CN103361060A - Tm<3+>-doped three-photon infrared quantum cutting material and preparation method thereof - Google Patents
Tm<3+>-doped three-photon infrared quantum cutting material and preparation method thereof Download PDFInfo
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- CN103361060A CN103361060A CN2013102966002A CN201310296600A CN103361060A CN 103361060 A CN103361060 A CN 103361060A CN 2013102966002 A CN2013102966002 A CN 2013102966002A CN 201310296600 A CN201310296600 A CN 201310296600A CN 103361060 A CN103361060 A CN 103361060A
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Abstract
The invention discloses a Tm<3+>-doped three-photon infrared quantum cutting material. The Tm<3+>-doped three-photon infrared quantum cutting material is characterized in that NaYF4 is taken as a matrix, an rare earth ion Tm<3+> is taken as an activator ion, and the chemical constitution is NaY1-yF4:Tmy, wherein y is more than or equal to 0.0025 and less than or equal to 0.30. The invention further discloses a preparation method of the infrared quantum cutting material. The preparation method comprises the following steps of: (1) dissolving NaF and NH4HF2 in deionized water so as to obtain mixed solution of the NaF and the NH4HF2, uniformly mixing the mixed solution of the NaF and the NH4HF2, Y(NO3)3 solution and Tm(NO3)3 solution in a magnetic stirring manner, and regulating the pH value, so as to form precursor suspension liquid; (2) crystallizing the precursor suspension liquid under a hydrothermal condition, carrying out centrifuging after cooling to the room temperature, and drying the product so as to obtain the three-photon infrared quantum cutting material. According to the three-photon infrared quantum cutting material disclosed by the invention, the quantum efficiency is high, and a condition that the conventional solar cell is low in working efficiency can be effectively improved.
Description
Technical field
The present invention relates to infrared quantum tailoring material, particularly a kind of Tm that mixes
3+Three-photon infrared quantum tailoring material and preparation method thereof.
Background technology
For a long time, quantum yield becomes the focus of people's research greater than 100% luminescent material, and it has great application prospect in the photoelectric devices such as efficient illumination, demonstration, Solid State Laser and solar cell.Quantum-cutting is widely studied as a kind of High Efficiency Luminescence mechanism, and its research the earliest is that the high energy vacuum ultraviolet photon of an absorption is converted to two optical photon emissions, and this process can be effectively by singly mixing Pr
3+Reach and mix altogether Gd
3+/ Eu
3+Fluorescent material realize (J.Lumin.1974,8,341; J.Lumin.1974,8,344; Science, 1999,283,663), this material is expected to for efficient non-mercury florescent lamp and plasma flat-panel display (Prog.Mater.Sci.2010,55,353).
In recent years, infrared quantum tailoring is a kind of efficient spectrum modulation means that can be applicable to improve conversion efficiency of solar cell: the high energy ultraviolet of an incident or optical photon are converted to two or more wavelength and are positioned at the infrared photon of solar cell optimal absorption band effectively, thereby can be used as that a kind of effective lower conversion layer reduces the thermosteresis of high energy incident solar photon and photoelectric transformation efficiency (the Sol.Energy Mater.Sol.Cells2006 that greatly improves solar cell, 80,1189).The two-photon infrared quantum tailoring is transmitted in Ln
3+/ Yb
3+(Ln=Tb, Tm, Pr, Er, and Nd) rare earth ion is to extensively being realized in the material of codoped, and its basic physical process is: Ln
3+Absorb a ultraviolet or blue light high-energy photon as donor ion, then excite two Yb that are adjacent by resonance or cooperation transmission ofenergy
3+Acceptor ion, thus make Yb
3+Launch two wavelength and be positioned at the approximately infrared photon of 1000nm, its quantum yield is greater than 100%.This two-photon quantum-cutting material is applied to improve silicon single crystal based solar battery efficient and is widely studied (Phys.Chem.Phys.Chem.2009,11,11081) owing to can be used as lower conversion layer.However, in a lot of situations, Yb
3+Infraluminescence just derive from donor ion Ln
3+First resonance transmission ofenergy rather than quantum-cutting process; On the other hand, the rare earth ion list is mixed the rare report of system infrared quantum tailoring material, does not especially have Tm
3+The ion list is mixed infrared quantum tailoring material of system and preparation method thereof.
Summary of the invention
Above-mentioned shortcoming and deficiency in order to overcome prior art the object of the present invention is to provide a kind of Tm of mixing
3+The three-photon infrared quantum tailoring material, the quantum yield of material is high, can effectively improve the inefficient situation of present solar cell working.
Purpose of the present invention is achieved through the following technical solutions:
A kind of Tm that mixes
3+The three-photon infrared quantum tailoring material is with NaYF
4Be matrix, with rare earth ion Tm
3+As activator ion, chemical constitution is NaY
1-yF
4: Tm
y, 0.0025≤y≤0.30 wherein.
