2o
3the green Up-conversion emission spectrum of sample under 980nm laser diode excites.
Fig. 5 (b): (Er prepared for embodiment 3 and comparative example 3
0.01y
0.89la
0.1)
2o
3with (Er
0.01y
0.99)
2o
3the Near-infrared luminescence of sample under 980nm laser diode excites.
Fig. 6 (a): (Er prepared for embodiment 4 and comparative example 4
0.04y
0.87la
0.09)
2o
3with (Er
0.04y
0.96)
2o
3the green Up-conversion emission spectrum of sample under 980nm laser diode excites.
Fig. 6 (b): (Er prepared for embodiment 4 and comparative example 4
0.04y
0.87la
0.09)
2o
3with (Er
0.04y
0.96)
2o
3the Near-infrared luminescence of sample under 980nm laser diode excites.
Embodiment
Various preferred embodiment of the present invention is described below in detail.But the present invention is not limited to these concrete preferred embodiments.
Embodiment 1:(Er
0.02y
0.88la
0.1)
2o
3preparation
Concentration is adopted to be the Er (NO of 0.5mol/L
3)
3, Y (NO
3)
3with La (NO
3)
3solution is raw material, by chemical formula (Er
0.02y
0.88la
0.1)
2o
3accurately measure 4 milliliters of Er (NO
3)
3solution, 176 milliliters of Y (NO
3)
3solution and 20 milliliters of La (NO
3)
3solution, by above-mentioned solution mixing and stirring; Add incendiary material Solid Glycine again, Er (NO
3)
3, Y (NO
3)
3with La (NO
3)
3mole total amount and the ratio of molar weight of Solid Glycine be 1:2; Magnetic stirring apparatus makes Solid Glycine dissolve completely in 80 DEG C of stirrings, forms transparent mixing solutions.
Then, mixing solutions is placed in the constant temperature oven heat drying being preheating to 120 DEG C.After solution transition is transparent wet gel, loaded by gel in corundum crucible, be transferred in the retort furnace of 300 DEG C, after insulation there is self-propagating combustion phenomenon in gel, and reaction terminates the fluffy white presoma of rear acquisition.
Will presoma grind after transfer in sintering oven, with after the ramp to 1200 of 10 DEG C/min DEG C, calcine 1 hour, take out after furnace cooling, grind gently, obtain white phosphor (Er
0.02y
0.88la
0.1)
2o
3.
Comparative example 1: do not adulterate La
3+(Er
0.02y
0.98)
2o
3preparation
Concentration is adopted to be the Er (NO of 0.5mol/L during batching
3)
3with Y (NO
3)
3solution is raw material, accurately measures 4 milliliters of Er (NO
3)
3solution and 196 milliliters of Y (NO
3)
3solution, by above-mentioned solution mixing and stirring; Add incendiary material Solid Glycine again, Er (NO
3)
3with Y (NO
3)
3mole total amount and the ratio of molar weight of Solid Glycine be 1:2, magnetic stirring apparatus makes Solid Glycine dissolve completely in 80 DEG C of stirrings, forms transparent mixing solutions.Subsequent process steps and parameter are identical with embodiment 1.
As shown in Figure 2, (Er
0.02y
0.88la
0.1)
2o
3with (Er
0.02y
0.98)
2o
3each diffraction peak and the Emission in Cubic Y of sample
2o
3diffraction peak corresponding (PDF card No.65-3178), illustrate and all define single phase cubic Y
2o
3, there is no dephasign.Compared to (Er
0.02y
0.98)
2o
3, (Er
0.02y
0.88la
0.1)
2o
3diffraction peak toward low angle direction skew, correspond to Y
2o
3the spacing of crystal increases.After least square fitting diffraction peak, can be calculated prepared (Er
0.02y
0.98)
2o
3with (Er
0.02y
0.88la
0.1)
2o
3powder lattice parameter is respectively 1.0603nm and 1.0678nm, illustrates and works as La
3+displacement Y
3+case after, Y
2o
3matrix generation lattice dilatation.According to Scherrer formula, can be calculated (Er
0.02y
0.98)
2o
3, (Er
0.02y
0.88la
0.1)
2o
3the median size of powder is respectively 36nm, 32nm.
