CN102942929A - A borotungstate up-conversion luminescent material activated by ytterbium ion Yb3+ and its preparation method - Google Patents
A borotungstate up-conversion luminescent material activated by ytterbium ion Yb3+ and its preparation method Download PDFInfo
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- CN102942929A CN102942929A CN201210503031XA CN201210503031A CN102942929A CN 102942929 A CN102942929 A CN 102942929A CN 201210503031X A CN201210503031X A CN 201210503031XA CN 201210503031 A CN201210503031 A CN 201210503031A CN 102942929 A CN102942929 A CN 102942929A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 59
- 239000000463 material Substances 0.000 title claims abstract description 48
- 229910052769 Ytterbium Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 238000004020 luminiscence type Methods 0.000 claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract 2
- -1 ytterbium ions Chemical class 0.000 claims description 89
- 238000001354 calcination Methods 0.000 claims description 63
- 150000001875 compounds Chemical class 0.000 claims description 50
- 239000012298 atmosphere Substances 0.000 claims description 42
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 229910052796 boron Inorganic materials 0.000 claims description 19
- 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 15
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 15
- 229940075624 ytterbium oxide Drugs 0.000 claims description 15
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- 239000004327 boric acid Substances 0.000 claims description 13
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 13
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 13
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- 150000002500 ions Chemical class 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
- 239000010937 tungsten Substances 0.000 claims description 7
- 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
- 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
- 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
- 239000008139 complexing agent Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052810 boron oxide Inorganic materials 0.000 claims description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical group [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
- 229910052727 yttrium Inorganic materials 0.000 claims 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 2
- 229910052731 fluorine Inorganic materials 0.000 claims 2
- 239000011737 fluorine Substances 0.000 claims 2
- ZVTQDOIPKNCMAR-UHFFFAOYSA-N sulfanylidene(sulfanylideneboranylsulfanyl)borane Chemical compound S=BSB=S ZVTQDOIPKNCMAR-UHFFFAOYSA-N 0.000 claims 2
- 230000005284 excitation Effects 0.000 abstract description 21
- 238000009776 industrial production Methods 0.000 abstract 1
- 150000002910 rare earth metals Chemical group 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 49
- 239000000523 sample Substances 0.000 description 38
- 238000000227 grinding Methods 0.000 description 35
- 239000002994 raw material Substances 0.000 description 24
- 238000002156 mixing Methods 0.000 description 15
- 238000005303 weighing Methods 0.000 description 14
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 10
- 239000000843 powder Substances 0.000 description 9
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 238000010304 firing Methods 0.000 description 8
- 239000004570 mortar (masonry) Substances 0.000 description 8
- 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 7
- 238000005516 engineering process Methods 0.000 description 6
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 3
- 238000001748 luminescence spectrum Methods 0.000 description 3
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 description 2
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- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000005281 excited state Effects 0.000 description 2
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 2
- 230000005283 ground state Effects 0.000 description 2
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- 230000018199 S phase Effects 0.000 description 1
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- 229910021644 lanthanide ion Inorganic materials 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 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
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Abstract
本发明公开了一种镱离子Yb3+激活的硼钨酸盐上转换发光材料及制备。其化学组成由通式R3-3xYb3xBWO9表示，其中，R为稀土Er3+、Eu3+、La3+、Y3+、Ce3+、Tm3+、Pr3+、Nd3+、Sm3+、Gd3+、Tb3+中的一种或多种；x为Yb3+掺杂的摩尔百分数，0.0001<x≤1.0。本发明提供的上转换发光材料采用高温固相法或化学合成法制得，材料的化学纯度高，发光质量好，性能稳定，在975纳米的红外激光激发下，能够实现绿色的上转换发光，且材料的发光强度随着激发二极管能量强度的增强而增大。材料的制备工艺简单、无污染，适合于工业化生产。
The invention discloses a borotungstate up-conversion luminescent material activated by ytterbium ion Yb 3+ and its preparation. Its chemical composition is represented by the general formula R 3-3x Yb 3x BWO 9 , wherein R is rare earth Er 3+ , Eu 3+ , La 3+ , Y 3+ , Ce 3+ , Tm 3+ , Pr 3+ , Nd One or more of 3+ , Sm 3+ , Gd 3+ , Tb 3+ ; x is the mole percentage of Yb 3+ doping, 0.0001<x≤1.0. The up-conversion luminescent material provided by the present invention is prepared by a high-temperature solid-phase method or a chemical synthesis method. The material has high chemical purity, good luminous quality, and stable performance. It can realize green up-conversion luminescence under the excitation of a 975-nm infrared laser, and The luminous intensity of the material increases with the increase of the energy intensity of the excitation diode. The preparation process of the material is simple and pollution-free, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of luminescent material and preparation method thereof, particularly a kind of ytterbium ion Yb
3+Boron tungstate up-conversion luminescent material that activates and preparation method thereof is used, and belongs to luminescent material and preparation technology field thereof in the shiner Neo-Confucianism.
