CN102585811A - Fluoroaluminate near-infrared quantum cutting material, and preparation method and application thereof - Google Patents

Fluoroaluminate near-infrared quantum cutting material, and preparation method and application thereof Download PDF

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CN102585811A
CN102585811A CN2012100022374A CN201210002237A CN102585811A CN 102585811 A CN102585811 A CN 102585811A CN 2012100022374 A CN2012100022374 A CN 2012100022374A CN 201210002237 A CN201210002237 A CN 201210002237A CN 102585811 A CN102585811 A CN 102585811A
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fluoaluminate
infrared quantum
raw material
cutting
infrared
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CN102585811B (en
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孙家跃
杜海燕
孙翊宁
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Beijing Technology and Business University
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Abstract

The invention discloses a fluoroaluminate near-infrared quantum cutting material, and a preparation method and application thereof. The fluoroaluminate near-infrared quantum cutting material has a chemical formula: Sr3(0.99-x)AlO4F: 0.01Ce<3+> and xYb<3+> (x is not less than 0 and not more than 0.1). The preparation method for the fluoroaluminate near-infrared quantum cutting material comprises the followings steps of: weighing a strontium raw material, an aluminium raw material, a cerium raw material and a ytterbium raw material according to the molar ratio in the chemical formula; and grinding each material and mixing uniformly, then heating to 1200 DEG C at the speed of 600 DEG C/h under the CO reducing atmosphere, keeping the constant temperature of 1200 DEG C for 4 h, and cooling to obtain the powdered fluoroaluminate near-infrared quantum cutting material. The fluoroaluminate near-infrared quantum cutting material disclosed by the invention has the advantages of high luminous intensity, good stability, high quantum efficiency and environment-friendliness.

