CN104861972B - A kind of Er3+and Yb3+double-doped VO2up-conversion luminescent material - Google Patents
A kind of Er3+and Yb3+double-doped VO2up-conversion luminescent material Download PDFInfo
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Abstract
A kind of Er3+And Yb3+Double-doped VO2Up-conversion luminescent material, it relates to a kind of up-conversion luminescent material.The invention aims to solve existing solaode and can not utilize infrared light, cause the problem that the conversion ratio of solaode is low.Method: by Er2O3And Yb2O3Join in the nitric acid that mass fraction is 65%～68%, add V2O5And oxalic acid, then carry out hydro-thermal reaction, obtain dried reactant；Again dried reactant is calcined, obtain Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.Five, Er prepared by the present invention3+And Yb3+Double-doped VO2Up-conversion luminescent material is nanometer sheet, and the thickness of sheet is 20nm～50nm, is a kind of nano material.The present invention can obtain a kind of Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of up-conversion luminescent material.
Background technology
In the case of Fossil fuel reduces increasingly, solar energy, as a kind of regenerative resource, is the environment protection clean energy truly, the zero-emission that achieve greenhouse gases the most friendly to environment.Solaode is the device directly luminous energy being changed into electric energy by photoelectric effect or Photochemical effects.Although the advantage of solaode has a lot, such as: faster, life-span length more than 5 times, charging temperature scope is wider in charging.But the photoelectric transformation efficiency of solaode is low, within 1883, first piece of solar cell is successfully prepared by Charles Fritts, the efficiency of only 1%, the photoelectric material conversion efficiency of current mono-crystalline silicon solar the highest the most just 24%.For a solaode, causing the reason mainly solaode that its conversion efficiency is low mainly to utilize the light that wavelength is 400nm-790nm, i.e. utilize visible ray, about accounted for 85%, for infrared light, conversion efficiency is the lowest.So how could people improve the utilization ratio of solaode in research.Being found by research, can pass through doping with rare-earth ions, in utilization, conversion is converted into visible ray infrared light, thus increases the utilization ratio of solaode.
VO2As one well on change host material, the characteristic that vanadium dioxide is had allows it have a wide range of applications potentiality in optical device, electronic installation and optoelectronic device.Doping Er3+/Yb3The VO of ion2, under the near-infrared laser of 980nm, VO2Can send the strongest green glow, its wavelength, at 515nm～560nm, is positioned at solaode absorption bands, and upper switch technology converts infrared light to visible ray, thus improves the conversion efficiency of solaode.
Summary of the invention
The invention aims to solve existing solaode and can not utilize infrared light, cause the problem that the conversion ratio of solaode is low, and a kind of Er is provided3+And Yb3+Double-doped VO2Up-conversion luminescent material.
A kind of Er3+And Yb3+Double-doped VO2Up-conversion luminescent material is prepared according to the following steps:
One, by Er2O3And Yb2O3Join in the nitric acid that mass fraction is 65%～68%, then on the universal electric furnace that power is 500W～1000W, heat 10min～20min, add distilled water, obtain mixed solution A；
Er described in step one2O3With Yb2O3The amount of material than for 2:(4～10)；
Er described in step one2O3The volume ratio of the nitric acid that amount and mass fraction are 65%～68% of material be 2mol:(2mL～10mL)；
Mass fraction described in step one is the nitric acid of 65%～68% and the volume ratio of distilled water is (2～10): 5；
Two, by V2O5With in dissolving oxalic acid to mixed solution A, add distilled water, then low whipping speed is stirring 2h～4h under 400r/min～600r/min, obtains black-and-blue mixed solution B；
V described in step 22O5It is 1:(2～6 with the mol ratio of oxalic acid)；
V described in step 22O5The amount of material and the volume ratio of mixed solution A be 1mol:(5mL～8mL)；
The volume of the distilled water described in step 2 and the volume ratio of mixed solution A are 15:(5～8)；
Three, mixed solution B is joined in reactor, then at temperature is 160 DEG C～200 DEG C, reacts 12h～48h, obtain reactant；Use distilled water and ethanol respectively reactant to be cleaned 3 times～5 times, then at temperature is 60 DEG C～80 DEG C, is dried 12h～16h, obtain dried reactant；
Four, dried reactant is joined in tube furnace, then sinter 1h～2h at nitrogen atmosphere and sintering temperature 350 DEG C～400 DEG C, then cool to room temperature with the furnace, obtain Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.
