CN103224790A - Material for conversion of ultraviolet light and emission of near-infrared light and its preparation method and use - Google Patents
Material for conversion of ultraviolet light and emission of near-infrared light and its preparation method and use Download PDFInfo
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- CN103224790A CN103224790A CN2013100247300A CN201310024730A CN103224790A CN 103224790 A CN103224790 A CN 103224790A CN 2013100247300 A CN2013100247300 A CN 2013100247300A CN 201310024730 A CN201310024730 A CN 201310024730A CN 103224790 A CN103224790 A CN 103224790A
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- 239000000463 material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 title abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 17
- 230000005284 excitation Effects 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
- -1 rare earth erbium ion Chemical group 0.000 claims description 68
- 150000001875 compounds Chemical class 0.000 claims description 48
- 238000001354 calcination Methods 0.000 claims description 32
- 150000002500 ions Chemical class 0.000 claims description 27
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 23
- 238000005303 weighing Methods 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 18
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 13
- 229940010552 ammonium molybdate Drugs 0.000 claims description 13
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 13
- 239000011609 ammonium molybdate Substances 0.000 claims description 13
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 13
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 13
- 229940075624 ytterbium oxide Drugs 0.000 claims description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 12
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- 239000011733 molybdenum Substances 0.000 claims description 7
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- 229910052691 Erbium Inorganic materials 0.000 claims description 6
- 229910052693 Europium Inorganic materials 0.000 claims description 6
- 229910052689 Holmium Inorganic materials 0.000 claims description 6
- 229910052765 Lutetium Inorganic materials 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 6
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052772 Samarium Inorganic materials 0.000 claims description 6
- 229910052771 Terbium Inorganic materials 0.000 claims description 6
- 229910052775 Thulium Inorganic materials 0.000 claims description 6
- 229910001422 barium ion Inorganic materials 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 6
- 229910001424 calcium ion Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 6
- RJOJUSXNYCILHH-UHFFFAOYSA-N gadolinium(3+) Chemical compound [Gd+3] RJOJUSXNYCILHH-UHFFFAOYSA-N 0.000 claims description 6
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 claims description 6
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 6
- WCWKKSOQLQEJTE-UHFFFAOYSA-N praseodymium(3+) Chemical compound [Pr+3] WCWKKSOQLQEJTE-UHFFFAOYSA-N 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 229910001427 strontium ion Inorganic materials 0.000 claims description 6
- PWYYWQHXAPXYMF-UHFFFAOYSA-N strontium(2+) Chemical compound [Sr+2] PWYYWQHXAPXYMF-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 3
- 238000003836 solid-state method Methods 0.000 claims description 3
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 3
- KUBYTSCYMRPPAG-UHFFFAOYSA-N ytterbium(3+);trinitrate Chemical compound [Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUBYTSCYMRPPAG-UHFFFAOYSA-N 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052710 silicon Inorganic materials 0.000 abstract description 8
- 239000010703 silicon Substances 0.000 abstract description 8
- 229910015667 MoO4 Inorganic materials 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 26
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 20
- 239000002994 raw material Substances 0.000 description 12
- 238000001228 spectrum Methods 0.000 description 12
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 10
- 238000000634 powder X-ray diffraction Methods 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 8
- 238000000695 excitation spectrum Methods 0.000 description 8
- 239000004570 mortar (masonry) Substances 0.000 description 6
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 244000191761 Sida cordifolia Species 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229910003440 dysprosium oxide Inorganic materials 0.000 description 2
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 2
- ZXGIFJXRQHZCGJ-UHFFFAOYSA-N erbium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Er+3].[Er+3] ZXGIFJXRQHZCGJ-UHFFFAOYSA-N 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001235 sensitizing effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Images
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/52—PV systems with concentrators
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- Luminescent Compositions (AREA)
Abstract
The invention discloses a material for conversion of ultraviolet light and emission of near-infrared light and its preparation method and use. The material has a general chemical formula of MR2-2xYb2x(MoO4)4, wherein R represents one or more of Er<3+>, Eu<3+>, La<3+>, Y<3+>, Ce<3+>, Tm<3+>, Pr<3+>, Nd<3+>, Sm<3+>, Gd<3+>, Tb<3+>, Dy<3+>, Ho<3+> and Lu<3+>; M represents one or more of Ca<2+>, Sr<2+> and Ba<2+>; and x represents a mole percentage of doped Yb<3+> and is greater than or equal to 0.0001 and less than or equal to 1.0. The material prepared by a high temperature solid phase method or a chemical synthesis method can emit near-infrared light having the wavelength of 950 to 1100nm under the excitation of ultraviolet light having the wavelength of 250 to 400nm, can be used as a light conversion material for a silicon-based solar cell, and can improve cell photoelectric conversion efficiency and performance stability.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of luminescent material, the particularly a kind of preparation methods and application thereof that can realize UV-light switching emission near infrared light belongs to the field of light emitting materials in the shiner Neo-Confucianism.
