CN102174323A - Ytterbium and thulium codoped dodecacalcium heptaluminate polycrystal and preparation method thereof - Google Patents
Ytterbium and thulium codoped dodecacalcium heptaluminate polycrystal and preparation method thereof Download PDFInfo
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- CN102174323A CN102174323A CN2011100644382A CN201110064438A CN102174323A CN 102174323 A CN102174323 A CN 102174323A CN 2011100644382 A CN2011100644382 A CN 2011100644382A CN 201110064438 A CN201110064438 A CN 201110064438A CN 102174323 A CN102174323 A CN 102174323A
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Abstract
The invention discloses an ytterbium and thulium codoped dodecacalcium heptaluminate polycrystal and a preparation method thereof, relating to dodecacalcium heptaluminate polycrystal and a preparation method thereof, and solving the technical problem that the conventional blue material does not contribute to application due to wide blue wavelength distribution. The ytterbium and thulium codoped dodecacalcium heptaluminate polycrystal is prepared from calcium oxide, aluminum oxide, ytterbium oxide and thulium oxide, wherein the molar ratio of the calcium oxide to the aluminum oxide is 12:7; the amount of substance of the ytterbium oxide is 0.042-0.42 percent of that of the calcium oxide; and the amount of substance of the thulium oxide is 0.042-0.21 percent of that of the calcium oxide. The method comprises the following steps of: grinding the calcium oxide, the aluminum oxide, the ytterbium oxide and the thulium oxide powder; sheeting; and sintering under an air atmosphere to obtain the ytterbium and thulium codoped dodecacalcium heptaluminate polycrystal. Single blue light emission with wavelength of 460-490nm is obtained under excitation of light with wavelength of 980nm. The polycrystal can be used in the fields of light storage technology, optoelectronic technology, sensor technology and submarine optical cable communication.
Description
Technical field
The present invention relates to C 12 A 7 polycrystalline 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 rare earth luminescent material energy absorption capability 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; Their physicochemical property are stable, can bear the advantages such as effect of powerful electron beam, energetic ray and strong UV-light, be that the Chinese patent of CN101671561A discloses a kind of blue long afterglow luminescence C 12 A 7 (chemical formula is 12CaO7Al as publication number
2O
3Be abbreviated as C12A7) powder preparation method, this invention adopts chemical coprecipitation to prepare europium, dysprosium co-doped C 12 A 7 powder, this powder ultraviolet excitation, blue monochromatic light emission with steady persistence, but the complexity because the energy level of most of rare earth elements distributes, the blue light Wavelength distribution that this material obtains is wide, is unfavorable for using.
Summary of the invention
The present invention is wide in order to solve existing blue light material blue light Wavelength distribution, is unfavorable for the technical problem used, and provides the ytterbium thulium two C 12 A 7 polycrystalline and preparation method thereof of mixing.
Ytterbium thulium of the present invention is two to be mixed the C 12 A 7 polycrystalline and is made by calcium oxide, aluminum oxide, ytterbium oxide and trioxide, wherein calcium oxide and alumina molar ratio are 12: 7, the amount of substance of ytterbium oxide is 0.042%～0.42% of a calcium oxide amount of substance, and the amount of substance of trioxide is 0.042%～0.21% of a calcium oxide amount of substance.
Ytterbium thulium of the present invention is two to be mixed C 12 A 7 polycrystalline preparation method and carries out according to the following steps: one, according to CaO and Al
2O
3The mol ratio of powder is to take by weighing CaO and Al at 12: 7
2O
3Powder also places agate mortar; Two, the amount of substance by ytterbium oxide is that 0.042%～0.42% of CaO amount of substance takes by weighing in the described agate mortar of ytterbium oxide adding step 1, accounting for 0.042%～0.21% of CaO amount of substance by the amount of substance of trioxide takes by weighing trioxide and also adds in the described agate mortar of step 1, grind 4h～6h, obtain uniform powder; Three, the uniform powder that step 2 obtained adds compression mold, at pressure is to keep 5min～10min under the condition of 7MPa～15MPa, obtains material piece; Four, with material piece sintering under air atmosphere of step 3 preparation, sintering temperature is 1300 ℃～1400 ℃, and sintering time is 10h～12h, obtains the two C 12 A 7 polycrystalline of mixing of ytterbium thulium.