The above-mentioned Tm that mixes
3+The three-photon infrared quantum tailoring material may further comprise the steps:
(1) with Na:Y:Tm:NH
4HF
2Mol ratio is 1:(1-y): the stoichiometric ratio of y:9 takes by weighing NaF, Y
2O
3, Tm
2O
3, NH
4HF
2, 0.0025≤y≤0.30 wherein; With NaF, NH
4HF
2Be dissolved in deionized water, obtain NaF and NH
4HF
2Mixing solutions; With Y
2O
3And Tm
2O
3Be dissolved in respectively nitric acid and be mixed with Y (NO
3)
3Solution and Tm (NO
3)
3Solution; With NaF and NH
4HF
2Mixing solutions, Y (NO
3)
3Solution, Tm (NO
3)
3Solution mixes with magnetic agitation, and to regulate pH value be 2～6, formation presoma suspension;
(2) presoma suspension is moved in the reactor, 160～220 ℃ of crystallization are 2～72 hours under hydrothermal condition, be cooled to room temperature after, water and dehydrated alcohol are centrifugal respectively with products therefrom, namely get after the product oven dry and mix Tm
3+The three-photon infrared quantum tailoring material.
The described oven dry of step (2) is specially: dry more than 10 hours at 60～80 ℃.
The described centrifugal rotating speed of step (2) is that per minute 3500 turns above.
Step (2) is described to be moved to presoma suspension in the reactor, is specially:
Presoma suspension is moved to band teflon-lined stainless steel cauldron, and compactedness is 70～85%.
The Tm that mixes of the present invention
3+The action principle of three-photon infrared quantum tailoring material is as follows: Tm
3+Can effectively absorb the optical photon of a 470nm, except itself launch a series of wavelength be positioned at 600-850nm visible-infrared photon, also can be respectively with
3H
4With
3F
4For middle energy state sequential transmissions wavelength lays respectively at 1165,1466 and 1800nm about three infrared photons, its quantum yield is up to 158%, the photon of these wavelength can (band gap be about 0.66eV by the germanium based solar battery effectively, corresponding to the about infrared photon wavelength of 1880nm) institute absorbs, this material is positioned over the solar cell upper surface as lower conversion layer, can its electricity conversion of Effective Raise; In addition, this material also can effectively be applied to design and be obtained other photoelectron devices.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention only relates to the quantum-cutting process of single activator ion, and this quantum-cutting material can effectively realize absorbing high energy Uv and visible light and the quantum-cutting process of launching three infrared photons, Ln different from the past
3+/ Yb
3+Mix altogether two-photon emission infrared quantum tailoring system.
(2) three-photon infrared quantum tailoring material provided by the invention, quantum yield are up to 158%, and the quantum yield of at present general luminescent material is all far below 100%.
(3) three-photon infrared quantum tailoring material of the present invention can be used in design efficiency light electronics device.NaY
1-yF
4: Tm
yIt is 1165 that the infrared quantum tailoring material emission produces wavelength, 1466 and three infrared photons of 1800nm, its energy all (is about 0.66eV greater than the band gap of germanium based solar battery, corresponding to the about infrared photon wavelength of 1880nm), therefore this kind infrared quantum tailoring material can be placed germanium based solar battery surface, this absorbed sunlight is launched the infrared photon that three energy are absorbed by the germanium based solar battery through the quantum-cutting process, can effectively improve the inefficient situation of present solar cell working.
Description of drawings
Fig. 1 is the embodiment of the invention 1 gained three-photon emission infrared quantum tailoring material NaY
0.99F
4: Tm
0.01(sample 2) infra-red emission of gained under different excitation wavelengths.
Fig. 2 is the embodiment of the invention 1 gained three-photon emission infrared quantum tailoring material NaY
0.99F
4: Tm
0.01The excitation spectrum of (sample 2).
Fig. 3 is the embodiment of the invention 1 gained three-photon emission infrared quantum tailoring material NaY
0.99F
4: Tm
0.01The infrared emission time resolved spectroscopy of (sample 2).
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
Prepare four parts in following sample: accurately take by weighing 0.5589g yttrium oxide (Y
2O
3) and 0.0096g trioxide (Tm
2O
3), be dissolved in an amount of hot concentratedly, being mixed with concentration is 0.05mol.L
-1Y (NO
3)
3Solution and Tm (NO
3)
3Solution; Then accurately weighing 0.2100g Sodium Fluoride (NaF) and 0.5668g ammonium bifluoride (NH
4HF
2), all be dissolved in an amount of deionized water solution, obtain NaF and NH
4HF
2Mixing solutions; Under the even mixing effect of magnetic agitation, the Y (NO for preparing
3)
3And Tm (NO
3)
3Mixing solutions slowly adds NaF and NH fully
4HF
2In the mixing solutions; Regulate mixing solutions PH=3 formation presoma suspension by dripping an amount of ammoniacal liquor, stir after 30 minutes, it is that compactedness is 80% in the 50ml band teflon-lined stainless steel cauldron that the presoma suspension that forms is moved to volume.