Description

Fluoaluminate near-infrared quantum-cutting material and preparation method thereof and application
Technical field
The present invention relates to a kind of novel near-infrared quantum-cutting material and preparation method thereof and application, relate in particular to a kind of fluoaluminate near-infrared quantum-cutting material and preparation method thereof and application.
Background technology
Quantum-cutting (conversion down) type near-infrared light-emitting material: it is cut to a plurality of wavelength X ≈ 1000nm near infrared photon quantum with a high-energy photons (wavelength region is generally 300-500nm).Cut out effect and can realize tailoring process through the transmission ofenergy between the energy level transition of single ionic, transmission ofenergy, ion and the matrix between the pair ion.
The quantum-cutting Study on Effect is confined to the visible region in the past, has begun to be extended to the near infrared field recent years.Near-infrared quantum-cutting is meant an optical photon is converted into two near infrared photons; Avoided optical photon in the power loss in energy photons conversion process more; It can effectively improve the efficient and the stability of solar cell, and the novel fluorescence body that therefore converts the visible light in the solar spectral and UV-light near infrared light is the main task that present luminescent material is studied.Using the most general matrix at present is rare earth ion doped fluoride system.But can produce human body, the deleterious gas of environment in the preparation process, destroy HUMAN HEALTH, contaminate environment.
Summary of the invention
The object of the invention is to provide a kind of luminous intensity height, good stability, fluoaluminate near-infrared quantum-cutting material that quantum yield is high.
Fluoaluminate near-infrared quantum-cutting material provided by the present invention, its chemical constitution are that chemical constitution formula is:
Sr 3(0.99-x)AlO 4F:0.01Ce 3+，xYb 3+，(0≤x≤0.1)。
Wherein, 0≤x≤0.01,0.01≤x≤0.02,0.02≤x≤0.03,0.03≤x≤0.04,0.04≤x≤0.05,0.05≤x≤0.06,0.06≤x≤0.07,0.07≤x≤0.08,0.08≤x≤0.09 or 0.09≤x≤0.10.
Another object of the present invention provides a kind of fluoaluminate near-infrared quantum-cutting preparation methods.
Fluoaluminate near-infrared quantum-cutting preparation methods provided by the present invention comprises the steps:
Press chemical constitution formula Sr 3 (0.99-x)AlO 4F:0.01Ce 3+, xYb 3+The mole proportioning of (0≤x≤0.1) takes by weighing strontium raw material, aluminum feedstock, fluorine raw material, cerium raw material and ytterbium raw material;
Under the reducing atmosphere of CO, be warmed up to 1200 ℃ behind the said former abrasive lapping mixing,, after the cooling, grind, obtain fluoaluminate near-infrared quantum-cutting material 1200 ℃ of constant temperature 4 hours with 600 ℃/h.
According to an aspect of the present invention, said strontium raw material be selected from Strontium carbonate powder, strontium nitrate and the strontium oxide any or appoint several kinds.
According to an aspect of the present invention, said aluminum feedstock be selected from aluminum oxide, white lake and the aluminium carbonate any or appoint several kinds.
According to an aspect of the present invention, said fluorine raw material be selected from strontium fluoride and the ammonium fluoride any or appoint several kinds.
According to an aspect of the present invention, said cerium raw material be selected from cerium oxide and the cerous nitrate any or appoint several kinds.
According to an aspect of the present invention, said ytterbium raw material be selected from ytterbium oxide and the ytterbium nitrate any or appoint several kinds.
According to an aspect of the present invention, 0≤x≤0.01,0.01≤x≤0.02,0.02≤x≤0.03; 0.03≤x≤0.04,0.04≤x≤0.05,0.05≤x≤0.06; 0.06≤x≤0.07,0.07≤x≤0.08,0.08≤x≤0.09 or 0.09≤x≤0.10.
Compared with prior art; Novel near-infrared quantum-cutting material of the present invention can be by the near ultraviolet excitation of 200～500nm; The non-constant width of excitation spectrum, (200～500nm) have its emission peak of strong absorption is positioned near infrared (900～1200nm) scopes in the near ultraviolet region.Being up to 185% through calculating its quantum yield, is a kind of new Near quantum-cutting material that is applicable to solar cell.It is matrix that novel near-infrared quantum-cutting material of the present invention has adopted common fluoaluminate, and compound method is simple, easy handling, environmental protection.