Background technology
Up-conversion luminescence refers in the excitation process of photoluminescence, produces short wavelength's light emission under the exciting of long wavelength light.Up-conversion luminescent material is a kind of important functional materials, the special property that it has makes it have broad application prospects in laser technology, optical fiber communication technology, fluorescent probe, 3 D stereo demonstration, infrared detection technique and the numerous areas such as false proof, so the good up-conversion luminescent material of processability has very great meaning.
Up-conversion generally includes activator, sensitizing agent and matrix.Because rare earth ytterbium ion Yb
3+Ground state is only arranged
2F
7/2And excited state
2F
5/2Two isolated energy levels, about 10000cm of being separated by
-1, its absorption band is wider, generally has characteristic light to absorb in 0.1～1.0 micron wave length scope, can with InGaAs semiconductor pumping sources efficient coupling, pumping wavelength and laser output wavelength are close, and fluorescence efficiency is very high, are the good active ions of a kind of luminescent properties.
Rare earth ytterbium ion Yb
3+Electronic configuration be 4f
13, because lanthanide contraction is compared with other lanthanide ions, the suffered shielding in this system of its 4f electronics is less, thereby the interaction stronger with the easy generation of lattice and neighbour's ion on every side, so mixing Yb
3+Laserable material in easily produce cooperative Luminescence.Nakazawa E in 1970 and Shinonnya S in the literature (Phys. Rev. Lett. 25,1710 – 1712 (1970)) reported first Yb
3+Ion is at YbPO
4The cooperation up-conversion luminescence behavior of middle blue green light wave band.Its up-conversion luminescence behavior is by the Yb of two close together that are in excited state
3+The mutual coupling of ion and while de excitation are dealt into ground state and realize.This peculiar up-conversion luminescence is got back in follow-up developments and is further studied, and M. Malinowski etc. has discussed Yb in document (Journal of Luminescence 94 – 95 (2001) 29 – 33)
3+: the blue cooperation up-conversion luminescence of YAG system, Degang Deng and Shiqing Xu etc. has reported Yb in document (J. Phys. D:Appl. Phys. 42 (2009) 105111)
3+The blue cooperation up-conversion luminescence of the devitrified glass that contains LiYF4 that mixes.
At present, up-conversion luminescent material can be used for developing the quick calculating of light and the new optical devices such as optical bistability and blue green light wave band of laser device.Offer Zang Jingcun, the Yb of the report in document ([J] laser and infrared, in June, 2002, the 3rd phase of the 32nd volume) such as Gong Feng
3+: YAG, Yb
3+: BCa
5(PO
4)
3The laser crystalss such as F, quantum yield is high, is suitable for InGaAs laser diode-pumped, generation can be applicable to the lidar in atmospheric layer space from the frequency multiplication visible laser, underwater lighting and detection, telemetering pickup, pharmaceutical chemicals detector, making sheet and materials processing etc.In addition, Yb is mixed in the application aspect new pattern laser material and fiber-optic signal transmission
3+Laserable material be regarded as developing a main path efficient, superpower laser.Therefore, to Yb
3+The research of ion-activated up-conversion luminescent material is one and has the work that scientific meaning has again bright prospects.
