CN102174323B - 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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Abstract
镱铥双掺七铝酸十二钙多晶及其制备方法，它涉及七铝酸十二钙多晶及其制备方法。本发明解决了现有的蓝光材料蓝色光波长分布宽，不利于应用的技术问题。本发明的镱铥双掺七铝酸十二钙多晶是由氧化钙、氧化铝、氧化镱和氧化铥制成的，其中氧化钙和氧化铝摩尔比为12∶7，氧化镱的物质的量为氧化钙物质的量的0.042％～0.42％，氧化铥的物质的量为氧化钙物质的量的0.042％～0.21％。方法：将氧化钙、氧化铝、氧化镱和氧化铥粉末研磨、压片后在空气氛下烧结得到镱铥双掺七铝酸十二钙多晶。在980nm的光激发下得到460nm～490nm的单一蓝光发射。可用于光存储技术、光电子技术、传感技术及海底光纤通讯领域。
Ytterbium thulium double-doped calcium dodecaaluminate polycrystal and a preparation method thereof relate to polycrystal dodecacalcium heptaaluminate and a preparation method thereof. The invention solves the technical problem that the existing blue light material has a wide blue light wavelength distribution and is unfavorable for application. The ytterbium-thulium double-doped calcium dodecaaluminate polycrystal of the present invention is made of calcium oxide, aluminum oxide, ytterbium oxide and thulium oxide, wherein the molar ratio of calcium oxide and aluminum oxide is 12:7, and the material of ytterbium oxide The amount is 0.042%-0.42% of the amount of calcium oxide substance, and the amount of thulium oxide substance is 0.042%-0.21% of the amount of calcium oxide substance. Method: Calcium oxide, aluminum oxide, ytterbium oxide and thulium oxide powders were ground, pressed into tablets and then sintered under air atmosphere to obtain ytterbium-thulium double-doped calcium dodecaaluminate polycrystals. Under the excitation of 980nm light, a single blue light emission of 460nm-490nm is obtained. It can be used in the fields of optical storage technology, optoelectronic technology, sensing technology and submarine optical fiber 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 again anti-Stokes luminescence, refers to two or more lower energy photons are converted to the phenomenon of a high-energy photon, up-conversion luminescent material need to be in matrix doped with rare-earth elements.The rare earth luminescent material energy absorption capability is strong, and efficiency of conversion is high; Can launch the spectrum from the UV-light to the infrared light, particularly at visible region very strong emissive power be arranged; 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 such 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 calcium oxide amount of substance, and the amount of substance of trioxide is 0.042%～0.21% of calcium oxide amount of substance.
Ytterbium thulium of the present invention is two preparation methods that mix the C 12 A 7 polycrystalline 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.
The present invention adopts broad-band gap oxide compound C 12 A 7 as the substrate material that mixes, by doping ytterbium, thulium element, and the doping content of regulating two kinds of elements, infrared ray excited lower at 980nm realized (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 the 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 mixing the C 12 A 7 polycrystalline of the ytterbium thulium of embodiment 13; Fig. 3 is the two luminous spectrograms of mixing the C 12 A 7 polycrystalline of the ytterbium thulium of embodiment 14; Fig. 4 is the two luminous spectrograms of mixing the C 12 A 7 polycrystalline of the ytterbium thulium of embodiment 15; Fig. 5 is the two luminous spectrograms of mixing the C 12 A 7 polycrystalline of the ytterbium thulium of embodiment 16; Fig. 6 is the two luminous spectrograms of mixing the C 12 A 7 polycrystalline 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 calcium oxide amount of substance, and the amount of substance of trioxide is 0.042%～0.21% of calcium oxide amount of substance.
Present embodiment adopts broad-band gap oxide compound C 12 A 7 as the substrate material that mixes, by doping ytterbium, thulium element, and the doping content of regulating two kinds of elements, infrared ray excited lower at 980nm realized (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 calcium oxide amount of substance, and the amount of substance of trioxide is 0.06%～0.18% of 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 calcium oxide amount of substance, and the amount of substance of trioxide is 0.10% of calcium oxide amount of substance.Other is identical with embodiment one.
Embodiment four: the ytterbium thulium of present embodiment is two preparation methods that mix the C 12 A 7 polycrystalline 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.
Present embodiment adopts broad-band gap oxide compound C 12 A 7 as the substrate material that mixes, by doping ytterbium, thulium element, and the doping content of regulating two kinds of elements, infrared ray excited lower at 980nm realized (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 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 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 from 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 from 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 from 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 from 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 from 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 from 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 preparation methods that mix the C 12 A 7 polycrystalline carry 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 X-ray diffraction spectrogram that the ytterbium thulium of present embodiment is two mixes the C 12 A 7 polycrystalline as shown in Figure 1, spectrogram a is the two X-ray diffraction spectrums of mixing the C 12 A 7 polycrystalline of ytterbium thulium among Fig. 1, spectrogram b is the standard spectrogram of standard C 12 A 7, the diffraction peak of polycrystalline 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 the ytterbium thulium ion that this explanation is mixed 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 preparation methods that mix the C 12 A 7 polycrystalline carry 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 preparation methods that mix the C 12 A 7 polycrystalline carry 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 preparation methods that mix the C 12 A 7 polycrystalline carry 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 preparation methods that mix the C 12 A 7 polycrystalline carry 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 (8)
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| CN102433120A (en) * | 2011-11-06 | 2012-05-02 | 北京科技大学 | Alkaline-earth metal silicate fluorescent material and preparation method thereof |
| CN102383186B (en) * | 2011-11-11 | 2013-12-11 | 哈尔滨工业大学 | Method of growing Ca12Al14O33 single crystal in non-stoichiometric melt by pulling method |
| 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 |
| 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 flower-like thulium-ytterbium double-doped dodecacalcium heptaaluminate and its application in temperature sensors |
| 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 |
| 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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