The present invention adopts broad-band gap oxide compound C 12 A 7 as adulterated substrate material, by doping ytterbium, thulium element, and the doping content of regulating two kinds of elements, 980nm infrared ray excited down, realize (the converting blue light emission on the good high strength of the monochromaticity of 460nm～490nm) of narrow wavelength region.
Ytterbium thulium of the present invention is two to be mixed the C 12 A 7 polycrystalline and can be used for aspects such as optical storage technology, photoelectron technology, sensing technology and seabed fiber communication.
Description of drawings
Fig. 1 is the two X-ray diffraction spectrograms of mixing C 12 A 7 polycrystalline and standard C 12 A 7 of the ytterbium thulium of embodiment 13 preparations; Fig. 2 is the two luminous spectrograms of C 12 A 7 polycrystalline of mixing of the ytterbium thulium of embodiment 13; Fig. 3 is the two luminous spectrograms of C 12 A 7 polycrystalline of mixing of the ytterbium thulium of embodiment 14; Fig. 4 is the two luminous spectrograms of C 12 A 7 polycrystalline of mixing of the ytterbium thulium of embodiment 15; Fig. 5 is the two luminous spectrograms of C 12 A 7 polycrystalline of mixing of the ytterbium thulium of embodiment 16; Fig. 6 is the two luminous spectrograms of C 12 A 7 polycrystalline of mixing of the ytterbium thulium of embodiment 17.
Embodiment
Embodiment one: the ytterbium thulium of present embodiment is two to be mixed the C 12 A 7 polycrystalline and is made by calcium oxide, aluminum oxide, ytterbium oxide and trioxide, wherein calcium oxide and alumina molar ratio are 12: 7, the amount of substance of ytterbium oxide is 0.042%～0.42% of a calcium oxide amount of substance, and the amount of substance of trioxide is 0.042%～0.21% of a calcium oxide amount of substance.
Present embodiment adopts broad-band gap oxide compound C 12 A 7 as adulterated substrate material, by doping ytterbium, thulium element, and the doping content of regulating two kinds of elements, 980nm infrared ray excited down, realize (the converting blue light emission on the good high strength of the monochromaticity of 460nm～490nm) of narrow wavelength region.
Embodiment two: present embodiment and embodiment one are different is that the amount of substance of ytterbium oxide is 0.06%～0.35% of a calcium oxide amount of substance, and the amount of substance of trioxide is 0.06%～0.18% of a calcium oxide amount of substance.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different is that the amount of substance of ytterbium oxide is 0.15% of a calcium oxide amount of substance, and the amount of substance of trioxide is 0.10% of a calcium oxide amount of substance.Other is identical with embodiment one.
Embodiment four: the ytterbium thulium of present embodiment is two to be mixed C 12 A 7 polycrystalline preparation method and carries out according to the following steps: one, according to CaO and Al
2O
3The mol ratio of powder is to take by weighing CaO and Al at 12: 7
2O
3Powder also places agate mortar; Two, the amount of substance by ytterbium oxide is that 0.042%～0.42% of CaO amount of substance takes by weighing in the described agate mortar of ytterbium oxide adding step 1, accounting for 0.042%～0.21% of CaO amount of substance by the amount of substance of trioxide takes by weighing trioxide and also adds in the described agate mortar of step 1, grind 4h～6h, obtain uniform powder; Three, the uniform powder that step 2 obtained adds compression mold, at pressure is to keep 5min～10min under the condition of 7MPa～15MPa, obtains material piece; Four, with material piece sintering under air atmosphere of step 3 preparation, sintering temperature is 1300 ℃～1400 ℃, and sintering time is 10h～12h, obtains the two C 12 A 7 polycrystalline of mixing of ytterbium thulium.