Background technology
Entered since 21 century, non-renewable Energy resources are day by day exhausted and be difficult to exploitation more, and the harm that in the recovery process environment is caused becomes increasingly conspicuous.Renewable energy source pollution-free, cleaning gets most of the attention, and objectively facilitates sun power to become the emphasis of development and use, and wherein most active is the research field of solar cell.
Solar cell is a kind of device that solar energy is converted into electric energy owing to photovoltaic effect, it is a semiconductor photo diode, when solar irradiation was to photorectifier, photorectifier will become electric energy to the luminous energy of the sun, produced electric current.Wherein, silicon is the most frequently used semiconductor material, is bringing into play absolute leading role in photovoltaic industry.Yet, the energy gap of crystalline silicon is 1.12eV approximately, silicon solar cell is 400 ~ 1100nm to the significant response spectral range of incident light, the spectral distribution of this and sunlight is not exclusively mated, cause the ultraviolet and the blue green light that account for very most short wavelength in the sunlight to be difficult to be absorbed by solar cell, this spectrum mismatch phenomenon will cause the very big loss of solar energy, therefore development of new can be adjusted the luminescent material of solar spectral, and the photoelectric transformation efficiency that improves crystal silicon solar batteries is one of focal issue of current extensive concern.
Down-conversion luminescence is meant the UV-light that absorbs a high-energy photon, the phenomenon of launching two or more lower energy photons.It can become the light conversion of the short-and-medium wavelength of sunlight long wavelength's light, can greatly eliminate the spectrum mismatch phenomenon, improves the utilization ratio of sunlight, thereby improves the electricity conversion of monocrystaline silicon solar cell indirectly.Because Yb
3+The ionic infrared emission is positioned at the 1000nm place, mates very much with the energy gap of silicon single crystal, therefore is often used as down the dopant ion of transition material.But Yb
3+Ion ultraviolet to the visible region specific absorption a little less than, perhaps almost do not absorb, studying maximum at present is by mixing trivalent rare earth ions (as: Tb altogether
3+, Pr
3+, Er
3+Deng) improve it in the absorption of ultraviolet as sensitizing agent to visible region, thus solar energy utilization rate improved.P. people such as Vergeer is at Phys. Rev. B, report in 71 (2005): codoped rare earth Tb in oxide powder
3+/ Yb
3+Ion pair has realized the quantum-cutting emission of visible light near infrared light; People such as Li Kaiyu are at luminous journal, report in 5 (2012): successfully prepared Pr
3+, Yb
3+The YPO of codoped
4Powder has realized that the following conversion under the 450nm optical excitation is near-infrared luminous.
Yet though these sensitized ions have absorption in ultraviolet to visible region, its absorption all is wire, and absorption intensity is more weak.And the light-converting material of the present invention's preparation is utilizing Yb
3+In the time of emission of ions, absorb transfer by interband and give the Doped Rare Earth ion transmission ofenergy, can realize wide band absorption like this, not only improved it in the absorption of ultraviolet to visible region, weaken the heat effect of silica-based solar cell simultaneously, be expected to obtaining to use aspect the raising crystal silicon solar energy battery transformation efficiency.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of silica-based solar cell light-converting material of realizing UV-light switching emission near infrared light is provided.
Another object of the present invention provides above-mentioned UV-light switching emission near infrared light preparation methods, and this preparation technology is simple, and production cost is low.
For achieving the above object, the technical solution used in the present invention is: a kind of material of UV-light switching emission near infrared light is provided, and it launches the near infrared light of 950nm～1100nm under the ultraviolet excitation of 250nm～400nm; The chemical general formula of described material is MR
2-2xYb
2x(MoO
4)
4, wherein, R is rare earth erbium ion Er
3+, europium ion Eu
3+, lanthanum ion La
3+, ruthenium ion Y
3+, cerium ion Ce
3+, thulium ion Tm
3+, praseodymium ion Pr
3+, neodymium ion Nd
3+, samarium ion Sm
3+, gadolinium ion Gd
3+, terbium ion Tb
3+, dysprosium ion Dy
3+, holmium ion Ho
3+, lutetium ion Lu
3+In a kind of or their arbitrary combination; M is alkaline-earth metal ions calcium ion Ca
2+, strontium ion Sr
2+, barium ion Ba
2+In a kind of or their arbitrary combination;
xBe Yb
3+Adulterated molecular fraction, 0.0001≤x≤1.0.