(Er
0.02y
0.98)
2o
3(Er
0.02y
0.88la
0.1)
2o
3the green Up-conversion emission spectrum of powder under 980nm laser diode excites is as shown in Fig. 3 (a).From Fig. 3 (a), both green glow bands are positioned at 516 ~ 570nm (highest peak is positioned at 562nm).And under 980nm excites, the near infrared spectrum of bi-material is shown in Fig. 3 (b), visible, both all have multiple emission peak in 1450 ~ 1650nm scope, and wherein highest peak is positioned at 1530nm.Contrast (Er
0.02y
0.98)
2o
3with (Er
0.02y
0.88la
0.1)
2o
3be not difficult to find out, when other conditions are identical, La
3+after doping, the emission peak positions of material does not change, but its green Up-conversion emission intensity and 1.5 ~ 1.6 mu m waveband emissive porwers are significantly increased.
Embodiment 2:(Er
0.05y
0.87la
0.08)
2o
3preparation
Concentration is adopted to be the Er (NO of 0.5mol/L
3)
3, Y (NO
3)
3with La (NO
3)
3solution is raw material, by chemical formula (Er
0.05y
0.87la
0.08)
2o
3accurately measure 10 milliliters of Er (NO
3)
3solution, 174 milliliters of Y (NO
3)
3solution and 16 milliliters of La (NO
3)
3solution, by above-mentioned solution mixing and stirring; Add incendiary material Solid Glycine, Er (NO
3)
3, Y (NO
3)
3with La (NO
3)
3mole total amount and the ratio of molar weight of Solid Glycine be 1:4, magnetic stirring apparatus makes Solid Glycine dissolve completely in 70 DEG C of stirrings, forms transparent solution.
Then, mixing solutions is placed in the constant temperature oven heat drying being preheating to 100 DEG C, after solution transition is transparent wet gel, gel is loaded in corundum crucible, be transferred in the retort furnace of 400 DEG C, after insulation there is self-propagating combustion phenomenon in gel, and reaction terminates the fluffy white presoma of rear acquisition.
Will presoma grind after transfer in sintering oven, with after the ramp to 1100 of 15 DEG C/min DEG C, calcine 2 hours, takes out after furnace cooling, grind gently, acquisition (Er
0.05y
0.87la
0.08)
2o
3luminescent material.
Comparative example 2:(Er
0.05y
0.95)
2o
3preparation
Concentration is adopted to be the Er (NO of 0.5mol/L
3)
3with Y (NO
3)
3solution is raw material, accurately measures 10 milliliters of Er (NO
3)
3solution and 190 milliliters of Y (NO
3)
3solution, by above-mentioned solution mixing and stirring; Add incendiary material Solid Glycine, Er (NO
3)
3with Y (NO
3)
3mole total amount and the ratio of molar weight of Solid Glycine be 1:4, magnetic stirring apparatus makes Solid Glycine dissolve completely in 70 DEG C of stirrings, forms transparent solution.Subsequent process steps and parameter are identical with embodiment 2, prepare the La that undopes
3+(Er
0.05y
0.95)
2o
3.
(Er
0.05y
0.95)
2o
3(Er
0.05y
0.87la
0.08)
2o
3the XRD figure spectrum of powder is basically identical with embodiment 1 feature, and both are respectively 44nm and 40nm at median size.Fig. 4 (a) shows (Er
0.05y
0.95)
2o
3with (Er
0.05y
0.87la
0.08)
2o
3the green Up-conversion emission spectrum of powder under 980nm laser diode excites.From Fig. 4 (a), both have multiple emission peak at 516 ~ 570nm place, and wherein highest peak is all positioned at 562nm; Meanwhile, La
3+doped with the increase helping green emission intensity.Fig. 4 (b) shows the near infrared spectrum exciting lower bi-material at 980nm, and both main peak peak positions are all positioned at 1530nm as seen, same, La
3+after doping, the near infrared emission intensity of material significantly strengthens.As can be seen here, even if at Er
3+in heavily doped situation, La
3+doping also can improve upper conversion green intensity and 1.5 ~ 1.6 mu m waveband emissive porwers of sample.