The principle of the present invention:
Sunlight by about 50% visible region (400～760nm) and infrared light the district (> 760nm of about 43%), ultra-violet (UV) band is little, only accounts for about 7%.The reason that solaode transformation efficiency is low at present is that it mainly absorbs visible ray, can account for 85%, and the efficiency utilizing infrared light is the lowest.By doping with rare-earth ions, under the exciting of 980nm laser, visible ray can be converted infrared light to by upper conversion, thus improve the conversion efficiency of solaode；Er3+Doping is capable of the transmitting of conversion green glow, Er3+Ion becomes the rare earth ion pursued by research worker due to its abundant energy level and higher quenching concentration；Yb3+Ion has wide absorption bands and big absorption cross-section, and Yb due to its simple level structure near 980nm wavelength3+The transmitting of ion and Er3+The absorption of ion spectrally also exists overlapping significantly so that Yb3+Ion is to Er3+Interionic has higher energy transfer efficiency, thus is greatly improved Er3+The absorption of ion pair 980nm exciting light and strengthen Er3+The up-conversion fluorescence of ion green glow is launched.
Advantages of the present invention:
One, the present invention utilizes hydro-thermal method to prepare Er3+And Yb3+Double-doped VO2The experimental raw of nano material is cheap and is easy to get, and experiment condition is the gentleest, and experimental procedure is less；
Two, Er prepared by the present invention3+And Yb3+Double-doped VO2Nano material is under the exciting of 980nm laser, it is possible to infrared light is converted into monochromatic visible green, and intensity is the strongest；
Three, Er prepared by the present invention3+And Yb3+Double-doped VO2Nano material is under the exciting of 980nm laser, it is possible to convert infrared light to visible ray, improves the conversion efficiency of solaode；
Four, Er prepared by the present invention3+And Yb3+Double-doped VO2Up-conversion luminescent material has light emission at 530nm and 550nm；Light emission at 530nm and 550nm is the green emission of visual field, corresponding to Er3+Ion2H11/2/4S3/2→4I15/2Energy level transition；
Five, Er prepared by the present invention3+And Yb3+Double-doped VO2Up-conversion luminescent material is nanometer sheet, and the thickness of sheet is 20nm～50nm, is a kind of nano material.
Accompanying drawing explanation
Fig. 1 is the Er of embodiment one preparation3+And Yb3+Double-doped VO2The XRD spectra of up-conversion luminescent material；
Fig. 2 is up-conversion luminescence spectrogram, and in Fig. 2,1 is the Er of embodiment one preparation3+And Yb3+Double-doped VO2Up-conversion luminescent material luminosity curve, 2 be implement two preparation Er3+And Yb3+Double-doped VO2Up-conversion luminescent material luminosity curve, 3 be embodiment three preparation Er3+And Yb3+Double-doped VO2Up-conversion luminescent material luminosity curve；
Fig. 3 is the Er implementing three preparations3+And Yb3+Double-doped VO2Amplify the SEM figure of 60000 times；
Fig. 4 is the Er implementing three preparations3+And Yb3+Double-doped VO2Amplify the SEM figure of 100000 times.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of Er3+And Yb3+Double-doped VO2Up-conversion luminescent material is prepared according to the following steps:
A kind of Er3+And Yb3+Double-doped VO2Up-conversion luminescent material is prepared according to the following steps:
One, by Er2O3And Yb2O3Join in the nitric acid that mass fraction is 65%～68%, then on the universal electric furnace that power is 500W～1000W, heat 10min～20min, add distilled water, obtain mixed solution A；
Er described in step one2O3With Yb2O3The amount of material than for 2:(4～10)；
Er described in step one2O3The volume ratio of the nitric acid that amount and mass fraction are 65%～68% of material be 2mol:(2mL～10mL)；
Mass fraction described in step one is the nitric acid of 65%～68% and the volume ratio of distilled water is (2～10): 5；
Two, by V2O5With in dissolving oxalic acid to mixed solution A, add distilled water, then low whipping speed is stirring 2h～4h under 400r/min～600r/min, obtains black-and-blue mixed solution B；
V described in step 22O5It is 1:(2～6 with the mol ratio of oxalic acid)；
V described in step 22O5The amount of material and the volume ratio of mixed solution A be 1mol:(5mL～8mL)；
The volume of the distilled water described in step 2 and the volume ratio of mixed solution A are 15:(5～8)；
Three, mixed solution B is joined in reactor, then at temperature is 160 DEG C～200 DEG C, reacts 12h～48h, obtain reactant；Use distilled water and ethanol respectively reactant to be cleaned 3 times～5 times, then at temperature is 60 DEG C～80 DEG C, is dried 12h～16h, obtain dried reactant；
Four, dried reactant is joined in tube furnace, then sinter 1h～2h at nitrogen atmosphere and sintering temperature 350 DEG C～400 DEG C, then cool to room temperature with the furnace, obtain Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.
