CN103923648A - Thulium-doped sulfide glass up-conversion luminescent material, preparation method and application - Google Patents
Thulium-doped sulfide glass up-conversion luminescent material, preparation method and application Download PDFInfo
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- CN103923648A CN103923648A CN201310008639.XA CN201310008639A CN103923648A CN 103923648 A CN103923648 A CN 103923648A CN 201310008639 A CN201310008639 A CN 201310008639A CN 103923648 A CN103923648 A CN 103923648A
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Abstract
The invention discloses a thulium-doped sulfide glass up-conversion luminescent material with a chemical formula being GeS2-Ga2S3:xTm<3+>, wherein x is a number ranging from 0.002-0.06. An excitation wavelength of the thulium-doped sulfide glass up-conversion luminescent material is 796 nm. A luminescent peak at 475 nm is respectively corresponding to the luminescent peak formed through a <1>G4 to <3>H6 transition radiation of Tm<3+> ions. A blue light short-wave luminescence can be excited through a long-wave radiation from red light to green light. The invention also provides a preparation method and an application for the thulium-doped sulfide glass up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of thulium doping chalcogenide glass up-conversion luminescent material, its preparation method and use the Organic Light Emitting Diode of this thulium doping chalcogenide glass up-conversion luminescent material.
Background technology
Organic Light Emitting Diode (OLED) because unit construction is simple, the characteristic such as cheap, the luminous of production cost, reaction times be short, flexible, and obtained the utmost point, apply widely.But owing to obtaining at present, the OLED blue light material of stability and high efficiency is more difficult, has limited greatly the development of white light OLED device and light source industry.
Upconverting fluorescent material can be launched visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in fields such as optical fiber communication technology, fibre amplifier, 3 D stereo demonstration, biomolecules fluorescence labelling, infrared detectives.But, can be by infrared, the long-wave radiations such as red-green glow inspire the thulium doping chalcogenide glass up-conversion luminescent material of blue emission, have not yet to see report.
Summary of the invention
Based on this, being necessary to provide a kind of can be inspired thulium doping chalcogenide glass up-conversion luminescent material, its preparation method of blue light and be used the Organic Light Emitting Diode of this thulium doping chalcogenide glass up-conversion luminescent material by long-wave radiation.
A thulium doping chalcogenide glass up-conversion luminescent material, its chemical formula is GeS
2-Ga
2s
3: xTm
3+, wherein, x is 0.002 ~ 0.06.
In an embodiment, x is 0.03 therein.
A preparation method for thulium doping chalcogenide glass up-conversion luminescent material, comprises the following steps:
According to GeS
2-Ga
2s
3: xTm
3+the stoichiometric ratio of each element takes GeS
2, Ga
2s
3and Tm
2s
3powder, wherein, x is 0.002 ~ 0.06;
The powder taking is dissolved in and in hydrogen sulfide, is mixed with the solution that the concentration of metallic cation is 0.05mol/L ~ 3mol/L;
Described solution mist is changed into after mist to carrier gas, to pass into temperature be that the silica tube of 100 ℃ ~ 220 ℃ generates presoma, wherein, the diameter of silica tube is 30mm ~ 150mm, and length is 0.5m ~ 3m, and the flow of carrier gas is 1L/min ~ 15L/min;
Described presoma being calcined at 600 ℃ ~ 1000 ℃ and within 2 hours ~ 5 hours, obtained chemical formula is GeS
2-Ga
2s
3: xTm
3+thulium doping chalcogenide glass up-conversion luminescent material.
In an embodiment, x is 0.03 therein.
Therein in an embodiment, the powder taking is dissolved in to the step that is mixed with solution in hydrogen sulfide and also comprises: in described solution, add dispersion agent, the concentration of described dispersion agent is 0.005mol/L ~ 0.05mol/L.
In an embodiment, described dispersion agent is polyoxyethylene glycol therein.
Therein in an embodiment, the step that described solution mist is changed into mist is, carrier gas and described solution are passed into together in spraying gun and makes described solution mist change into mist, and described carrier gas is rare gas element or reducing gas.
In an embodiment, the flow of described carrier gas is 5L/min ~ 8L/min therein.