The preparation methods of above-mentioned UV-light switching emission near infrared light adopts high temperature solid-state method, comprises the steps:
1, presses chemical formula MR
2-2xYb
2x(MoO
4)
4In the stoichiometric ratio of each element, wherein 0.0001≤x≤1.0 take by weighing respectively and contain ytterbium ion Yb
3+Compound, contain ion
RCompound, contain ion
MCompound, contain molybdenum ion Mo
6+Compound, grind and mix, obtain mixture; Described ion R is rare earth erbium ion Er
3+, europium ion Eu
3+, lanthanum ion La
3+, ruthenium ion Y
3+, cerium ion Ce
3+, thulium ion Tm
3+, praseodymium ion Pr
3+, neodymium ion Nd
3+, samarium ion Sm
3+, gadolinium ion Gd
3+, terbium ion Tb
3+, dysprosium ion Dy
3+, holmium ion Ho
3+, lutetium ion Lu
3+In a kind of or their arbitrary combination; Described ion M is alkaline-earth metal ions calcium ion Ca
2+, strontium ion Sr
2+, barium ion Ba
2+In a kind of or their arbitrary combination;
2, the mixture that step 1 is obtained is calcined under air atmosphere 1～2 time; Described calcining temperature is 200～600 ℃, and calcination time is 1～12 hour;
3, the mixture naturally cooling that step 2 is obtained after grinding and mixing, is calcined in air atmosphere, and calcining temperature is 600～850 ℃, and calcination time is 1～12 hour;
4, the mixture naturally cooling that step 3 is obtained after grinding and mixing, is calcined in air atmosphere, calcining temperature is 850～1000 ℃, calcination time is 1～12 hour, naturally cools to room temperature, obtains a kind of material of UV-light switching emission near infrared light.
The preferred version that above-mentioned high temperature solid-state method prepares UV-light switching emission near infrared light material is: the calcining temperature of step 2 is 250～550 ℃, and calcination time is 2～10 hours.The calcining temperature of step 3 is 650～800 ℃, and calcination time is 2～10 hours.The calcining temperature of step 4 is 850～950 ℃, and calcination time is 2～10 hours.
The preparation methods of the described a kind of UV-light switching emission near infrared light of technical solution of the present invention also comprises the employing chemical synthesis, step specific as follows:
1, presses chemical formula MR
2-2xYb
2x(MoO
4)
4In the stoichiometric ratio of each element, wherein 0.0001≤x≤1.0 take by weighing and contain ytterbium ion Yb
3+Compound, contain ion R compound, contain the compound of ion M, they are dissolved in respectively in the dilute nitric acid solution, obtain various clear solutions; 0.5～2.0wt% by each reactant quality adds complexing agent citric acid or oxalic acid respectively, stirs under 50～100 ℃ temperature condition; Described ion R is rare earth erbium ion Er
3+, europium ion Eu
3+, lanthanum ion La
3+, ruthenium ion Y
3+, cerium ion Ce
3+, thulium ion Tm
3+, praseodymium ion Pr
3+, neodymium ion Nd
3+, samarium ion Sm
3+, gadolinium ion Gd
3+, terbium ion Tb
3+, dysprosium ion Dy
3+, holmium ion Ho
3+, lutetium ion Lu
3+In a kind of or their arbitrary combination; Described ion M is alkaline-earth metal ions calcium ion Ca
2+, strontium ion Sr
2+, barium ion Ba
2+In a kind of or their arbitrary combination; Take by weighing respectively and contain ytterbium ion Yb
3+Compound, contain rare earth ion R compound, contain the compound of alkaline-earth metal ions M;
2, press chemical formula MR
2-2xYb
2x(MoO
4)
4In the stoichiometric ratio of each element, wherein 0.0001≤x≤1.0 take by weighing and contain molybdenum ion Mo
6+Compound, be dissolved in deionized water or the ethanolic soln, the 0.5～2.0wt% that presses the reactant quality adds complexing agent citric acid or oxalic acid, stirs under 50～100 ℃ temperature condition;
3, the various solution that step 1 and 2 is obtained slowly mix, and after stirring 1～2 hour under 50～100 ℃ the temperature condition, leave standstill, and oven dry obtains fluffy presoma;
4, place retort furnace to calcine presoma, temperature is 850～1000 ℃, and the time is 1～15 hour, naturally cools to room temperature, obtains a kind of material of realizing UV-light switching emission near infrared light.