Present embodiment adopts broad-band gap oxide compound C 12 A 7 as adulterated substrate material, by doping ytterbium, thulium element, and the doping content of regulating two kinds of elements, 980nm infrared ray excited down, realize (the converting blue light emission on the good high strength of the monochromaticity of 460nm～490nm) of narrow wavelength region.
Embodiment five: present embodiment and embodiment four are different is that the amount of substance of ytterbium oxide in the step 2 is 0.06%～0.38% of a CaO amount of substance, and the amount of substance of trioxide accounts for 0.06%～0.18% of CaO amount of substance.Other is identical with embodiment four.
Embodiment six: present embodiment and embodiment four are different is that the amount of substance of ytterbium oxide in the step 2 is 0.20% of a CaO amount of substance, and the amount of substance of trioxide accounts for 0.10% of CaO amount of substance.Other is identical with embodiment four.
Embodiment seven: present embodiment is different with one of embodiment four to six is that milling time in the step 2 is 4.5h～5.5h.Other is identical with one of embodiment four to six.
Embodiment eight: what present embodiment was different with one of embodiment four to six is that milling time is 5.0h in the step 2.Other is identical with one of embodiment four to six.
Embodiment nine: present embodiment is different with one of embodiment four to eight is that pressure in the step 3 is 7.5MPa～14MPa, and the dwell time is 6min～9min.Other is identical with one of embodiment four to eight.
Embodiment ten: present embodiment is different with one of embodiment four to eight is that pressure in the step 3 is 10MPa, and the dwell time is 8min.Other is identical with one of embodiment four to eight.
Embodiment 11: what present embodiment was different with one of embodiment four to ten is that sintering temperature is 1320 ℃～1380 ℃ in the step 4, and sintering time is 10.5h～11.5h.Other is identical with one of embodiment four to ten.
Embodiment 12: what present embodiment was different with one of embodiment four to ten is that sintering temperature is 1350 ℃ in the step 4, and sintering time is 11.0h.Other is identical with one of embodiment four to ten.
Embodiment 13: the ytterbium thulium of present embodiment is two to be mixed C 12 A 7 polycrystalline preparation method and carries out according to the following steps: one, take by weighing 2.6379g purity and be 99.99% CaO and 2.7978g purity and be 99.99% Al
2O
3Powder also places agate mortar; Two, taking by weighing 0.0158g purity is 99.99% Yb
2O
3Ytterbium oxide adds in the described agate mortar of step 1, and taking by weighing 0.0077g purity is 99.99%Tm
2O
3Also add in the described agate mortar of step 1, grind 4h, obtain uniform powder; Three, the uniform powder that step 2 obtained adds compression mold, at pressure is to keep 5min under the condition of 10MPa, obtains material piece; Four, with material piece sintering under air atmosphere of step 3 preparation, sintering temperature is 1300 ℃, and sintering time is 10h, obtains the two C 12 A 7 polycrystalline of mixing of ytterbium thulium.
The two doping volumetric molar concentrations of mixing thulium ion in the C 12 A 7 polycrystalline of the ytterbium thulium that present embodiment obtains are 1%, and the doping volumetric molar concentration of ytterbium ion is 2%.The ytterbium thulium of present embodiment is two mixes C 12 A 7 polycrystalline X-ray diffraction spectrogram as shown in Figure 1, spectrogram a is the two C 12 A 7 polycrystalline X-ray diffraction spectrums of mixing of ytterbium thulium among Fig. 1, spectrogram b is the standard spectrogram of standard C 12 A 7, the polycrystalline diffraction peak of ytterbium and thulium ion of as can be seen from Figure 1 having mixed can match with the standard X-ray diffraction spectra of C 12 A 7, and this illustrates that adulterated ytterbium thulium ion does not change the crystalline network of C 12 A 7.
The two C 12 A 7 polycrystalline of mixing of the ytterbium thulium that present embodiment is obtained, carry out 980nm and excite the up-conversion fluorescence spectrum test, the 980nm that obtains excites the up-conversion fluorescence spectrogram as shown in Figure 2, as can be seen from Figure 2, utilize 980nm laser excitation, the ytterbium thulium is two mixes the C 12 A 7 polycrystalline only has the blue-light-emitting of a narrow wavelength region at 460nm～490nm place.