Embodiment 3:(Er
0.01y
0.89la
0.1)
2o
3preparation
Concentration is adopted to be the Er (NO of 0.5mol/L
3)
3, Y (NO
3)
3with La (NO
3)
3solution is raw material, by chemical formula (Er
0.01y
0.89la
0.1)
2o
3accurately measure 2 milliliters of Er (NO
3)
3solution, 178 milliliters of Y (NO
3)
3solution and 20 milliliters of La (NO
3)
3solution, by above-mentioned solution mixing and stirring; Add incendiary material solid citric acid, Er (NO
3)
3, Y (NO
3)
3with La (NO
3)
3mole total amount and the ratio of molar weight of solid citric acid be 1:2, magnetic stirring apparatus forms transparent solution after 60 DEG C of stirrings make solid citric acid dissolve completely.
Then, mixing solutions is placed in the constant temperature oven heat drying being preheating to 80 DEG C, after solution transition is transparent wet gel, gel is loaded in corundum crucible, be transferred in the retort furnace of 300 DEG C, after insulation there is self-propagating combustion phenomenon in gel, and reaction terminates the fluffy white presoma of rear acquisition.
Transfer in sintering oven after presoma is ground, with the ramp to 900 DEG C of 20 DEG C/min, calcine 3 hours, take out after furnace cooling, grind gently, obtain (Er
0.01y
0.89la
0.1)
2o
3luminescent material.
Comparative example 3:(Er
0.01y
0.99)
2o
3preparation
Concentration is adopted to be the Er (NO of 0.5mol/L
3)
3with Y (NO
3)
3solution is raw material, accurately measures 2 milliliters of Er (NO
3)
3solution and 198 milliliters of Y (NO
3)
3solution, by above-mentioned solution mixing and stirring; Add incendiary material solid citric acid, Er (NO
3)
3with Y (NO
3)
3mole total amount and the ratio of molar weight of solid citric acid be 1:2, magnetic stirring apparatus makes solid citric acid dissolve completely in 60 DEG C of stirrings, forms transparent solution.Subsequent process steps and parameter are identical with embodiment 3, prepare the La that undopes
3+(Er
0.01y
0.99)
2o
3.
(Er
0.01y
0.99)
2o
3(Er
0.01y
0.89la
0.1)
2o
3the XRD figure spectrum of powder is basically identical with embodiment 1 feature, and both are respectively 35nm and 28nm at median size.Fig. 5 (a) and Fig. 5 (b) respectively illustrates (Er
0.01y
0.99)
2o
3with (Er
0.01y
0.89la
0.1)
2o
3conversion and near infrared spectroscopy in the green of powder under 980nm laser diode excites, visible (Er
0.01y
0.89la
0.1)
2o
3in the green of powder, conversion and near infrared emission intensity are all higher than (Er
0.01y
0.99)
2o
3powder.
Embodiment 4:(Er
0.04y
0.87la
0.09)
2o
3preparation
Concentration is adopted to be the Er (NO of 0.5mol/L
3)
3, Y (NO
3)
3with La (NO
3)
3solution is raw material, by chemical formula (Er
0.04y
0.87la
0.09)
2o
3accurately measure 8 milliliters of Er (NO
3)
3solution, 174 milliliters of Y (NO
3)
3solution and 18 milliliters of La (NO
3)
3solution, by above-mentioned solution mixing and stirring; Add incendiary material solid urea, Er (NO
3)
3, Y (NO
3)
3with La (NO
3)
3mole total amount and the ratio of molar weight of solid urea be 1:4, magnetic stirring apparatus makes solid urea dissolve completely in 60 DEG C of stirrings, forms transparent solution.
Then, mixing solutions is placed in the constant temperature oven heat drying being preheating to 80 DEG C, after solution transition is transparent wet gel, gel is loaded in corundum crucible, be transferred in the retort furnace of 400 DEG C, after insulation there is self-propagating combustion phenomenon in gel, and reaction terminates the fluffy white presoma of rear acquisition.