A kind of in the oxide compound that the compound that contains ion R of the present invention is R, fluorochemical, the nitrate or their arbitrary combination; Contain ytterbium ion Yb
3+Compound be ytterbium oxide, fluoridize a kind of in ytterbium, the ytterbium nitrate or their arbitrary combination; The compound that contains ion M is a kind of in the oxide compound of M, fluorochemical, carbonate, vitriol, the nitrate or their arbitrary combination; Contain molybdenum ion Mo
6+Compound be a kind of in molybdenum oxide and the ammonium molybdate or their arbitrary combination.
Technical solution of the present invention provides a kind of application of material of UV-light switching emission near infrared light, uses it for the light-converting material of silica-based solar cell.
Compared with prior art, the present invention has following beneficial effect:
1, the material of UV-light switching emission near infrared light of the present invention, the emission main peak is positioned at 960nm～1100nm, the energy gap perfection of its energy and silicon is complementary, and can effectively improve the photoelectric transformation efficiency of silica-based solar cell, is potential silica-based solar cell rare earth light-converting material.
2, UV-light switching emission near infrared light material of the present invention, (250nm～400nm) have very strong absorption can improve solar energy utilization rate, weakens the heat effect of solar cell simultaneously in the ultraviolet region.
3, because the present invention calcines to make, need not to provide reducing atmosphere under air atmosphere, preparation technology is simple, does not have any pollution, and is environmentally friendly, and the stable performance of synthetic light-converting material.
Description of drawings
Fig. 1 is the embodiment of the invention 1 preparation sample BaGd
1.999Yb
0.001(MoO
4)
4The X-ray powder diffraction collection of illustrative plates;
Fig. 2 is the embodiment of the invention 1 preparation sample BaGd
1.999Yb
0.001(MoO
4)
4Exciting light spectrogram under the 1000nm wavelength monitor;
Fig. 3 is the embodiment of the invention 1 preparation sample BaGd
1.999Yb
0.001(MoO
4)
4Fluorescence spectrum figure under the 355nm wavelength excites;
Fig. 4 is the embodiment of the invention 2 preparation sample BaGd
1.7Yb
0.3(MoO
4)
4Exciting light spectrogram under the 1000nm wavelength monitor;
Fig. 5 is the embodiment of the invention 2 preparation sample BaGd
1.7Yb
0.3(MoO
4)
4Fluorescence spectrum figure under the 355nm wavelength excites;
Fig. 6 is the embodiment of the invention 3 preparation sample BaEu
1.99Yb
0.01(MoO
4)
4The X-ray powder diffraction collection of illustrative plates;
Fig. 7 is the embodiment of the invention 4 preparation sample BaY
1.9Yb
0.1(MoO
4)
4The X-ray powder diffraction collection of illustrative plates;
Fig. 8 is the embodiment of the invention 5 preparation sample BaLa
1.6Yb
0.4(MoO
4)
4The X-ray powder diffraction collection of illustrative plates.
Embodiment
Below in conjunction with drawings and Examples the present invention is further described.
Embodiment 1
According to chemical formula BaGd
1.999Yb
0.001(MoO
4)
4In the stoichiometric ratio of each element, take by weighing barium carbonate BaCO respectively
3: 0.387 gram, gadolinium sesquioxide Gd
2O
3: 1.812 grams, ytterbium oxide Yb
2O
3: 0.001 gram, ammonium molybdate (NH
4)
6MO
7O
24-4H
2The O:3.531 gram after grinding in agate mortar and mixing, selects air atmosphere to calcine for the first time, and temperature is 250 ℃, and calcination time 2 hours is chilled to room temperature then, takes out sample.After first time incinerating raw material, once more the compound thorough mixing is ground evenly, among air atmosphere, 650 ℃ of sintering for the second time down, sintering time is 6 hours, is cooled to room temperature, takes out sample.After second time incinerating raw material, once more the compound thorough mixing is ground evenly, among air atmosphere, sintering for the third time under 850 ℃, sintering time is 6 hours, is cooled to room temperature, take out the back and fully grinding promptly obtain sample.
Referring to accompanying drawing 1, be the X-ray powder diffraction collection of illustrative plates that the present embodiment technical scheme prepares sample; With the card 36-0192 of standard contrast, in full accord from the position of diffraction peak and relative intensity and standard card, illustrate that this routine prepared sample is pure thing phase.
Referring to accompanying drawing 2, be the excitation spectrum of sample under the 1000nm wavelength monitor by the preparation of present embodiment technical scheme; Referring to accompanying drawing 3, be the emmission spectrum figure of sample under the 355nm wavelength excites by the preparation of present embodiment technical scheme.As seen from the figure, the near-infrared luminous of 960nm～1100nm wave band appears in emmission spectrum, and obtained material effectively is converted to UV-light near-infrared luminous.