Sample with in the above-mentioned stainless steel cauldron places baking oven, under hydrothermal condition, respectively at 160 ℃ (samples 1), 180 ℃ (sample 2), 200 ℃ (sample 3), 220 ℃ of (sample 4) crystallization 20 hours.After being cooled to room temperature, with products therefrom respectively water and the centrifugal several of alcohol, centrifugal rotating speed is per minute more than 5000, and final product got final product to get prepared NaY under the different crystallization temperatures in 12 hours in 80 ℃ of oven dry
0.99F
4: Tm
0.01Sample.
After testing, the NaY of the present embodiment preparation
0.99F
4: Tm
0.01The diffraction peak of the XRD result of sample and JCPDS card (#16-0334) is in full accord, illustrates to be six side's phase NaYF
4: Tm
3+Pure phase, lattice parameter is
Fig. 1 is the infra-red emission of gained under the different excitation wavelengths of sample 2.As seen from the figure, when with 470nm excited sample 2, except observing a series of Tm
3+Feature visible emissivity peak outside, can also obtain peak value and lay respectively at 1165,1466 and three infrared emission peaks of 1800nm; When exciting NaY with 798nm
0.99F
4: Tm
0.01During sample, do not observe the infrared emission light of 1165nm, and just observed 1466 and 1800nm infrared emission peak; And when exciting NaY with 976nm
0.98F
4: Tm
0.01Yb
0.01During sample, only to obtain the infrared emission peak of 1800nm.Correspondingly, the excitation spectrum of sample 2 when monitoring respectively 1466 and during the 1800nm utilizing emitted light, can obtain the Tm before a series of 850nm of being positioned at as shown in Figure 2
3+The feature excitation peak; And when monitoring 1165nm utilizing emitted light, be positioned at only the Tm of 470nm to obtain peak value
3+The feature excitation peak.By Fig. 1 and the shown Spectral Phenomenon of Fig. 2, can analyze judgement, the present embodiment obtained a kind of based on
3H
4With
3F
4Three-photon emission for intermediate level.Figure 3 shows that the infrared emission temporal resolution light of sample 2, also detected Tm
3+Three-photon cascade emission, through experimental and theoretical computation, its quantum yield is up to 158%.
The stable state of sample 1, sample 3 and sample 4 and transient state spectral signature and three-photon emission process are similar to Example 1, but temperature of reaction is higher, and the sample particle size is larger, and its luminous intensity is also larger.
Accurately take by weighing 0.5631g yttrium oxide (Y
2O
3) and 0.0024g trioxide (Tm
2O
3), be dissolved in an amount of hot concentratedly, being mixed with concentration is 0.05mol.L
-1Y (NO
3)
3Solution and Tm (NO
3)
3Solution; Then accurately weighing 0.2100g Sodium Fluoride (NaF) and 0.5668g ammonium bifluoride (NH
4HF
2), all be dissolved in an amount of deionized water solution, obtain NaF and NH
4HF
2Mixing solutions; Under the even mixing effect of magnetic agitation, the Y (NO for preparing
3)
3And Tm (NO
3)
3Mixing solutions slowly adds NaF and NH fully
4HF
2In the mixing solutions; Regulate mixing solutions PH=2 formation presoma suspension by dripping an amount of ammoniacal liquor, stir after 30 minutes, it is that compactedness is 70% in the 50ml band teflon-lined stainless steel cauldron that the presoma suspension that forms is moved to volume.In baking oven under hydrothermal condition 180 ℃ of crystallization 72 hours.After being cooled to room temperature, with products therefrom difference water and the centrifugal several of alcohol, centrifugal rotating speed is that per minute 3500 turns above, and final product got final product to get NaY in 12 hours in 60 ℃ of oven dry
0.9975F
4: Tm
0.0025Sample.
Accurately take by weighing 0.3952g yttrium oxide (Y
2O
3) and 0.2894g trioxide (Tm
2O
3), be dissolved in an amount of hot concentratedly, being mixed with concentration is 0.05mol.L
-1Y (NO
3)
3Solution and Tm (NO
3)
3Solution; Then accurately weighing 0.2100g Sodium Fluoride (NaF) and 0.5668g ammonium bifluoride (NH
4HF
2), all be dissolved in an amount of deionized water solution, obtain NaF and NH
4HF
2Mixing solutions; Under the even mixing effect of magnetic agitation, the Y (NO for preparing
3)
3And Tm (NO
3)
3Mixing solutions slowly adds NaF and NH fully
4HF
2In the mixing solutions; Regulate mixing solutions PH=6 formation presoma suspension by dripping an amount of ammoniacal liquor, stir after 30 minutes, it is that compactedness is 85% in the 50ml band teflon-lined stainless steel cauldron that the presoma suspension that forms is moved to volume.In baking oven under hydrothermal condition 220 ℃ of crystallization 2 hours.After being cooled to room temperature, with products therefrom difference water and the centrifugal several of alcohol, centrifugal rotating speed is that per minute 3500 turns above, and final product got final product to get NaY in 20 hours in 70 ℃ of oven dry
0.70F
4: Tm
0.30Sample.