Er prepared by present embodiment3+And Yb3+Double-doped VO2Up-conversion luminescent material is under the exciting of 980nm laser, it is possible to infrared light is converted into monochromatic visible green, under the exciting of 980nm laser, it is possible to convert infrared light to visible ray；
Er prepared by present embodiment3+And Yb3+Double-doped VO2The wave-length coverage of up-conversion luminescent material is 520nm～540nm.
Purpose in present embodiment step one is by Er2O3And Yb2O3It is dissolved in nitric acid, thus obtains Er3+And Yb3+；
Purpose in present embodiment step 2 is as reducing agent using oxalic acid, by V5+It is reduced to V4+, obtain presoma VOC2O4；
Purpose in present embodiment step 3 is to utilize water heat transfer target product；
Purpose in present embodiment step 4 is to utilize sintering to remove moisture remaining in sample, makes Up-conversion Intensity strengthen.
The advantage of present embodiment:
One, present embodiment utilizes hydro-thermal method to prepare Er3+And Yb3+Double-doped VO2The experimental raw of nano material is cheap and is easy to get, and experiment condition is the gentleest, and experimental procedure is less；
Two, Er prepared by present embodiment3+And Yb3+Double-doped VO2Nano material is under the exciting of 980nm laser, it is possible to infrared light is converted into monochromatic visible green, and intensity is the strongest；
Three, Er prepared by present embodiment3+And Yb3+Double-doped VO2Nano material is under the exciting of 980nm laser, it is possible to convert infrared light to visible ray, improves the conversion efficiency of solaode；
Four, Er prepared by present embodiment3+And Yb3+Double-doped VO2Up-conversion luminescent material has light emission at 530nm and 550nm；Light emission at 530nm and 550nm is the green emission of visual field, corresponding to Er3+Ion2H11/2/4S3/2→4I15/2Energy level transition；
Five, Er prepared by present embodiment3+And Yb3+Double-doped VO2Up-conversion luminescent material is nanometer sheet, and the thickness of sheet is 20nm～50nm, is a kind of nano material.
Detailed description of the invention two: present embodiment with detailed description of the invention one difference is: the Er described in step one2O3With Yb2O3The amount of material than for 2:(4～7).Other steps are identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment with one of detailed description of the invention one or two difference is: the Er described in step one2O3With Yb2O3The amount of material than for 2:(7～10).Other steps are identical with detailed description of the invention one or two.
Detailed description of the invention four: present embodiment with one of detailed description of the invention one to three difference is: the Er described in step one2O3The volume ratio of the nitric acid that amount and mass fraction are 65%～68% of material be 2mol:(2mL～6mL).Other steps are identical with detailed description of the invention one to three.
Detailed description of the invention five: present embodiment with one of detailed description of the invention one to four difference is: the Er described in step one2O3The volume ratio of the nitric acid that amount and mass fraction are 65%～68% of material be 2mol:(6mL～10mL).Other steps are identical with detailed description of the invention one to four.
Detailed description of the invention six: present embodiment with one of detailed description of the invention one to five difference is: the V described in step 22O5It is 1:(2～4 with the mol ratio of oxalic acid).Other steps are identical with detailed description of the invention one to five.