Description of drawings
Fig. 1 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.97AlO 4F:0.01Ce 3+The XRD diffracting spectrum;
Fig. 2 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.94AlO 4F:0.01Ce 3+, 0.01Yb 3+The XRD diffracting spectrum;
Fig. 3 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.82AlO 4F:0.01Ce 3+, 0.05Yb 3+The XRD diffracting spectrum;
Fig. 4 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.67AlO 4F:0.01Ce 3+, 0.1Yb 3+The XRD diffracting spectrum.
Fig. 5 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.97AlO 4F:0.01Ce 3+Exciting and emmission spectrum figure at room temperature;
Fig. 6 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.94AlO 4F:0.01Ce 3+, 0.01Yb 3+Detecting with 980nm and 464nm at room temperature obtains the exciting light spectrogram;
Fig. 7 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.94AlO 4F:0.01Ce 3+, 0.01Yb 3+The emmission spectrum figure that excites of 401nm at room temperature;
Fig. 8 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.82AlO 4F:0.01Ce 3+, 0.05Yb 3+The emmission spectrum figure that excites of 401nm at room temperature;
Fig. 9 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.67AlO 4F:0.01Ce 3+, 0.1Yb 3+The emmission spectrum figure that excites of 401nm at room temperature;
Figure 10 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.97AlO 4F:0.01Ce 3+Ce at room temperature 3+The life-span decay pattern;
Figure 11 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.94AlO 4F:0.01Ce 3+, 0.01Yb 3+Ce at room temperature 3+The life-span decay pattern;
Figure 12 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.82AlO 4F:0.01Ce 3+, 0.05Yb 3+Ce at room temperature 3+The life-span decay pattern;
Figure 13 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 2.67AlO 4F:0.01Ce 3+, 0.1Yb 3+Ce at room temperature 3+The life-span decay pattern;
Figure 14 is fluoaluminate near-infrared quantum-cutting material Sr of the present invention 3 (0.99-x)AlO 4F:0.01Ce 3+, xYb 3+(0≤x≤0.1) is through calculating gained transmission ofenergy rate and quantum yield comparison diagram.
Embodiment
Embodiment 1: fluoaluminate near-infrared quantum-cutting material Sr 2.97AlO 4F:0.01Ce 3+Preparation
Take by weighing Strontium carbonate powder (SrCO respectively 3) 0.7324g, strontium fluoride (SrF 2) 0.1256g, aluminum oxide (Al 2O 3) 0.1019g, cerium oxide (CeO 2) 0.0034g.Above-mentioned raw materials after agate mortar grinds mixing, in the corundum crucible of packing into, is put into High Temperature Furnaces Heating Apparatus, under the reducing atmosphere of CO, be warmed up to 1200 ℃ with 600 ℃/h, 1200 ℃ of constant temperature 4 hours, bulk material was taken out in cooling, grinds and obtains pulverous sample.The XRD diffractogram of this sample is seen Fig. 1, through with SrAlO 4The standard card contrast of F finds that the diffraction peak position is in full accord, and a spot of Ce that mixes is described 3+Crystalline network to matrix does not have influence.Sample excites under 401nm, and the room temperature of this sample excites with emmission spectrum sees Fig. 5, and the emission main peak of near ultraviolet region is positioned at 464nm, and the near-infrared region does not have emission.The life-span decay collection of illustrative plates of this sample is seen Figure 10, through quadratic fit, calculates Ce 3+Fluorescence lifetime be 0.035 μ s.
Embodiment 2: fluoaluminate near-infrared quantum-cutting material Sr 2.94AlO 4F:0.01Ce 3+, 0.01Yb 3+Preparation
Take by weighing Strontium carbonate powder (SrCO respectively 3) 0.7279g, strontium fluoride (SrF 2) 0.1256g, aluminum oxide (Al 2O 3) 0.1019g, cerium oxide (CeO 2) 0.0034g and ytterbium oxide (Yb 2O 3) 0.0039g.Above-mentioned raw materials after agate mortar grinds mixing, in the corundum crucible of packing into, is put into High Temperature Furnaces Heating Apparatus, under the reducing atmosphere of CO, be warmed up to 1200 ℃ with 600 ℃/h, 1200 ℃ of constant temperature 4 hours, bulk material was taken out in cooling, grinds and obtains pulverous sample.The XRD diffractogram of this sample is seen Fig. 2, through with SrAlO 4The standard card contrast of F finds that the diffraction peak position is in full accord, and a spot of Ce that mixes is described 3+, Yb 3+Crystalline network to matrix does not have influence.The excitation spectrum that the