CN102191049A - Ytterbium erbium double-doped calcium tungstate polycrystal powder green ray up-conversion material and preparation method thereof - Google Patents
Ytterbium erbium double-doped calcium tungstate polycrystal powder green ray up-conversion material and preparation method thereof Download PDFInfo
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Abstract
The invention provides an ytterbium erbium double-doped calcium tungstate polycrystal powder green ray up-conversion material and a preparation method thereof, and relates to an rare-earth element doped calcium tungstate polycrystal powder green ray up-conversion material and a preparation method thereof. By the ytterbium erbium double-doped calcium tungstate polycrystal powder green ray up-conversion material and the preparation method thereof, the problem that emitted light with high singleness is difficult to obtain when the rare-earth elements are doped in a matrix material is solved. The chemical formula of the ytterbium erbium double-doped calcium tungstate polycrystal powder green ray up-conversion material is Ca0.99-xWO4:Yb0.01/Erx, wherein x is more than or equal to 0.001 and less than or equal to 0.08. The preparation method comprises the following steps of: 1, weighing according to the stoichiometric ratio of the chemical formula; 2, grinding and tabletting; and 3, sintering at a high temperature. The ytterbium erbium double-doped calcium tungstate polycrystal powder green ray up-conversion material can emit bright up-conversion green ray uniformly under the conditions of laser pumping of 980 nm and laser power of 300 mW.
Description
Technical field
The present invention relates to a kind of rare earth doped calcium wolframate polycrystalline powder green glow up-conversion and preparation method thereof.
Background technology
Up-conversion luminescence is called anti-Stokes luminescence again, is meant the phenomenon that two or more lower energy photons is converted to a high-energy photon, up-conversion luminescent material need be in matrix doped with rare-earth elements.The energy absorption capability of rare earth luminescent material is strong, the efficiency of conversion height; Can launch the spectrum from the UV-light to the infrared light, particularly very strong emissive power be arranged at visible region.The physicochemical property of rare earth element are stable, can bear the advantages such as effect of powerful electron beam, energetic ray and strong UV-light, but because the energy level branch of most of rare earth elements is complicated, doped with rare-earth elements in substrate material is difficult to obtain unicity and well launches light.
Summary of the invention
The objective of the invention is in order to solve doped with rare-earth elements in the substrate material, be difficult to obtain the good radiative problem of unicity, and a kind of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion that provides and preparation method thereof.
The chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.001≤x≤0.08 wherein.
Above-mentioned ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.001≤x≤0.08 wherein;
Two, place agate mortar to grind 4 ± 0.5 hours in lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ± 50 ℃, and sintering time is 10 ± 0.5 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion.
Ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of the present invention is made by lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder.
Erbium ion is as the activator of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion among the present invention, and ytterbium ion is as the sensitizing agent of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion, and ytterbium ion can transmit the up-conversion luminescence of energy excitation erbium ion.The present invention is by regulating substrate material (CaWO
4) in the ratio of activator and sensitizing agent, erbium ion and ytterbium ion produce on the cooperative sensitization and change, what obtained the unicity excellence goes up the conversion green emission.
Because calcium wolframate has excellent thermostability and chemical stability, therefore select its substrate material as ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of the present invention.
Ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of the present invention is can send under the 300mW condition to change green glow on bright in 980nm laser pumping, exciting power, and luminous evenly.
The preparation method of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of the present invention is simple, and the accurate control element doping of energy, and its resulting ytterbium erbium codope calcium wolframate polycrystalline powder has high-luminous-efficiency.
Ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of the present invention is changed green emission intensity with Er in wavelength 530nm and 552nm place
3+The corresponding curve of change in concentration as shown in Figure 3.Along with improving constantly of erbium ion concentration, ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion up-conversion emission intensity on wavelength 530nm and 552nm place green strengthens afterwards earlier and weakens, in erbium ion-doped concentration is 0.5% o'clock, and up-conversion emission intensity is the strongest on the green glow.
Description of drawings
Fig. 1 is the X-ray diffractogram of the ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of embodiment 11 preparations.Fig. 2 be under embodiment nine to the 16 prepared ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversions condition that is 300mW in 980nm laser pumping, exciting power on the convert light spectrogram.Fig. 3 is that ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is changed green emission intensity with Er in wavelength 530nm and 552nm place
3+Concentration curve figure.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the chemical formula of present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.001≤x≤0.08 wherein.
Present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is doping Yb
3+And Er
3+CaWO
4The polycrystalline powder.
Embodiment two: the chemical formula of present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.002≤x≤0.04 wherein.
Embodiment three: the chemical formula of present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.005≤x≤0.02 wherein.
Embodiment four: the chemical formula of present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.008≤x≤0.01 wherein.
Embodiment five: present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.001≤x≤0.08 wherein;
Two, place agate mortar to grind 4 ± 0.5 hours in lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ± 50 ℃, and sintering time is 10 ± 0.5 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion.
The purity of lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder is 99.99% in the present embodiment step 1.