Detailed description of the invention seven: present embodiment with one of detailed description of the invention one to six difference is: the V described in step 22O5It is 1:(4～6 with the mol ratio of oxalic acid).Other steps are identical with detailed description of the invention one to six.
Detailed description of the invention eight: present embodiment with one of detailed description of the invention one to seven difference is: the V described in step 22O5The amount of material and the volume ratio of mixed solution A be 1mol:5mL.Other steps are identical with detailed description of the invention one to seven.
Detailed description of the invention nine: present embodiment with one of detailed description of the invention one to eight difference is: joined in tube furnace by dried reactant in step 4, then sinter 2h at nitrogen atmosphere and sintering temperature 350 DEG C, then cool to room temperature with the furnace, obtain Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.Other steps are identical with detailed description of the invention one to eight.
Detailed description of the invention ten: present embodiment with one of detailed description of the invention one to nine difference is: joined in tube furnace by dried reactant in step 4, then sinter 1h at nitrogen atmosphere and sintering temperature 400 DEG C, then cool to room temperature with the furnace, obtain Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.Other steps are identical with detailed description of the invention one to nine.
Employing following example checking beneficial effects of the present invention:
Embodiment one: a kind of Er3+And Yb3+Double-doped VO2Up-conversion luminescent material is prepared according to the following steps:
One, by Er2O3And Yb2O3Join in the nitric acid that mass fraction is 65%, then on the universal electric furnace that power is 1000W, heat 10min, add distilled water, obtain mixed solution A；
Er described in step one2O3With Yb2O3The amount of material than for 2:4；
Er described in step one2O3The volume ratio of the nitric acid that amount and mass fraction are 65% of material be 2mol:4mL；
Mass fraction described in step one is the nitric acid of 65% and the volume ratio of distilled water is 4:5；
Two, by V2O5With in dissolving oxalic acid to mixed solution A, add distilled water, then low whipping speed is stirring 3h under 400r/min, obtains black-and-blue mixed solution B；
V described in step 22O5It is 1:2 with the mol ratio of oxalic acid；
V described in step 22O5The amount of material and the volume ratio of mixed solution A be 1mol:5mL；
The volume of the distilled water described in step 2 and the volume ratio of mixed solution A are 15:5；
Three, mixed solution B is joined in reactor, then at temperature is 180 DEG C, reacts 24h, obtain reactant；Use distilled water and ethanol respectively reactant to be cleaned 4 times, then at temperature is 60 DEG C, is dried 12h, obtain dried reactant；
Four, dried reactant is joined in tube furnace, then sinter 2h at nitrogen atmosphere and sintering temperature 400 DEG C, then cool to room temperature with the furnace, obtain Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.
Embodiment two: a kind of Er3+And Yb3+Double-doped VO2Up-conversion luminescent material is prepared according to the following steps:
One, by Er2O3And Yb2O3Joining in the nitric acid that mass fraction is 65%, then heat on universal electric furnace, power is 1000W, heats 15min, adds distilled water, obtain mixed solution A；
Er described in step one2O3With Yb2O3The amount of material than for 2:6；
Er described in step one2O3The volume ratio of the nitric acid that amount and mass fraction are 65% of material be 2mol:6mL；
Mass fraction described in step one is the nitric acid of 65% and the volume ratio of distilled water is 4:5；
Two, by V2O5With in dissolving oxalic acid to mixed solution A, add distilled water, then low whipping speed is stirring 3h under 400r/min, obtains black-and-blue mixed solution B；
V described in step 22O5It is 1:2 with the mol ratio of oxalic acid；
V described in step 22O5The amount of material and the volume ratio of mixed solution A be 1mol:5mL；
The volume of the distilled water described in step 2 and the volume ratio of mixed solution A are 15:5；
Three, mixed solution B is joined in reactor, then at temperature is 180 DEG C, reacts 24h, obtain reactant；Use distilled water and ethanol respectively reactant to be cleaned 4 times, then at temperature is 60 DEG C, is dried 12h, obtain dried reactant；
Four, dried reactant is joined in tube furnace, then sinter 2h at nitrogen atmosphere and sintering temperature 400 DEG C, then cool to room temperature with the furnace, obtain Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.