Embodiment 2
According to chemical formula BaGd
1.7Yb
0.3(MoO
4)
4In the stoichiometric ratio of each element, take by weighing barium carbonate BaCO respectively
3: 0.395 gram, gadolinium sesquioxide Gd
2O
3: 0.616 gram, ytterbium oxide Yb
2O
3: 0.118 gram, ammonium molybdate (NH
4)
6MO
7O
24-4H
2The O:1.412 gram after grinding in agate mortar and mixing, selects air atmosphere to calcine for the first time, and temperature is 350 ℃, and calcination time 6 hours is chilled to room temperature then, takes out sample.After first time incinerating raw material, once more the compound thorough mixing is ground evenly, among air atmosphere, 750 ℃ of sintering for the second time down, sintering time is 5 hours, is cooled to room temperature, takes out sample.After second time incinerating raw material, once more the compound thorough mixing is ground evenly, among air atmosphere, sintering for the third time under 900 ℃, sintering time is 9 hours, is cooled to room temperature, take out the back and fully grinding promptly obtain sample.
The X-ray powder diffraction collection of illustrative plates that the present embodiment technical scheme prepares sample is consistent with the sample of preparation among the embodiment 1.
Referring to accompanying drawing 4, be the excitation spectrum of sample under the 1000nm wavelength monitor by the preparation of present embodiment technical scheme; Referring to accompanying drawing 5, be the emmission spectrum figure of sample under the 355nm wavelength excites by the preparation of present embodiment technical scheme.As seen from the figure, the near-infrared luminous of 960nm ~ 1100nm wave band appears in emmission spectrum, and obtained material effectively is converted to UV-light near-infrared luminous.
Embodiment 3
According to chemical formula BaEu
1.99Yb
0.01(MoO
4)
4In the stoichiometric ratio of each element, take by weighing barium carbonate BaCO respectively
3: 0.395 gram, europium sesquioxide Eu
2O
3: 0.71 gram, ytterbium oxide Yb
2O
3: 0.0039 gram, ammonium molybdate (NH
4)
6MO
7O
24-4H
2The O:1.412 gram after grinding in agate mortar and mixing, selects air atmosphere to calcine for the first time, and temperature is 400 ℃, and calcination time 8 hours is chilled to room temperature then, takes out sample.After first time incinerating raw material, once more the compound thorough mixing is ground evenly, among air atmosphere, 700 ℃ of sintering for the second time down, sintering time is 7 hours, is cooled to room temperature, takes out sample.After second time incinerating raw material, once more the compound thorough mixing is ground evenly, among air atmosphere, sintering for the third time under 880 ℃, sintering time is 9 hours, is cooled to room temperature, take out the back and fully grinding promptly obtain sample.
Referring to accompanying drawing 6, be the X-ray powder diffraction collection of illustrative plates that the present embodiment technical scheme prepares sample, its excitation spectrum is similar with accompanying drawing 3 to accompanying drawing 2 respectively with emmission spectrum.
Embodiment 4
According to chemical formula BaY
1.9Yb
0.1(MoO
4)
4In the stoichiometric ratio of each element, take by weighing barium carbonate BaCO respectively
3: 0.395 gram, yttrium oxide Y
2O
3: 0.429 gram, ytterbium oxide Yb
2O
3: 0.039 gram, ammonium molybdate (NH
4)
6MO
7O
24-4H
2The O:1.412 gram after grinding in agate mortar and mixing, selects air atmosphere to calcine for the first time, and temperature is 450 ℃, and calcination time 9 hours is chilled to room temperature then, takes out sample.After first time incinerating raw material, once more the compound thorough mixing is ground evenly, among air atmosphere, 720 ℃ of sintering for the second time down, sintering time is 8 hours, is cooled to room temperature, takes out sample.After second time incinerating raw material, once more the compound thorough mixing is ground evenly, among air atmosphere, sintering for the third time under 890 ℃, sintering time is 10 hours, is cooled to room temperature, take out the back and fully grinding promptly obtain sample.
Referring to accompanying drawing 7, be the X-ray powder diffraction collection of illustrative plates that the present embodiment technical scheme prepares sample, its excitation spectrum is similar with accompanying drawing 3 to accompanying drawing 2 respectively with emmission spectrum.