Embodiment 14: the ytterbium thulium of present embodiment is two to be mixed C 12 A 7 polycrystalline preparation method and carries out according to the following steps: one, take by weighing 2.6379g purity and be 99.99% CaO and 2.7978g purity and be 99.99% Al
2O
3Powder also places agate mortar; Two, taking by weighing 0.0395g purity is 99.99% Yb
2O
3Ytterbium oxide adds in the described agate mortar of step 1, and taking by weighing 0.0077g purity is 99.99%Tm
2O
3Also add in the described agate mortar of step 1, grind 4h, obtain uniform powder; Three, the uniform powder that step 2 obtained adds compression mold, at pressure is to keep 5min under the condition of 10MPa, obtains material piece; Four, with material piece sintering under air atmosphere of step 3 preparation, sintering temperature is 1300 ℃, and sintering time is 10h, obtains the two C 12 A 7 polycrystalline of mixing of ytterbium thulium.
The two doping volumetric molar concentrations of mixing thulium ion in the C 12 A 7 polycrystalline of the ytterbium thulium that present embodiment obtains are 1%, and the doping volumetric molar concentration of ytterbium ion is 5%.
The two C 12 A 7 polycrystalline of mixing of the ytterbium thulium that present embodiment is obtained, carry out 980nm and excite the up-conversion fluorescence spectrum test, the 980nm that obtains excites the up-conversion fluorescence spectrogram as shown in Figure 3, as can be seen from Figure 3, utilize 980nm laser excitation, the ytterbium thulium is two mixes the C 12 A 7 polycrystalline only has the blue-light-emitting of a narrow wavelength region at 460nm～490nm place, the luminous intensity height.
Embodiment 15: the ytterbium thulium of present embodiment is two to be mixed C 12 A 7 polycrystalline preparation method and carries out according to the following steps: one, take by weighing 2.6379g purity and be 99.99% CaO and 2.7978g purity and be 99.99% Al
2O
3Powder also places agate mortar; Two, taking by weighing 0.0790g purity is 99.99% Yb
2O
3Ytterbium oxide adds in the described agate mortar of step 1, and taking by weighing 0.0077g purity is 99.99%Tm
2O
3Also add in the described agate mortar of step 1, grind 4h, obtain uniform powder; Three, the uniform powder that step 2 obtained adds compression mold, at pressure is to keep 5min under the condition of 10MPa, obtains material piece; Four, with material piece sintering under air atmosphere of step 3 preparation, sintering temperature is 1300 ℃, and sintering time is 10h, obtains the two C 12 A 7 polycrystalline of mixing of ytterbium thulium.
The two doping volumetric molar concentrations of mixing thulium ion in the C 12 A 7 polycrystalline of the ytterbium thulium that present embodiment obtains are 1%, and the doping volumetric molar concentration of ytterbium ion is 10%.
The two C 12 A 7 polycrystalline of mixing of the ytterbium thulium that present embodiment is obtained, carry out 980nm and excite the up-conversion fluorescence spectrum test, the 980nm that obtains excites the up-conversion fluorescence spectrogram as shown in Figure 4, as can be seen from Figure 4, utilize 980nm laser excitation, the ytterbium thulium is two mixes the C 12 A 7 polycrystalline only has the blue-light-emitting of a narrow wavelength region at 460nm～490nm place, the luminous intensity height.
Embodiment 16: the ytterbium thulium of present embodiment is two to be mixed C 12 A 7 polycrystalline preparation method and carries out according to the following steps: one, take by weighing 2.6379g purity and be 99.99% CaO and 2.7978g purity and be 99.99% Al
2O
3Powder also places agate mortar; Two, taking by weighing 0.0790g purity is 99.99% Yb
2O
3Ytterbium oxide adds in the described agate mortar of step 1, and taking by weighing 0.0154g purity is 99.99%Tm
2O
3Also add in the described agate mortar of step 1, grind 5h, obtain uniform powder; Three, the uniform powder that step 2 obtained adds compression mold, at pressure is to keep 6min under the condition of 15MPa, obtains material piece; Four, with material piece sintering under air atmosphere of step 3 preparation, sintering temperature is 1350 ℃, and sintering time is 10h, obtains the two C 12 A 7 polycrystalline of mixing of ytterbium thulium.