Six side's phase NaYF
4Be the upper the highest substrate material of transformation efficiency in the up-conversion of having studied at present, but its synthesis temperature that needs is higher, and can be to environment.But by comparison, Preparation is simple, stable performance, and cost is lower.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, provide a kind of chemical purity high, luminous mass is good, and simple, the free of contamination boron tungstate up-conversion luminescent material of preparation technology and preparation method thereof.
For reaching above purpose, the technical solution used in the present invention provides a kind of ytterbium ion Yb
3+The boron tungstate up-conversion luminescent material that activates, its chemical formula is R
3-3xYb
3xBWO
9, 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+In a kind of, or their arbitrary combination;
xBe ytterbium ion Yb
3+The molecular fraction of mixing, 0.0001＜x≤1.0; Described up-conversion luminescent material is under the infrared laser pumping of 975 nanometers, and obtaining wavelength is the green up-conversion luminescence of 530～560 nanometers.
A kind of aforesaid ytterbium ion Yb
3+The preparation method of the boron tungstate up-conversion luminescent material that activates adopts high temperature solid-state method, comprises the steps:
(1) presses chemical formula R
3-3xYb
3xBWO
9In the stoichiometric ratio of each element, take by weighing respectively and contain ytterbium ion Yb
3+Compound, contain rare earth ion R compound, contain boron ion B
3+Compound, contain tungsten ion W
6+Compound, grind and mix, obtain mixture; 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+In a kind of, or their arbitrary combination;
xBe ytterbium ion Yb
3+The molecular fraction of mixing, 0.0001＜x≤1.0;
(2) mixture is calcined under air atmosphere 1～2 time, calcining temperature is 200～600 ℃, and calcination time is 1～15 hour;
(3) the mixture naturally cooling that step (2) is obtained after grinding and mixing, is calcined in air atmosphere, and calcining temperature is 600～800 ℃, and calcination time is 1～15 hour;
(4) the mixture naturally cooling that step (3) is obtained after grinding and mixing, is calcined in air atmosphere, and calcining temperature is 800～1000 ℃, and calcination time is 1～15 hour;
(5) the mixture naturally cooling that step (4) is obtained after grinding and mixing, is calcined in air atmosphere, and calcining temperature is 1000～1300 ℃, and calcination time is 1～15 hour, naturally cools to room temperature, obtains a kind of ytterbium ion Yb
3+The boron tungstate up-conversion luminescent material that activates.
Adopt high temperature solid-state method to prepare ytterbium ion Yb
3+The preferred version of the boron tungstate up-conversion luminescent material that activates is: the calcining temperature of step (2) is 250～550 ℃, and calcination time is 2～12 hours; The calcining temperature of step (3) is 600～750 ℃, and calcination time is 2～12 hours; The calcining temperature of step (4) is 800～950 ℃, and calcination time is 2～12 hours; The calcining temperature of step (5) is 1000～1250 ℃, and calcination time is 2～12 hours.
Technical solution of the present invention also provides a kind of employing chemical synthesis to prepare described ytterbium ion Yb
3+The boron tungstate up-conversion luminescent material that activates comprises the steps:
(1) presses chemical formula R
3-3xYb
3xBWO
9In the stoichiometric ratio of each element, take by weighing and contain ytterbium ion Yb
3+Compound, contain rare earth ion R compound, contain tungsten ion W
6+Compound, they are dissolved in respectively in the dilute nitric acid solution, obtain the clear solution of various elements; 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+In a kind of, or their arbitrary combination;
xBe ytterbium ion Yb
3+The molecular fraction of mixing, 0.0001＜x≤1.0; 0.5～2.0wt% by each reactant quality adds respectively complexing agent citric acid or oxalic acid again, stirs under 50～100 ℃ temperature condition;
(2) press chemical formula R
3-3xYb
3xBWO
9Middle boron ion B
3+The stoichiometric ratio of element takes by weighing and contains boron ion B
3+Compound, it is dissolved in deionized water or the ethanolic soln, obtain solution; 0.5～the 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) 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, calcining temperature is 1000～1300 ℃, and calcination time is 1～15 hour, naturally cools to room temperature, obtains a kind of ytterbium ion Yb
3+The boron tungstate up-conversion luminescent material that activates.