Embodiment 5
According to chemical formula BaLa
1.6Yb
0.4(MoO
4)
4In the stoichiometric ratio of each element, take by weighing barium carbonate BaCO respectively
3: 0.395 gram, lanthanum trioxide La
2O
3: 0.521 gram, ytterbium oxide Yb
2O
3: 0.157 gram, ammonium molybdate (NH
4)
6MO
7O
24-4H
2The O:1.412 gram after grinding in agate mortar and mixing, selects air atmosphere to calcine for the first time, and temperature is 500 ℃, and calcination time 10 hours is chilled to room temperature then, takes out sample.After first time incinerating raw material, once more the compound thorough mixing is ground evenly, among air atmosphere, 750 ℃ of sintering for the second time down, sintering time is 7 hours, is cooled to room temperature, takes out sample.After second time incinerating raw material, once more the compound thorough mixing is ground evenly, sintering for the third time under among the air atmosphere 900 ℃, sintering time is 8 hours, is cooled to room temperature, take out the back and fully grinding promptly obtain sample.
Referring to accompanying drawing 8, be the X-ray powder diffraction collection of illustrative plates that the present embodiment technical scheme prepares sample, its excitation spectrum is similar with accompanying drawing 5 to accompanying drawing 4 respectively with emmission spectrum.
Embodiment 6
According to chemical formula BaErYb (MoO
4)
4In the stoichiometric ratio of each element, take by weighing barium carbonate BaCO respectively
3: 0.395 gram, Erbium trioxide Er
2O
3: 0.383 gram, ytterbium oxide Yb
2O
3: 0.394 gram, ammonium molybdate (NH
4)
6MO
7O
24-4H
2O:1.412 gram, and the citric acid of the 1.8wt% of above medicine total mass are with the barium carbonate BaCO that takes by weighing
3, Erbium trioxide Er
2O
3With ytterbium oxide Yb
2O
3Be dissolved in respectively in an amount of dilute nitric acid solution, with the ammonium molybdate (NH that takes by weighing
4)
6MO
7O
24-4H
2O is dissolved in deionized water or the ethanolic soln, adds proper amount of deionized water and citric acid respectively in 70 ℃ of stirrings; Then above-mentioned each solution is slowly mixed and constantly stirred 1.5 hours; Leave standstill, oven dry obtains fluffy precursor; Place retort furnace to calcine precursor, sintering temperature is 920 ℃, and calcination time is 10 hours, is cooled to room temperature, takes out also fully grinding and promptly obtains sample.Its XRD is consistent with accompanying drawing 1, and its excitation spectrum is similar with accompanying drawing 5 to accompanying drawing 4 respectively with emmission spectrum.
Embodiment 7
According to chemical formula BaBi
0.6Yb
1.4(MoO
4)
4In the stoichiometric ratio of each element, take by weighing barium carbonate BaCO respectively
3: 0.395 gram, bismuth oxide Bi
2O
3: 0.279 gram, ytterbium oxide Yb
2O
3: 0.552 gram, ammonium molybdate (NH
4)
6MO
7O
24-4H
2The O:1.412 gram after grinding in agate mortar and mixing, selects air atmosphere to calcine for the first time, and temperature is 550 ℃, and calcination time 10 hours is chilled to room temperature then, takes out sample.After first time incinerating raw material, once more the compound thorough mixing is ground evenly, among air atmosphere, 780 ℃ of sintering for the second time down, sintering time is 9 hours, is cooled to room temperature, takes out sample.After second time incinerating raw material, once more the compound thorough mixing is ground evenly, sintering for the third time under among the air atmosphere 930 ℃, sintering time is 10 hours, is cooled to room temperature, take out and fully grinding promptly obtain sample.Its XRD is consistent with accompanying drawing 1, and excitation spectrum is similar with accompanying drawing 3 to accompanying drawing 2 respectively with emmission spectrum.
Embodiment 8
According to chemical formula BaDy
0.2Yb
1.8(MoO
4)
4In the stoichiometric ratio of each element, take by weighing barium carbonate BaCO respectively
3: 0.395 gram, dysprosium oxide Dy
2O
3: 0.074 gram, ytterbium oxide Yb
2O
3: 0.709 gram, ammonium molybdate (NH
4)
6MO
7O
24-4H
2O:1.412 gram, and the citric acid of the 1.8wt% of above medicine total mass are with the barium carbonate BaCO that takes by weighing
3, dysprosium oxide Dy
2O
3With ytterbium oxide Yb
2O
3Be dissolved in respectively in an amount of dilute nitric acid solution, with the ammonium molybdate (NH that takes by weighing
4)
6MO
7O
24-4H
2O is dissolved in deionized water or the ethanolic soln, adds proper amount of deionized water and citric acid respectively in 70 ℃ of stirrings; Then above-mentioned solution is slowly mixed and constantly stirred 2 hours; Leave standstill, oven dry obtains fluffy precursor; Place retort furnace to calcine precursor, sintering temperature is 950 ℃, and calcination time is 10 hours, is cooled to room temperature, takes out the also abundant grinding in back and promptly obtains sample.Its XRD is consistent with accompanying drawing 1, and excitation spectrum is similar with accompanying drawing 5 to accompanying drawing 4 respectively with emmission spectrum.