excitation spectrum that this sample records under the 980nm wavelength detects and this sample are measured under the 464nm wavelength detects is seen Fig. 6, find that through contrast their peak type is similar, and main peak is all at 401nm.Explain that 401nm excites down Ce 3+→ Yb 3+Transmission ofenergy can take place.Sample excites under 401nm, and the room temperature emmission spectrum of this sample is seen Fig. 7, and the emission main peak of near ultraviolet region is positioned at 464nm, and the near-infrared region does not have the emission main peak and is positioned at 980nm.The life-span decay collection of illustrative plates of this sample is seen Figure 11, through quadratic fit, calculates Ce 3+Fluorescence lifetime be 0.029 μ s.
Embodiment 3: fluoaluminate near-infrared quantum-cutting material Sr 2.82AlO 4F:0.01Ce 3+, 0.05Yb 3+
Take by weighing Strontium carbonate powder (SrCO respectively 3) 0.7103g, strontium fluoride (SrF 2) 0.1256g, aluminum oxide (Al 2O 3) 0.1019g, cerium oxide (CeO 2) 0.0034g and ytterbium oxide (Yb 2O 3) 0.0197g.Above-mentioned raw materials after agate mortar grinds mixing, in the corundum crucible of packing into, is put into High Temperature Furnaces Heating Apparatus, under the reducing atmosphere of CO, be warmed up to 1200 ℃ with 600 ℃/h, 1200 ℃ of constant temperature 4 hours, bulk material was taken out in cooling, grinds and obtains pulverous sample.The XRD diffractogram of this sample is seen Fig. 3, through with SrAlO 4The standard card contrast of F finds that the diffraction peak position is in full accord, and a spot of Ce that mixes is described 3+, Yb 3+Crystalline network to matrix does not have influence.Sample excites under 401nm, and the room temperature emmission spectrum of this sample is seen Fig. 8, and the emission main peak of near ultraviolet region is positioned at 464nm, and the near-infrared region does not have the emission main peak and is positioned at 980nm.The life-span decay collection of illustrative plates of this sample is seen Figure 12, through the quadratic fit method, calculates Ce 3+Fluorescence lifetime be 0.020 μ s.
Embodiment 4: fluoaluminate near-infrared quantum-cutting material Sr 2.67AlO 4F:0.01Ce 3+, 0.1Yb 3+
Take by weighing Strontium carbonate powder (SrCO respectively 3) 0.6882g, strontium fluoride (SrF 2) 0.1256g, aluminum oxide (Al 2O 3) 0.1019g, cerium oxide (CeO 2) 0.0034g and ytterbium oxide (Yb 2O 3) 0.0394g.Above-mentioned raw materials after agate mortar grinds mixing, in the corundum crucible of packing into, is put into High Temperature Furnaces Heating Apparatus, under the reducing atmosphere of CO, be warmed up to 1200 ℃ with 600 ℃/h, 1200 ℃ of constant temperature 4 hours, bulk material was taken out in cooling, grinds and obtains pulverous sample.The XRD diffractogram of this sample is seen Fig. 4, through with SrAlO 4The standard card contrast of F finds that the diffraction peak position is in full accord, and a spot of Ce that mixes is described 3+, Yb 3+Crystalline network to matrix does not have influence.Sample excites under 401nm, and the room temperature emmission spectrum of this sample is seen Fig. 9, and the emission main peak of near ultraviolet region is positioned at 464nm, and the near-infrared region does not have the emission main peak and is positioned at 980nm.The life-span decay collection of illustrative plates of this sample is seen Figure 13, through quadratic fit, calculates Ce 3+Fluorescence lifetime be 0.016 μ s.。
Near-infrared quantum-cutting material Sr 2.97AlO 4F:0.01Ce 3+, Sr 2.94AlO 4F:0.01Ce 3+, 0.01Yb 3+, CaSr 2.82AlO 4F:0.01Ce 3+, 0.05Yb 3+, Sr 2.67AlO 4F:0.01Ce 3+, 0.1Yb 3+The decay life-span through calculating gained is respectively 0.035 μ s, 0.029 μ s, 0.020 μ s, 0.016 μ s; Quantum yield is respectively 0,42.28%, and 78.30%, 185.21%.Life-span and quantum yield are with respect to Yb 3+The variation contrast of doping is shown in figure 14
Can find out Ce by Figure 14 3+Fluorescence lifetime along with Yb 3+The increase of doping content descends gradually, further proves Ce 3+Transmission ofenergy given Yb 3+Quantum yield is with Yb 3+The increase of doping content increases gradually, works as Yb 3+Doping content be 10%Ce 3+→ Yb 3+Following conversion quantum yield reach 185.2%, Ce is described 3+, Yb 3+The near-infrared quantum-cutting fluorescent material of mixing altogether has higher quantum yield, has the potential that is applied to monocrystaline silicon solar cell.