The ytterbium ion Yb that contains of the present invention
3+Compound be ytterbium oxide, fluoridize a kind of in ytterbium, the ytterbium nitrate or their arbitrary combination; The described boron ion B that contains
3+Compound be a kind of in boron oxide, boron nitride, sulfuration boron, the boric acid, or their arbitrary combination; The described tungsten ion W that contains
6+Compound be a kind of in Tungsten oxide 99.999, the ammonium tungstate, or their arbitrary combination.
Compared with prior art, the advantage of technical solution of the present invention is:
1, the present invention utilizes ytterbium ion Yb
3+Between unique upper conversion behavior, realized the preparation of up-conversion luminescent material, under the 975nm infrared laser light source, material can be realized green up-conversion luminescence, and luminosity is high, stable luminescent property has broad application prospects at aspects such as photoelectronics, laser technology, high-density storage, laser anti-counterfeits.
2, compare with other up-conversion luminescent material take fluorochemical as matrix, the preparation process of substrate material of the present invention is without any pollution, and preparation process is simple, and the product easily collecting is without the waste water and gas discharging, environmentally friendly.
3, because the present invention calcines to make, need not to provide reducing atmosphere, so operating process is simple in air atmosphere, lower to the requirement of equipment, can reduce production costs, and synthetic up-conversion luminescent material stable performance.
Description of drawings
Fig. 1 is sample Yb in the embodiment of the invention 1
2.85Eu
0.15BWO
9The X-ray powder diffraction collection of illustrative plates and the comparison of standard card PDF#51-0101;
Fig. 2 is the embodiment of the invention 1 preparation sample Yb
2.85Eu
0.15BWO
9It is 0.998 watt the infrared ray excited lower up-conversion luminescence spectrogram that obtains in 975nm, excitation energy intensity;
Fig. 3 is the embodiment of the invention 2 preparation sample Yb
2.7Eu
0.3BWO
9It is 0.998 watt the infrared ray excited lower up-conversion luminescence spectrogram that obtains in 975nm, excitation energy intensity;
Fig. 4 is the embodiment of the invention 4 preparation sample Yb
2.4Eu
0.6BWO
9The infrared ray excited lower up-conversion luminescence spectrogram that obtains in 975nm, different excitation energy intensity;
Fig. 5 is the embodiment of the invention 5 preparation sample Yb
2.1Eu
0.9BWO
9The infrared ray excited lower up-conversion luminescence spectrogram that obtains in 975nm, different excitation energy intensity;
Fig. 6 is the embodiment of the invention 7 preparation sample Yb
1.2Eu
1.8BWO
9It is 0.998 watt the infrared ray excited lower up-conversion luminescence spectrogram that obtains in 975nm, excitation energy intensity;
Fig. 7 is the embodiment of the invention 9 preparation sample Yb
0.6Eu
2.4BWO
9The infrared ray excited lower up-conversion luminescence spectrogram that obtains in 975nm, different excitation energy intensity.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1
According to chemical formula Yb
2.85Eu
0.15BWO
9The stoichiometric ratio of each element in 975nm takes by weighing respectively ytterbium oxide Yb
2O
3: 1.404 grams, europium sesquioxide Eu
2O
3: 0.066 gram, boric acid H
3BO
3: 0.1623 gram, Tungsten oxide 99.999 WO
3: 0.597 gram, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 550 ℃, then calcination time 7 hours is chilled to room temperature, takes out sample.After the raw material of for the first time calcining, again even the abundant mixed grinding of compound, among air atmosphere, 750 ℃ of lower for the second time sintering, sintering time is 10 hours, is cooled to room temperature, takes out sample.After the raw material of for the second time calcining, again even the abundant mixed grinding of compound, among air atmosphere, sintering for the third time under 950 ℃, sintering time is 8 hours, is cooled to room temperature, takes out sample.After the raw material of third firing, again even the abundant mixed grinding of compound, among air atmosphere, 1250 ℃ of lower the 4th sintering, sintering time is 10 hours, is cooled to room temperature, namely obtains pulverous upconversion fluorescent powder.