Claims (9)
1. the material of a UV-light switching emission near infrared light is characterized in that: it under the ultraviolet excitation of 250nm～400nm, the near infrared light of emission 950nm～1100nm; The chemical general formula of described material is MR
2-2xYb
2x(MoO
4)
4, wherein, R is rare earth erbium ion Er
3+, europium ion Eu
3+, lanthanum ion La
3+, ruthenium ion Y
3+, cerium ion Ce
3+, thulium ion Tm
3+, praseodymium ion Pr
3+, neodymium ion Nd
3+, samarium ion Sm
3+, gadolinium ion Gd
3+, terbium ion Tb
3+, dysprosium ion Dy
3+, holmium ion Ho
3+, lutetium ion Lu
3+In a kind of or their arbitrary combination; M is alkaline-earth metal ions calcium ion Ca
2+, strontium ion Sr
2+, barium ion Ba
2+In a kind of or their arbitrary combination;
xBe Yb
3+Adulterated molecular fraction, 0.0001≤x≤1.0.
2. the preparation methods of a UV-light switching emission near infrared light as claimed in claim 1 adopts high temperature solid-state method, it is characterized in that comprising the steps:
Press chemical formula MR
2-2xYb
2x(MoO
4)
4In the stoichiometric ratio of each element, wherein 0.0001≤x≤1.0 take by weighing respectively and contain ytterbium ion Yb
3+Compound, contain ion
RCompound, contain ion
MCompound, contain molybdenum ion Mo
6+Compound, grind and mix, obtain mixture; Described ion R is rare earth erbium ion Er
3+, europium ion Eu
3+, lanthanum ion La
3+, ruthenium ion Y
3+, cerium ion Ce
3+, thulium ion Tm
3+, praseodymium ion Pr
3+, neodymium ion Nd
3+, samarium ion Sm
3+, gadolinium ion Gd
3+, terbium ion Tb
3+, dysprosium ion Dy
3+, holmium ion Ho
3+, lutetium ion Lu
3+In a kind of or their arbitrary combination; Described ion M is alkaline-earth metal ions calcium ion Ca
2+, strontium ion Sr
2+, barium ion Ba
2+In a kind of or their arbitrary combination;
The mixture that step (1) obtains is calcined under air atmosphere 1～2 time; Described calcining temperature is 200～600 ℃, and calcination time is 1～12 hour;
With the mixture naturally cooling that step (2) obtains, after grinding and mixing, in air atmosphere, to calcine, calcining temperature is 600～850 ℃, calcination time is 1～12 hour;
With the mixture naturally cooling that step (3) obtains, after grinding and mixing, in air atmosphere, calcine, calcining temperature is 850～1000 ℃, calcination time is 1～12 hour, naturally cools to room temperature, obtains a kind of material of UV-light switching emission near infrared light.
3. according to claims 2 described a kind of preparation methods that realize UV-light switching emission near infrared light, it is characterized in that: the calcining temperature of step (2) is 250～550 ℃, and calcination time is 2～10 hours.
4. according to claims 2 described a kind of preparation methods that realize UV-light switching emission near infrared light, it is characterized in that: the calcining temperature of step (3) is 650～800 ℃, and calcination time is 2～10 hours.
5. according to claims 2 described a kind of preparation methods that realize UV-light switching emission near infrared light, it is characterized in that: the calcining temperature of step (4) is 850～950 ℃, and calcination time is 2～10 hours.
6. according to the preparation methods of claims 2 described a kind of UV-light switching emission near infrared lights, it is characterized in that: a kind of in the oxide compound that the described compound that contains ion R is R, fluorochemical, the nitrate or their arbitrary combination; Contain ytterbium ion Yb
3+Compound be ytterbium oxide, fluoridize a kind of in ytterbium, the ytterbium nitrate or their arbitrary combination; The compound that contains ion M is a kind of in the oxide compound of M, fluorochemical, carbonate, vitriol, the nitrate or their arbitrary combination; Contain molybdenum ion Mo
6+Compound be a kind of in molybdenum oxide and the ammonium molybdate or their arbitrary combination.