Embodiment three: a kind of Er3+And Yb3+Double-doped VO2Up-conversion luminescent material is prepared according to the following steps:
One, by Er2O3And Yb2O3Joining in the nitric acid that mass fraction is 65%, then heat on universal electric furnace, power is 1000W, heats 20min, adds distilled water, obtain mixed solution A；
Er described in step one2O3With Yb2O3The amount of material than for 2:8；
Er described in step one2O3The volume ratio of the nitric acid that amount and mass fraction are 65% of material be 2mol:8mL；
Mass fraction described in step one is the nitric acid of 65% and the volume ratio of distilled water is 4:5；
Two, by V2O5With in dissolving oxalic acid to mixed solution A, add distilled water, then low whipping speed is stirring 3h under 400r/min, obtains black-and-blue mixed solution B；
V described in step 22O5It is 1:2 with the mol ratio of oxalic acid；
V described in step 22O5The amount of material and the volume ratio of mixed solution A be 1mol:5mL；
The volume of the distilled water described in step 2 and the volume ratio of mixed solution A are 15:5；
Three, mixed solution B is joined in reactor, then at temperature is 180 DEG C, reacts 24h, obtain reactant；Use distilled water and ethanol respectively reactant to be cleaned 4 times, then at temperature is 60 DEG C, is dried 12h, obtain dried reactant；
Four, dried reactant is joined in tube furnace, then sinter 2h at nitrogen atmosphere and sintering temperature 400 DEG C, then cool to room temperature with the furnace, obtain Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.
Fig. 1 is the Er of embodiment one preparation3+And Yb3+Double-doped VO2The XRD spectra of up-conversion luminescent material；It will be seen from figure 1 that by contrasting with normal data, find that each peak all coincide fine, do not find and Er3+、Yb3+The appearance of the impurity peaks that ion is relevant, and peak shape is the most sharp-pointed；Can draw accordingly and prepare pure Er3+/Yb3+Double-doped VO2。
Using optical maser wavelength is that the diode of 980nm is as excitation source, exciting power can be adjusted to: 100mW～900mW, spectrogrph model is Zolix-SBP300, step-length is 1nm, spectrum test scope is 400nm～900nm, photomultiplier tube model is CR131, the Er to the preparation of embodiment one, embodiment two and embodiment three3+And Yb3+Double-doped VO2Up-conversion luminescent material is tested, as shown in Figure 2.
Fig. 2 is up-conversion luminescence spectrogram, and in Fig. 2,1 is the Er of embodiment one preparation3+And Yb3+Double-doped VO2The luminosity curve of up-conversion luminescent material, 2 is the Er implementing two preparations3+And Yb3+Double-doped VO2The luminosity curve of up-conversion luminescent material, 3 is the Er of embodiment three preparation3+And Yb3+Double-doped VO2The luminosity curve of up-conversion luminescent material；
As can be seen from Figure 2: when at room temperature exciting with the laser instrument that excitation wavelength is 980nm, the Er to same concentrations3+, variable concentrations Yb3+The sample of ion doping, all has light emission at 530nm and 550nm.Light emission at 530nm and 550nm is the green emission of visual field, corresponding to Er3+Ion2H11/2/4S3/2→4I15/2Energy level transition.And along with Yb3+The increase of ion concentration, luminous intensity strengthens the most therewith.
Fig. 3 is the Er implementing three preparations3+And Yb3+Double-doped VO2Amplify the SEM figure of 60000 times；Fig. 4 is the Er implementing three preparations3+And Yb3+Double-doped VO2Amplify the SEM figure of 100000 times；
Er is can be seen that from Fig. 3 and Fig. 43+And Yb3+Double-doped VO2Material is nanometer sheet, and the thickness of sheet is 20nm～50nm.The most one-dimensional it is in nanoscale scope (1-100nm) or the material being made up of them as elementary cell.Er3+And Yb3+Double-doped VO2A kind of nano material.