Referring to accompanying drawing 1, be the X-ray powder diffraction collection of illustrative plates that the present embodiment technical scheme prepares sample, PDF#51-0101 is in full accord with standard card.
Referring to accompanying drawing 2, to be 0.998 watt infrared ray excited lower up-conversion luminescence spectrum in 975nm, excitation energy intensity by the sample of the present embodiment technical scheme preparation, as seen from Figure 2, this material emission main peak is green up-conversion luminescence near 540 nanometers.
Embodiment 2
According to chemical formula Yb
2.7Eu
0.3BWO
9The stoichiometric ratio of each element in 975nm takes by weighing respectively ytterbium oxide Yb
2O
3: 1.33 grams, europium sesquioxide Eu
2O
3: 0.132 gram, boric acid H
3BO
3: 0.1623 gram, Tungsten oxide 99.999 WO
3: 0.597 gram, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 500 ℃, then calcination time 6 hours is chilled to room temperature, takes out sample.After the raw material of for the first time calcining, again even the abundant mixed grinding of compound, among air atmosphere, 700 ℃ of lower for the second time sintering, sintering time is 8 hours, is cooled to room temperature, takes out sample.After the raw material of for the second time calcining, again even the abundant mixed grinding of compound, among air atmosphere, sintering for the third time under 900 ℃, sintering time is 10 hours, is cooled to room temperature, takes out sample.After the raw material of third firing, again even the abundant mixed grinding of compound, among air atmosphere, 1200 ℃ of lower the 4th sintering, sintering time is 10 hours, is cooled to room temperature, namely obtains pulverous upconversion fluorescent powder.Its XRD diffraction spectrogram and accompanying drawing 1 are approximate.
Referring to accompanying drawing 3, that sample by the present embodiment technical scheme preparation is 0.998 watt the infrared ray excited lower up-conversion luminescence spectrum that obtains in 975nm, excitation energy intensity, as seen from Figure 3, this material emission main peak is green up-conversion luminescence near 540 nanometers.
Embodiment 3
According to chemical formula Yb
2.55Y
0.45BWO
9The stoichiometric ratio of each element in 975nm takes by weighing respectively ytterbium oxide Yb
2O
3: 1.256 grams, yttrium oxide Y
2O
3: 0.127 gram, boric acid H
3BO
3: 0.1623 gram, Tungsten oxide 99.999 WO
3: 0.597 gram, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 400 ℃, then calcination time 5 hours is chilled to room temperature, takes out sample.After the raw material of for the first time calcining, again even the abundant mixed grinding of compound, among air atmosphere, 680 ℃ of lower for the second time sintering, sintering time is 8 hours, is cooled to room temperature, takes out sample.After the raw material of for the second time calcining, again even the abundant mixed grinding of compound, among air atmosphere, sintering for the third time under 860 ℃, sintering time is 9 hours, is cooled to room temperature, takes out sample.After the raw material of third firing, again even the abundant mixed grinding of compound, among air atmosphere, 1150 ℃ of lower the 4th sintering, sintering time is 12 hours, is cooled to room temperature, namely obtains pulverous upconversion fluorescent powder.Its XRD diffraction spectrogram and accompanying drawing 1 are approximate, and its excitation spectrum and accompanying drawing 3 are approximate.
Embodiment 4
According to chemical formula Yb
2.4Eu
0.6BWO
9The stoichiometric ratio of each element in 975nm takes by weighing respectively ytterbium oxide Yb
2O
3: 1.182 grams, europium sesquioxide Eu
2O
3: 0.264 gram, boric acid H
3BO
3: 0.1623 gram, Tungsten oxide 99.999 WO
3: 0.597 gram, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 350 ℃, then calcination time 5 hours is chilled to room temperature, takes out sample.After the raw material of for the first time calcining, again even the abundant mixed grinding of compound, among air atmosphere, 650 ℃ of lower for the second time sintering, sintering time is 7 hours, is cooled to room temperature, takes out sample.After the raw material of for the second time calcining, again even the abundant mixed grinding of compound, among air atmosphere, sintering for the third time under 850 ℃, sintering time is 9 hours, is cooled to room temperature, takes out sample.After the raw material of third firing, again even the abundant mixed grinding of compound, among air atmosphere, 1100 ℃ of lower the 4th sintering, sintering time is 10 hours, is cooled to room temperature, namely obtains pulverous upconversion fluorescent powder.Its XRD diffraction spectrogram and accompanying drawing 1 are approximate.