The present embodiment step was ground in agate mortar 4 ± 0.5 hours, made lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder thorough mixing even.
Embodiment six: the difference of present embodiment and embodiment five is: the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.002≤x≤0.04 wherein.Other step and parameter are identical with embodiment five.
Embodiment seven: the difference of present embodiment and embodiment five is: the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.005≤x≤0.02 wherein.Other step and parameter are identical with embodiment five.
Embodiment eight: the difference of present embodiment and embodiment five is: the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.008≤x≤0.01 wherein.Other step and parameter are identical with embodiment five.
Embodiment nine: present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.989WO
4: Yb
0.01/ Er
0.001
Two, lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing placed agate mortar ground 4 hours, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ℃, and sintering time is 10 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion; The purity of lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder is 99.99% in the step 1.
Present embodiment accurately takes by weighing 0.03956mol CaO, 0.04mol WO
3, 0.0002mol Yb
2O
3And 0.00002molEr
2O
3
The doping volumetric molar concentration of ytterbium ion is 1.0% in the prepared ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment, the doping volumetric molar concentration of erbium ion is 0.1%.
The ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment preparation is to send under the condition of 300mW to change green glow on bright in 980nm laser pumping, exciting power, and last inversion spectrum is shown in Fig. 2 curve a, and is and luminous even.
Embodiment ten: present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.988WO
4: Yb
0.01/ Er
0.002
Two, lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing placed agate mortar ground 4 hours, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ℃, and sintering time is 10 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion; The purity of lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder is 99.99% in the step 1.
Present embodiment accurately takes by weighing 0.03952mol CaO, 0.04mol WO
3, 0.0002mol Yb
2O
3And 0.00004molEr
2O
3
The doping volumetric molar concentration of ytterbium ion is 1.0% in the prepared ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment, the doping volumetric molar concentration of erbium ion is 0.2%.
The ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment preparation is to send under the condition of 300mW to change green glow on bright in 980nm laser pumping, exciting power, and last inversion spectrum is shown in Fig. 2 curve b, and is and luminous even.
Embodiment 11: present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.985WO
4: Yb
0.01/ Er
0.005
Two, lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing placed agate mortar ground 4 hours, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ℃, and sintering time is 10 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion; The purity of lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder is 99.99% in the step 1.
Present embodiment accurately takes by weighing 0.0394mol CaO, 0.04mol WO
3, 0.0002mol Yb
2O
3With 0.0001mol Er
2O
3
The doping volumetric molar concentration of ytterbium ion is 1.0% in the prepared ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment, the doping volumetric molar concentration of erbium ion is 0.5%.
The ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment preparation is to send under the condition of 300mW to change green glow on bright in 980nm laser pumping, exciting power, and last inversion spectrum is shown in Fig. 2 curve c, and is and luminous even.
The X-ray diffraction analysis result of the ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment preparation as shown in Figure 1.Fig. 1 X-ray diffraction analysis result and standard x RD card (JCPDS 77-2236) match, and illustrate that the ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment preparation has sheelite CaWO
4Structure.
Embodiment 12: present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.982WO
4: Yb
0.01/ Er
0.008
Two, lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing placed agate mortar ground 4 hours, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ℃, and sintering time is 10 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion; The purity of lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder is 99.99% in the step 1.
Present embodiment accurately takes by weighing 0.03928mol CaO, 0.04mol WO
3, 0.0002mol Yb
2O
3And 0.00016molEr
2O
3
The doping volumetric molar concentration of ytterbium ion is 1.0% in the prepared ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment, the doping volumetric molar concentration of erbium ion is 0.8%.
The ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment preparation is to send under the condition of 300mW to change green glow on bright in 980nm laser pumping, exciting power, and last inversion spectrum is shown in Fig. 2 curve d, and is and luminous even.
Embodiment 13: present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.98WO
4: Yb
0.01/ Er
0.01
Two, lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing placed agate mortar ground 4 hours, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ℃, and sintering time is 10 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion; The purity of lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder is 99.99% in the step 1.
Present embodiment accurately takes by weighing 0.0392mol CaO, 0.04mol WO
3, 0.0002mol Yb
2O
3With 0.0002mol Er
2O
3
The doping volumetric molar concentration of ytterbium ion is 1.0% in the prepared ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment, the doping volumetric molar concentration of erbium ion is 1.0%.
The ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment preparation is to send under the condition of 300mW to change green glow on bright in 980nm laser pumping, exciting power, and last inversion spectrum is shown in Fig. 2 curve e, and is and luminous even.
Embodiment 14: present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.97WO
4: Yb
0.01/ Er
0.02
Two, lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing placed agate mortar ground 4 hours, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ℃, and sintering time is 10 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion; The purity of lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder is 99.99% in the step 1.