The two doping volumetric molar concentrations of mixing thulium ion in the C 12 A 7 polycrystalline of the ytterbium thulium that present embodiment obtains are 2%, and the doping volumetric molar concentration of ytterbium ion is 10%.
The two C 12 A 7 polycrystalline of mixing of the ytterbium thulium that present embodiment is obtained, carry out 980nm and excite the up-conversion fluorescence spectrum test, the 980nm that obtains excites the up-conversion fluorescence spectrogram as shown in Figure 5, as can be seen from Figure 5, utilize 980nm laser excitation, the ytterbium thulium is two mixes the C 12 A 7 polycrystalline only has the blue-light-emitting of a narrow wavelength region at 460nm～490nm place, the luminous intensity height.
Embodiment 17: the ytterbium thulium of present embodiment is two to be mixed C 12 A 7 polycrystalline preparation method and carries out according to the following steps: one, take by weighing 2.6379g purity and be 99.99% CaO and 2.7978g purity and be 99.99% Al
2O
3Powder also places agate mortar; Two, taking by weighing 0.0790g purity is 99.99% Yb
2O
3Ytterbium oxide adds in the described agate mortar of step 1, and taking by weighing 0.0385g purity is 99.99%Tm
2O
3Also add in the described agate mortar of step 1, grind 5h, obtain uniform powder; Three, the uniform powder that step 2 obtained adds compression mold, at pressure is to keep 6min under the condition of 15MPa, obtains material piece; Four, with material piece sintering under air atmosphere of step 3 preparation, sintering temperature is 1350 ℃, and sintering time is 10h, obtains the two C 12 A 7 polycrystalline of mixing of ytterbium thulium.
The two doping volumetric molar concentrations of mixing thulium ion in the C 12 A 7 polycrystalline of the ytterbium thulium that present embodiment obtains are 5%, and the doping volumetric molar concentration of ytterbium ion is 10%.
The two C 12 A 7 polycrystalline of mixing of the ytterbium thulium that present embodiment is obtained, carry out 980nm and excite the up-conversion fluorescence spectrum test, the 980nm that obtains excites the up-conversion fluorescence spectrogram as shown in Figure 6, as can be seen from Figure 6, utilize 980nm laser excitation, the ytterbium thulium is two mixes the C 12 A 7 polycrystalline only has the blue-light-emitting of a narrow wavelength region at 460nm～490nm place, the luminous intensity height.
Claims (10)
1. two C 12 A 7 polycrystalline of mixing of ytterbium thulium, it is characterized in that the ytterbium thulium is two mixes the C 12 A 7 polycrystalline and is made by calcium oxide, aluminum oxide, ytterbium oxide and trioxide, wherein calcium oxide and alumina molar ratio are 12: 7, the amount of substance of ytterbium oxide is 0.042%～0.42% of a calcium oxide amount of substance, and the amount of substance of trioxide is 0.042%～0.21% of a calcium oxide amount of substance.
2. ytterbium thulium according to claim 1 is two mixes the C 12 A 7 polycrystalline, and the amount of substance that it is characterized in that ytterbium oxide is 0.06%～0.35% of a calcium oxide amount of substance, and the amount of substance of trioxide is 0.06%～0.18% of a calcium oxide amount of substance.
3. ytterbium thulium according to claim 1 is two mixes the C 12 A 7 polycrystalline, and the amount of substance that it is characterized in that ytterbium oxide is 0.15% of a calcium oxide amount of substance, and the amount of substance of trioxide is 0.10% of a calcium oxide amount of substance.