Claims (10)

1. fluoaluminate near-infrared quantum-cutting material, its chemical constitution formula is:
Sr 3(0.99-x)AlO 4F:0.01Ce 3+，xYb 3+，(0≤x≤0.1)。
2. fluoaluminate near-infrared quantum-cutting material according to claim 1 is characterized in that,
0≤x≤0.01,0.01≤x≤0.02,0.02≤x≤0.03,0.03≤x≤0.04,0.04≤x≤0.05,0.05≤x≤0.06,0.06≤x≤0.07,0.07≤x≤0.08,0.08≤x≤0.09 or 0.09≤x≤0.10.
3. a fluoaluminate near-infrared quantum-cutting preparation methods comprises the steps:
Press chemical constitution formula Sr 3 (0.99-x)AlO 4F:0.01Ce 3+, xYb 3+The mole proportioning of (0≤x≤0.1) takes by weighing strontium raw material, aluminum feedstock, fluorine raw material, cerium raw material and ytterbium raw material;
Under the reducing atmosphere of CO, be warmed up to 1200 ℃ behind the said former abrasive lapping mixing,, after the cooling, obtain fluoaluminate near-infrared quantum-cutting material 1200 ℃ of constant temperature 4 hours with 600 ℃/h.
4. fluoaluminate near-infrared quantum-cutting preparation methods according to claim 3 is characterized in that, said strontium raw material be selected from Strontium carbonate powder, strontium nitrate and the strontium oxide any or appoint several kinds.
5. according to claim 3 or 4 described fluoaluminate near-infrared quantum-cutting preparation methods, it is characterized in that, said aluminum feedstock be selected from aluminum oxide, white lake and the aluminium carbonate any or appoint several kinds.
6. fluoaluminate near-infrared quantum-cutting preparation methods according to claim 5 is characterized in that, said fluorine raw material be selected from strontium fluoride and the ammonium fluoride any or appoint several kinds.
7. fluoaluminate near-infrared quantum-cutting preparation methods according to claim 6 is characterized in that, said cerium raw material be selected from cerium oxide and the cerous nitrate any or appoint several kinds.
8. fluoaluminate near-infrared quantum-cutting preparation methods according to claim 7 is characterized in that, said ytterbium raw material be selected from ytterbium oxide and the ytterbium nitrate any or appoint several kinds.
9. fluoaluminate near-infrared quantum-cutting preparation methods according to claim 3 is characterized in that 0≤x≤0.01; 0.01≤x≤0.02,0.02≤x≤0.03,0.03≤x≤0.04; 0.04≤x≤0.05,0.05≤x≤0.06,0.06≤x≤0.07; 0.07≤x≤0.08,0.08≤x≤0.09 or 0.09≤x≤0.10.
10. claim 1 or the 2 described fluoaluminate near-infrared quantum-cutting materials application in the preparation solar cell.
CN201210002237.4A 2012-01-05 2012-01-05 Fluoroaluminate near-infrared quantum cutting material, and preparation method and application thereof Expired - Fee Related CN102585811B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102977880A (en) * 2012-12-04 2013-03-20 中国科学院半导体研究所 Preparation method of downconversion fluorescent material
CN108384536A (en) * 2018-05-16 2018-08-10 长春理工大学 Er3+/Yb3+Codope calcium aluminum fluoride green up conversion luminescent material and preparation method thereof

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WO2006111568A2 (en) * 2005-04-20 2006-10-26 Etech Ag Novel materials used for emitting light

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WO2006111568A2 (en) * 2005-04-20 2006-10-26 Etech Ag Novel materials used for emitting light

Non-Patent Citations (2)

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Title
MENGMENG SHANG ET AL.: "Tunable Luminescence and Energy Transfer properties of Sr3AlO4F:RE3+ (RE = Tm/Tb, Eu, Ce) Phosphors", 《ACS APPL. MATER. INTERFACES》 *
WANPING CHEN ET AL.: "Chromaticity-Tunable Emission of Sr3AlO4F:Ce3+ Phosphor: Correlation with Matrix Structure and Application in LEDs", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102977880A (en) * 2012-12-04 2013-03-20 中国科学院半导体研究所 Preparation method of downconversion fluorescent material
CN108384536A (en) * 2018-05-16 2018-08-10 长春理工大学 Er3+/Yb3+Codope calcium aluminum fluoride green up conversion luminescent material and preparation method thereof

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