Claims (10)
1. an Er3+And Yb3+Double-doped VO2Up-conversion luminescent material, its spy is a kind of Er3+And Yb3+Double-doped VO2
Up-conversion luminescent material is prepared according to the following steps:
One, by Er2O3And Yb2O3Join in the nitric acid that mass fraction is 65%～68%, then be 500W～1000W at power
Universal electric furnace on heat 10min～20min, add distilled water, obtain mixed solution A；
Er described in step one2O3With Yb2O3The amount of material than for 2:(4～10)；
Er described in step one2O3Material the nitric acid that amount and mass fraction are 65%～68% volume ratio 2mol:(2mL～
10mL)；
Mass fraction described in step one is the nitric acid of 65%～68% and the volume ratio of distilled water is (2～10): 5；
Two, by V2O5With in dissolving oxalic acid to mixed solution A, add distilled water, then low whipping speed be 400r/min～
Stir 2h～4h under 600r/min, obtain black-and-blue mixed solution B；
V described in step 22O5It is 1:(2～6 with the mol ratio of oxalic acid)；
V described in step 22O5The amount of material and the volume ratio of mixed solution A be 1mol:(5mL～8mL)；
The volume of the distilled water described in step 2 and the volume ratio of mixed solution A are 15:(5～8)；
Three, mixed solution B is joined in reactor, then at temperature is 160 DEG C～200 DEG C, reacts 12h～48h, obtain
Reactant；Use distilled water and ethanol respectively reactant to be cleaned 3 times～5 times, then be dried at temperature is 60 DEG C～80 DEG C
12h～16h, obtains dried reactant；
Four, dried reactant is joined in tube furnace, then at nitrogen atmosphere and 350 DEG C～400 DEG C sintering of sintering temperature
1h～2h, then cool to room temperature with the furnace, obtain Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.
A kind of Er the most according to claim 13+And Yb3+Double-doped VO2Up-conversion luminescent material, its spy is step
Er described in rapid one2O3With Yb2O3The amount of material than for 2:(4～7).
A kind of Er the most according to claim 13+And Yb3+Double-doped VO2Up-conversion luminescent material, its spy is step
Er described in rapid one2O3With Yb2O3The amount of material than for 2:(7～10).
A kind of Er the most according to claim 13+And Yb3+Double-doped VO2Up-conversion luminescent material, its spy is step
Er described in rapid one2O3Volume ratio 2mol:(2mL of the nitric acid that amount and mass fraction are 65%～68% of material～6mL).
A kind of Er the most according to claim 13+And Yb3+Double-doped VO2Up-conversion luminescent material, its spy is step
Er described in rapid one2O3The volume ratio of the nitric acid that amount and mass fraction are 65%～68% of material be 2mol:(6mL～
10mL)。
A kind of Er the most according to claim 13+And Yb3+Double-doped VO2Up-conversion luminescent material, its spy is step
V described in rapid two2O5It is 1:(2～4 with the mol ratio of oxalic acid).
A kind of Er the most according to claim 13+And Yb3+Double-doped VO2Up-conversion luminescent material, its spy is step
V described in rapid two2O5It is 1:(4～6 with the mol ratio of oxalic acid).
A kind of Er the most according to claim 13+And Yb3+Double-doped VO2Up-conversion luminescent material, its spy is step
V described in rapid two2O5The amount of material and the volume ratio of mixed solution A be 1mol:5mL.
A kind of Er the most according to claim 13+And Yb3+Double-doped VO2Up-conversion luminescent material, its spy is step
In rapid four, dried reactant is joined in tube furnace, then at nitrogen atmosphere and sintering temperature 350 DEG C sintering 2h, then with
Stove is cooled to room temperature, obtains Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.
A kind of Er the most according to claim 13+And Yb3+Double-doped VO2Up-conversion luminescent material, its spy is step
In rapid four, dried reactant is joined in tube furnace, then at nitrogen atmosphere and sintering temperature 400 DEG C sintering 1h, then with
Stove is cooled to room temperature, obtains Er3+And Yb3+Double-doped VO2Up-conversion luminescent material.
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| Green and red up conversion emissions of Er3+-Yb3+ Co-doped TiO2 nanocrystals prepared by sol gel method;Qingkun Shang et al;《Journal of Luminescence》;20071217;第128卷;第1211页实验部分 * |
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