4. ytterbium thulium as claimed in claim 1 is two mixes C 12 A 7 polycrystalline preparation method, it is characterized in that the ytterbium thulium is two to mix C 12 A 7 polycrystalline preparation method and carry out according to the following steps: one, according to CaO and Al
2O
3The mol ratio of powder is to take by weighing CaO and Al at 12: 7
2O
3Powder also places agate mortar; Two, the amount of substance by ytterbium oxide is that 0.042%～0.42% of CaO amount of substance takes by weighing in the described agate mortar of ytterbium oxide adding step 1, accounting for 0.042%～0.21% of CaO amount of substance by the amount of substance of trioxide takes by weighing trioxide and also adds in the described agate mortar of step 1, grind 4h～6h, obtain uniform powder; Three, the uniform powder that step 2 obtained adds compression mold, at pressure is to keep 5min～10min under the condition of 7MPa～15MPa, obtains material piece; Four, with material piece sintering under air atmosphere of step 3 preparation, sintering temperature is 1300 ℃～1400 ℃, and sintering time is 10h～12h, obtains the two C 12 A 7 polycrystalline of mixing of ytterbium thulium.
5. the two C 12 A 7 polycrystalline preparation methods that mix of ytterbium thulium according to claim 4, the amount of substance that it is characterized in that ytterbium oxide in the step 2 is 0.06%～0.38% of a CaO amount of substance, and the amount of substance of trioxide accounts for 0.06%～0.18% of CaO amount of substance.
6. mix C 12 A 7 polycrystalline preparation method according to claim 4 or 5 described ytterbium thuliums are two, it is characterized in that the milling time in the step 2 is 4.5h～5.5h.
7. mix C 12 A 7 polycrystalline preparation method according to claim 4 or 5 described ytterbium thuliums are two, it is characterized in that the pressure in the step 3 is 7.5MPa～14MPa, the dwell time is 6min～9min.
8. mix C 12 A 7 polycrystalline preparation method according to claim 4 or 5 described ytterbium thuliums are two, it is characterized in that the pressure in the step 3 is 10MPa, the dwell time is 8min.
9. mix C 12 A 7 polycrystalline preparation method according to claim 4 or 5 described ytterbium thuliums are two, it is characterized in that sintering temperature is 1320 ℃～1380 ℃ in the step 4, sintering time is 10.5h～11.5h.
10. mix C 12 A 7 polycrystalline preparation method according to claim 4 or 5 described ytterbium thuliums are two, it is characterized in that sintering temperature is 1350 ℃ in the step 4, sintering time is 11.0h.
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| CN103421491A (en) * | 2012-05-14 | 2013-12-04 | 海洋王照明科技股份有限公司 | Terbium and ytterbium co-doped '12:7' calcium aluminate group up-conversion luminescent material, and preparation method and application thereof |
| CN103421491B (en) * | 2012-05-14 | 2016-04-13 | 海洋王照明科技股份有限公司 | Terbium ytterbium codoped C 12 A 7 base up-conversion luminescent material, preparation method and Organic Light Emitting Diode |
| CN103311365A (en) * | 2013-05-21 | 2013-09-18 | 哈尔滨工业大学 | Rare earth-doped mayenite thin-film material preparation method |
| CN103311365B (en) * | 2013-05-21 | 2016-05-25 | 哈尔滨工业大学 | A kind of preparation method of rear-earth-doped C 12 A 7 thin-film material |
| CN109292805A (en) * | 2018-09-13 | 2019-02-01 | 广东工业大学 | A kind of flower-shaped thulium ytterbium codope C 12 A 7 and its application in temperature sensor |
| CN109439320A (en) * | 2018-09-13 | 2019-03-08 | 广东工业大学 | A kind of flower-shaped thulium ytterbium codope C 12 A 7 and preparation method thereof |
| CN109439320B (en) * | 2018-09-13 | 2021-11-26 | 广东工业大学 | Flower-shaped thulium ytterbium double-doped dodecacalcium heptaluminate and preparation method thereof |
| CN109880615A (en) * | 2019-04-11 | 2019-06-14 | 广东工业大学 | A kind of C 12 A 7 up-conversion luminescent material and preparation method thereof |
| CN109880615B (en) * | 2019-04-11 | 2021-09-03 | 广东工业大学 | Calcium dodecaheptaluminate up-conversion luminescent material and preparation method thereof |
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