Present embodiment accurately takes by weighing 0.0388mol CaO, 0.04mol WO
3, 0.0002mol Yb
2O
3With 0.0004mol Er
2O
3
The doping volumetric molar concentration of ytterbium ion is 1.0% in the prepared ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment, the doping volumetric molar concentration of erbium ion is 2.0%.
The ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment preparation is to send under the condition of 300mW to change green glow on bright in 980nm laser pumping, exciting power, and last inversion spectrum is shown in Fig. 2 curve f, and is and luminous even.
Embodiment 15: present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.95WO
4: Yb
0.01/ Er
0.04
Two, lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing placed agate mortar ground 4 hours, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ℃, and sintering time is 10 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion; The purity of lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder is 99.99% in the step 1.
Present embodiment accurately takes by weighing 0.038mol CaO, 0.04mol WO
3, 0.0002mol Yb
2O
3With 0.0008mol Er
2O
3
The doping volumetric molar concentration of ytterbium ion is 1.0% in the prepared ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment, the doping volumetric molar concentration of erbium ion is 4.0%.
The ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment preparation is to send under the condition of 300mW to change green glow on bright in 980nm laser pumping, exciting power, and last inversion spectrum is shown in Fig. 2 curve g, and is and luminous even.
Embodiment 16: present embodiment ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.91WO
4: Yb
0.01/ Er
0.08
Two, lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing placed agate mortar ground 4 hours, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ℃, and sintering time is 10 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion; The purity of lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder is 99.99% in the step 1.
Present embodiment accurately takes by weighing 0.0364mol CaO, 0.04mol WO
3, 0.0002mol Yb
2O
3With 0.0016mol Er
2O
3
The doping volumetric molar concentration of ytterbium ion is 1.0% in the prepared ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment, the doping volumetric molar concentration of erbium ion is 8.0%.
The ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion of present embodiment preparation is to send under the condition of 300mW to change green glow on bright in 980nm laser pumping, exciting power, and last inversion spectrum is shown in Fig. 2 curve h, and is and luminous even.
Can find out doping different concns Er according to Fig. 2
3+Ca
0.99-xWO
4: Yb
0.01/ Er
xThe conversion steady emission spectrum of going up of polycrystalline powder green glow up-conversion mainly is made of two photoluminescent bands in 400～750nm scope; One be by
2H
11/2→
4I
15/2The green emission peak that is positioned at 530nm wave band place that transition produced, another be by
4S
3/2→
4I
15/2The green emission peak that is positioned at 552nm wave band place that transition produced.The presentation of results of Fig. 2 ytterbium erbium of the present invention codope calcium wolframate polycrystalline powder green glow up-conversion excites at the 980nm laser apparatus the good green emission of monochromaticity down.
Claims (9)
1. ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is characterized in that the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.001≤x≤0.08 wherein.
2. ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion according to claim 1 is characterized in that the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.002≤x≤0.04 wherein.
3. ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion according to claim 1 is characterized in that the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.005≤x≤0.02 wherein.
4. ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion according to claim 1 is characterized in that the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.008≤x≤0.01 wherein.
5. prepare the described ytterbium erbium of claim 1 codope calcium wolframate polycrystalline powder green glow up-conversion, it is characterized in that ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion prepares by following step:
One, the stoichiometric ratio by ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion chemical formula takes by weighing lime powder, tungsten trioxide powder, yttria powder and erbium oxide powder, and the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.001≤x≤0.08 wherein;
Two, place agate mortar to grind 4 ± 0.5 hours in lime powder, tungsten trioxide powder, yttria powder and the erbium oxide powder that takes by weighing, placing pressure then is the pressure environment compressing tablet 10min of 18MPa, obtains the sheet precast body;
Three, the sheet precast body is put into carried out high temperature sintering under the air atmosphere, sintering temperature is 1300 ± 50 ℃, and sintering time is 10 ± 0.5 hours, and naturally cooling, grinding then promptly obtains ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion.
6. the preparation method of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion according to claim 5 is characterized in that the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.002≤x≤0.04 wherein.
7. the preparation method of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion according to claim 5 is characterized in that the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.005≤x≤0.02 wherein.
8. the preparation method of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion according to claim 5 is characterized in that the chemical formula of ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversion is Ca
0.99-xWO
4: Yb
0.01/ Er
x, 0.008≤x≤0.01 wherein.
9. according to the preparation method of claim 5,6,7 or 8 described ytterbium erbium codope calcium wolframate polycrystalline powder green glow up-conversions, it is characterized in that CaO powder, WO in the step 1
3Powder, Yb
2O
3Powder and Er
2O
3The purity of powder is 99.99%.
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| CN108962608A (en) * | 2018-07-19 | 2018-12-07 | 黑龙江大学 | A kind of preparation method of rare earth ion doped artificial schellite/titanium dioxide complex light anode |
| CN116285984A (en) * | 2023-03-31 | 2023-06-23 | 安徽工业大学 | Erbium ion activated ytterbium potassium molybdate self-activated up-conversion green light luminescent material and preparation method thereof |
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