Referring to accompanying drawing 4, by the sample of the present embodiment technical scheme preparation infrared ray excited lower up-conversion luminescence spectrogram that obtains in 975nm, different excitation energy intensity, as seen from Figure 4, the luminous intensity of this material increases along with the enhancing of excitation diode energy intensity.
Embodiment 5
According to chemical formula Yb
2.1Eu
0.9BWO
9The stoichiometric ratio of each element in 975nm takes by weighing respectively ytterbium oxide Yb
2O
3: 1.035 grams, europium sesquioxide Eu
2O
3: 0.396 gram, boric acid H
3BO
3: 0.1623 gram, Tungsten oxide 99.999 WO
3: 0.597 gram, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 320 ℃, then calcination time 4 hours is chilled to room temperature, takes out sample.After the raw material of for the first time calcining, again even the abundant mixed grinding of compound, among air atmosphere, 630 ℃ of lower for the second time sintering, sintering time is 8 hours, is cooled to room temperature, takes out sample.After the raw material of for the second time calcining, again even the abundant mixed grinding of compound, among air atmosphere, sintering for the third time under 830 ℃, sintering time is 8 hours, is cooled to room temperature, takes out sample.After the raw material of third firing, again even the abundant mixed grinding of compound, among air atmosphere, 1080 ℃ of lower the 4th sintering, sintering time is 12 hours, is cooled to room temperature, namely obtains pulverous upconversion fluorescent powder.Its XRD diffraction spectrogram and accompanying drawing 1 are approximate.
Referring to accompanying drawing 5, by the sample of the present embodiment technical scheme preparation infrared ray excited lower up-conversion luminescence spectrogram that obtains in 975nm, different excitation energy intensity, as seen from Figure 5, the luminous intensity of this material increases along with the enhancing of excitation diode energy intensity.
Embodiment 6
According to chemical formula Yb
1.8Ga
1.2BWO
9The stoichiometric ratio of each element in 975nm takes by weighing respectively ytterbium oxide Yb
2O
3: 1.035 grams, gadolinium sesquioxide Ga
2O
3: 0.489 gram, boric acid H
3BO
3: 0.1623 gram, Tungsten oxide 99.999 WO
3: 0.597 gram, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 310 ℃, then calcination time 3 hours is chilled to room temperature, takes out sample.After the raw material of for the first time calcining, again even the abundant mixed grinding of compound, among air atmosphere, 630 ℃ of lower for the second time sintering, sintering time is 9 hours, is cooled to room temperature, takes out sample.After the raw material of for the second time calcining, again even the abundant mixed grinding of compound, among air atmosphere, sintering for the third time under 840 ℃, sintering time is 5 hours, is cooled to room temperature, takes out sample.After the raw material of third firing, again even the abundant mixed grinding of compound, among air atmosphere, 1100 ℃ of lower the 4th sintering, sintering time is 11 hours, is cooled to room temperature, namely obtains pulverous upconversion fluorescent powder.Its XRD diffraction spectrogram and accompanying drawing 1 is approximate, and the up-conversion luminescence spectrogram under its different excitation energy intensity infrared ray excited is similar to accompanying drawing 5.