7. the preparation methods of a UV-light switching emission near infrared light as claimed in claim 1 adopts chemical synthesis, it is characterized in that comprising the steps:
Press chemical formula MR
2-2xYb
2x(MoO
4)
4In the stoichiometric ratio of each element, wherein 0.0001≤x≤1.0 take by weighing and contain ytterbium ion Yb
3+Compound, contain ion R compound, contain the compound of ion M, they are dissolved in respectively in the dilute nitric acid solution, obtain various clear solutions; 0.5～2.0wt% by each reactant quality adds complexing agent citric acid or oxalic acid respectively, stirs under 50～100 ℃ temperature condition; Described ion R is rare earth erbium ion Er
3+, europium ion Eu
3+, lanthanum ion La
3+, ruthenium ion Y
3+, cerium ion Ce
3+, thulium ion Tm
3+, praseodymium ion Pr
3+, neodymium ion Nd
3+, samarium ion Sm
3+, gadolinium ion Gd
3+, terbium ion Tb
3+, dysprosium ion Dy
3+, holmium ion Ho
3+, lutetium ion Lu
3+In a kind of or their arbitrary combination; Described ion M is alkaline-earth metal ions calcium ion Ca
2+, strontium ion Sr
2+, barium ion Ba
2+In a kind of or their arbitrary combination; Take by weighing respectively and contain ytterbium ion Yb
3+Compound, contain rare earth ion R compound, contain the compound of alkaline-earth metal ions M;
Press chemical formula MR
2-2xYb
2x(MoO
4)
4In the stoichiometric ratio of each element, wherein 0.0001≤x≤1.0 take by weighing and contain molybdenum ion Mo
6+Compound, be dissolved in deionized water or the ethanolic soln, the 0.5～2.0wt% that presses the reactant quality adds complexing agent citric acid or oxalic acid, stirs under 50～100 ℃ temperature condition;
The various solution that step (1) and (2) are obtained slowly mix, and after stirring 1～2 hour under 50～100 ℃ the temperature condition, leave standstill, and oven dry obtains fluffy presoma;
Place retort furnace to calcine presoma, temperature is 850～1000 ℃, and the time is 1～15 hour, naturally cools to room temperature, obtains a kind of material of realizing UV-light switching emission near infrared light.
8. according to the preparation methods of claims 7 described a kind of UV-light switching emission near infrared lights, it is characterized in that: a kind of in the oxide compound that the described compound that contains ion R is R, fluorochemical, the nitrate or their arbitrary combination; Contain ytterbium ion Yb
3+Compound be ytterbium oxide, fluoridize a kind of in ytterbium, the ytterbium nitrate or their arbitrary combination; The compound that contains ion M is a kind of in the oxide compound of M, fluorochemical, carbonate, vitriol, the nitrate or their arbitrary combination; Contain molybdenum ion Mo
6+Compound be a kind of in molybdenum oxide and the ammonium molybdate or their arbitrary combination.
9. the application of the material of a UV-light switching emission near infrared light as claimed in claim 1 is characterized in that: the light-converting material that is used for silica-based solar cell.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103834400A (en) * | 2014-03-13 | 2014-06-04 | 重庆理工大学 | Calcium tungstate fluorescent powder and preparation method thereof |
| CN104673308A (en) * | 2015-02-02 | 2015-06-03 | 江苏师范大学 | Material for realizing near-infrared luminescence under ultraviolet excitation and preparation method thereof |
| CN109652011A (en) * | 2019-01-21 | 2019-04-19 | 广东工业大学 | Ultraviolet-near infrared absorption material of one kind and the preparation method and application thereof |
-
2013
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Non-Patent Citations (1)
| Title |
|---|
| HAIYAN DU ET.AL.: "《Synthesis and upconversion luminescence properties of Yb3+/Er3+ codoped BaGd2(MoO4)4 powder》", 《MATERIALS RESEARCH BULLETIN》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103834400A (en) * | 2014-03-13 | 2014-06-04 | 重庆理工大学 | Calcium tungstate fluorescent powder and preparation method thereof |
| CN103834400B (en) * | 2014-03-13 | 2015-06-17 | 重庆理工大学 | Calcium tungstate fluorescent powder and preparation method thereof |
| CN104673308A (en) * | 2015-02-02 | 2015-06-03 | 江苏师范大学 | Material for realizing near-infrared luminescence under ultraviolet excitation and preparation method thereof |
| CN104673308B (en) * | 2015-02-02 | 2017-02-22 | 江苏师范大学 | Material for realizing near-infrared luminescence under ultraviolet excitation and preparation method thereof |
| CN109652011A (en) * | 2019-01-21 | 2019-04-19 | 广东工业大学 | Ultraviolet-near infrared absorption material of one kind and the preparation method and application thereof |
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