Above-described embodiment is the better embodiment of the present invention; but embodiments of the present invention are not limited by the examples; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (5)
1. mix Tm for one kind
3+The three-photon infrared quantum tailoring material is characterized in that, with NaYF
4Be matrix, with rare earth ion Tm
3+As activator ion, chemical constitution is NaY
1-yF
4: Tm
y, 0.0025≤y≤0.30 wherein.
2. the described Tm that mixes of claim 1
3+The three-photon infrared quantum tailoring material is characterized in that, may further comprise the steps:
(1) with Na:Y:Tm:NH
4HF
2Mol ratio is 1:(1-y): the stoichiometric ratio of y:9 takes by weighing NaF, Y
2O
3, Tm
2O
3, NH
4HF
2, 0.0025≤y≤0.30 wherein; With NaF, NH
4HF
2Be dissolved in deionized water, obtain NaF and NH
4HF
2Mixing solutions; With Y
2O
3And Tm
2O
3Be dissolved in respectively nitric acid and be mixed with Y (NO
3)
3Solution and Tm (NO
3)
3Solution; With NaF and NH
4HF
2Mixing solutions, Y (NO
3)
3Solution, Tm (NO
3)
3Solution mixes with magnetic agitation, and to regulate pH value be 2～6, formation presoma suspension;
(2) presoma suspension is moved in the reactor, 180～220 ℃ of crystallization are 2～72 hours under hydrothermal condition, be cooled to room temperature after, water and dehydrated alcohol are centrifugal respectively with products therefrom, namely get after the product oven dry and mix Tm
3+The three-photon infrared quantum tailoring material.
3. the described Tm that mixes according to claim 2
3+The three-photon infrared quantum tailoring material is characterized in that, the described oven dry of step (2) is specially: dry more than 10 hours at 60～80 ℃.
4. the described Tm that mixes according to claim 2
3+The three-photon infrared quantum tailoring material is characterized in that, the described centrifugal rotating speed of step (2) is that per minute 3500 turns above.
5. the described Tm that mixes according to claim 2
3+The three-photon infrared quantum tailoring material is characterized in that, step (2) is described to be moved to presoma suspension in the reactor, is specially:
Presoma suspension is moved to band teflon-lined stainless steel cauldron, and compactedness is 70～85%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774221A (en) * | 2014-02-20 | 2014-05-07 | 宁波大学 | Thulium-doped sodium yttrium fluoride laser crystal and preparation method thereof |
| US10510915B2 (en) | 2017-01-26 | 2019-12-17 | United Arab Emirates University | Porous silicon nanowire photovoltaic cell |
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| US20020020830A1 (en) * | 1998-11-25 | 2002-02-21 | Michael Bass | Composites of inorganic luminophores stabilized in polymer hosts |
| CN102382654A (en) * | 2011-09-15 | 2012-03-21 | 上海大学 | Preparation method of up-conversion fluorescent material rare earth doped NaYF4 nanocrystal |
-
2013
- 2013-07-15 CN CN2013102966002A patent/CN103361060A/en active Pending
Patent Citations (2)
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| US20020020830A1 (en) * | 1998-11-25 | 2002-02-21 | Michael Bass | Composites of inorganic luminophores stabilized in polymer hosts |
| CN102382654A (en) * | 2011-09-15 | 2012-03-21 | 上海大学 | Preparation method of up-conversion fluorescent material rare earth doped NaYF4 nanocrystal |
Non-Patent Citations (2)
| Title |
|---|
| D.C.YU等: "Sequential three-step three-photon near-infrared quantum splitting in β-NaYF4:Tm3+", 《APPLIED PHYSICS LETTERS》 * |
| X.P. CHEN等: "Towards efficient upconversion and downconversion of NaYF4:Ho3+,Yb3+ phosphors", 《PHYSICA B: CONDENSED MATTER》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774221A (en) * | 2014-02-20 | 2014-05-07 | 宁波大学 | Thulium-doped sodium yttrium fluoride laser crystal and preparation method thereof |
| US10510915B2 (en) | 2017-01-26 | 2019-12-17 | United Arab Emirates University | Porous silicon nanowire photovoltaic cell |
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Application publication date: 20131023 |