Embodiment 7
According to chemical formula Yb
1.2Eu
1.8BWO
9The stoichiometric ratio of each element in 975nm takes by weighing respectively ytterbium oxide Yb
2O
3: 0.591 gram, europium sesquioxide Eu
2O
3: 0.792 gram, boric acid H
3BO
3: 0.1623 gram, Tungsten oxide 99.999 WO
3: 0.597 gram, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 300 ℃, then calcination time 5 hours is chilled to room temperature, takes out sample.After the raw material of for the first time calcining, again even the abundant mixed grinding of compound, among air atmosphere, 620 ℃ of lower for the second time sintering, sintering time is 8 hours, is cooled to room temperature, takes out sample.After the raw material of for the second time calcining, again even the abundant mixed grinding of compound, among air atmosphere, sintering for the third time under 810 ℃, sintering time is 10 hours, is cooled to room temperature, takes out sample.After the raw material of third firing, again even the abundant mixed grinding of compound, among air atmosphere, 1050 ℃ of lower the 4th sintering, sintering time is 10 hours, is cooled to room temperature, namely obtains pulverous upconversion fluorescent powder.Its XRD diffraction spectrogram and accompanying drawing 1 are approximate.
Referring to accompanying drawing 6, that sample by the present embodiment technical scheme preparation is 0.998 watt the infrared ray excited lower up-conversion luminescence spectrum that obtains in 975nm, excitation energy intensity, as seen from Figure 6, this material emission main peak is green up-conversion luminescence near 530 nanometers.
Embodiment 8
According to chemical formula Yb
0.9La
2.1BWO
9The stoichiometric ratio of each element in 975nm takes by weighing respectively ytterbium oxide Yb
2O
3: 0.444 gram, lanthanum trioxide La
2O
3: 0.855 gram, boric acid H
3BO
3: 0.1623 gram, Tungsten oxide 99.999 WO
3: 0.597 gram, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 280 ℃, then calcination time 6 hours is chilled to room temperature, takes out sample.After the raw material of for the first time calcining, again even the abundant mixed grinding of compound, among air atmosphere, 610 ℃ of lower for the second time sintering, sintering time is 8 hours, is cooled to room temperature, takes out sample.After the raw material of for the second time calcining, again even the abundant mixed grinding of compound, among air atmosphere, sintering for the third time under 825 ℃, sintering time is 9 hours, is cooled to room temperature, takes out sample.After the raw material of third firing, again even the abundant mixed grinding of compound, among air atmosphere, 1050 ℃ of lower the 4th sintering, sintering time is 12 hours, is cooled to room temperature, namely obtains pulverous upconversion fluorescent powder.Its XRD diffraction spectrogram and accompanying drawing 1 is approximate, and the up-conversion luminescence spectrogram under its different excitation energy intensity infrared ray excited is similar to accompanying drawing 5.
According to chemical formula Yb
0.6Eu
2.4BWO
9The stoichiometric ratio of each element in 975nm takes by weighing respectively ytterbium oxide Yb
2O
3: 0.296 gram, europium sesquioxide Eu
2O
3: 1.056 grams, boric acid H
3BO
3: 0.1623 gram, Tungsten oxide 99.999 WO
3: 0.597 gram, and the citric acid of the 1.8wt% of above medicine total mass, with the ytterbium oxide Y that takes by weighing
2O
3, europium sesquioxide Eu
2O
3With Tungsten oxide 99.999 WO
3Be dissolved in an amount of dilute nitric acid solution, add an amount of deionized water and citric acid in 70 ℃ of stirrings; Then the boric acid that takes by weighing is dissolved in an amount of deionized water, adds again remaining citric acid, and constantly in 70 ℃ of lower stirrings; Above-mentioned two kinds of solution are slowly mixed and constantly stirred 1.5 hours; Leave standstill, oven dry obtains fluffy precursor; Place retort furnace to calcine precursor, sintering temperature is 1000 ℃, and calcination time is 10 hours, is cooled to room temperature, namely obtains pulverous upconversion fluorescent powder, and its XRD diffraction spectrogram and accompanying drawing 1 are approximate.
Referring to accompanying drawing 7, by the sample of the present embodiment technical scheme preparation infrared ray excited lower up-conversion luminescence spectrogram that obtains in 975nm, different excitation energy intensity, as seen from Figure 7, the luminous intensity of this material increases along with the enhancing of excitation diode energy intensity.
Claims (9)
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