Will presoma grind after transfer in sintering oven, with after the ramp to 1200 of 15 DEG C/min DEG C, calcine 2 hours, takes out after furnace cooling, grind gently, acquisition (Er
0.04y
0.87la
0.09)
2o
3luminescent material.
Comparative example 4:(Er
0.04y
0.96)
2o
3preparation
Concentration is adopted to be the Er (NO of 0.5mol/L
3)
3with Y (NO
3)
3solution is raw material, accurately measures 8 milliliters of Er (NO
3)
3solution and 192 milliliters of Y (NO
3)
3solution, by above-mentioned solution mixing and stirring; Add incendiary material solid urea, Er (NO
3)
3with Y (NO
3)
3mole total amount and the ratio of molar weight of solid urea be 1:4, magnetic stirring apparatus makes solid urea dissolve completely in 60 DEG C of stirrings, forms transparent solution.Subsequent process steps and parameter are identical with embodiment 4, prepare the La that undopes
3+(Er
0.04y
0.96)
2o
3.
(Er
0.04y
0.96)
2o
3(Er
0.04y
0.87la
0.09)
2o
3the XRD figure spectrum of powder is basically identical with embodiment 1 feature, and both are respectively 26nm and 20nm at median size.Fig. 6 (a) and Fig. 6 (b) respectively illustrates (Er
0.04y
0.96)
2o
3with (Er
0.04y
0.87la
0.09)
2o
3conversion and near infrared spectroscopy in the green of powder under 980nm laser diode excites, visible (Er
0.04y
0.87la
0.09)
2o
3in the green of powder, conversion and near infrared emission intensity are all higher than (Er
0.04y
0.96)
2o
3powder.
Claims (5)
1. an Er ions lanthanum yttrium oxide luminescent material, is characterized in that: the chemical expression of described luminescent material is (Er
xy
1-x-yla
y)
2o
3, wherein, 0<x≤0.05,0.08≤y≤0.1.
2. a preparation method for the Er ions lanthanum yttrium oxide luminescent material of claim 1, is characterized in that, comprise the following steps:
(1) with the Er (NO of analytical pure purity
3)
3, Y (NO
3)
3, La (NO
3)
3solution as raw material, by chemical formula (Er
xy
1-x-yla
y)
2o
3stoichiometric ratio mixing after stir, obtain mixing solutions;
(2) in described mixing solutions, incendiary material is added, Er (NO
3)
3, Y (NO
3)
3with La (NO
3)
3total amount and the mol ratio of incendiary material be 1:2 ~ 4, carry out stirring and incendiary material being dissolved completely at 60 ~ 80 DEG C; Then solution is placed in the constant temperature oven heat drying being preheating to 80 ~ 120 DEG C, obtains transparent wet gel;
(3) described transparent wet gel is placed in the retort furnace that furnace temperature is 300 ~ 400 DEG C, is incubated under air atmosphere, wet gel generation spontaneous combustion, obtains presoma after combustion reactions terminates;
(4) by after described presoma grinding evenly, put into the flat-temperature zone of high temperature sintering furnace, calcine 1 ~ 3 hour at 900 ~ 1200 DEG C, obtain Er ions lanthanum yttrium oxide luminescent material.
3. preparation method according to claim 2, is characterized in that: in described step (4), rise to calcining temperature with the temperature rise rate of 10 ~ 20 DEG C/min.
4. the preparation method according to Claims 2 or 3, is characterized in that: the median size of the Er ions lanthanum yttrium oxide luminescent material obtained is 20 ~ 40 nanometers.
5. the preparation method according to any one of claim 2 to 4, is characterized in that: described incendiary material is glycine, urea or citric acid.
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| CN111057544A (en) * | 2019-12-04 | 2020-04-24 | 西安交通大学 | Lamellar bismuth-doped yttrium oxide fluorescent powder and preparation method and application thereof |
| CN112521148A (en) * | 2020-12-21 | 2021-03-19 | 中国计量大学上虞高等研究院有限公司 | Erbium/yttrium-doped zirconia transparent ceramic and preparation method and application thereof |
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