A kind of Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, in described transparent encapsulated layer, doped with thulium doping chalcogenide glass up-conversion luminescent material, the chemical general formula of described thulium doping chalcogenide glass up-conversion luminescent material is GeS
2-Ga
2s
3: xTm
3+, wherein, x is 0.002 ~ 0.06.
In an embodiment, x is 0.03 therein.
The preparation method of above-mentioned thulium doping chalcogenide glass up-conversion luminescent material is comparatively simple, and cost is lower; In the photoluminescence spectra of the thulium doping chalcogenide glass up-conversion luminescent material of preparation, the excitation wavelength of thulium doping chalcogenide glass up-conversion luminescent material is 796nm, and corresponding respectively at the glow peak of 475nm is Tm
3+ion
1g
4→
3h
6transition radiation form glow peak, realized that by the infrared long-wave radiation to green glow, to inspire blue light shortwave luminous; In the transparent encapsulated layer of Organic Light Emitting Diode, be dispersed with thulium doping chalcogenide glass up-conversion luminescent material, the excitation wavelength of thulium doping chalcogenide glass up-conversion luminescent material is 796nm, and corresponding respectively at the glow peak of 475nm is Tm
3+ion
1g
4→
3h
6transition radiation form glow peak, by red-green glow, excite and can launch blue light, blue light mixes the Organic Light Emitting Diode that formation emits white light afterwards with red-green glow.
Accompanying drawing explanation
Fig. 1 is the structural representation of the spray pyrolysis equipment of an embodiment;
Fig. 2 is the structural representation of the Organic Light Emitting Diode of an embodiment
Fig. 3 is the photoluminescence spectrogram of the thulium doping chalcogenide glass up-conversion luminescent material of embodiment 1 preparation;
Fig. 4 is the XRD spectra of the thulium doping chalcogenide glass up-conversion luminescent material of embodiment 1 preparation.
Fig. 5 has Organic Light Emitting Diode that thulium doping chalcogenide glass up-conversion luminescent material forms and the spectrogram of comparative example in the transparent encapsulated layer of embodiment 1 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments to thulium doping chalcogenide glass up-conversion luminescent material, its preparation method and use the Organic Light Emitting Diode of this thulium doping chalcogenide glass up-conversion luminescent material further to illustrate.
The thulium doping chalcogenide glass up-conversion luminescent material of one embodiment, its chemical formula is GeS
2-Ga
2s
3: xTm
3+, wherein, x is 0.002 ~ 0.06.
Preferably, x is 0.03.
In the photoluminescence spectra of this thulium doping chalcogenide glass up-conversion luminescent material, the excitation wavelength of thulium doping chalcogenide glass up-conversion luminescent material is 796nm, when material is subject to long wavelength's (as 796nm) radiation, and Tm
3+the energy of this illumination of ionic absorption, now Tm
3+ion by
1g
4→
3h
6transition, send the blue light of 475nm, realized that by the infrared long-wave radiation to green glow, to inspire blue light shortwave luminous.
The preparation method of above-mentioned thulium doping chalcogenide glass up-conversion luminescent material, comprises the following steps;
Step S101, according to GeS
2-Ga
2s
3: xTm
3+the stoichiometric ratio of each element takes GeS
2, Ga
2s
3and Tm
2s
3powder, wherein, x is 0.002 ~ 0.06.
Preferably, x is 0.03.
Being appreciated that in this step also can be according to mol ratio (0.4 ~ 0.8): (0.14 ~ 0.598): (0.002 ~ 0.06) takes GeS
2, Ga
2s
3and Tm
2s
3powder.
Preferably, in this step, also can take GeS according to mol ratio 0.6:0.37:0.03
2, Ga
2s
3and Tm
2s
3powder.
Step S102, the powder taking is dissolved in and in hydrogen sulfide, is mixed with the solution that the concentration of metallic cation is 0.05mol/L ~ 3mol/L.
Metallic cation in solution is Ge
4+, Ga
3+and Tm
3+.
Preferably, the powder taking being dissolved in to the step that is mixed with solution in hydrogen sulfide also comprises: in solution, add dispersion agent, the concentration of dispersion agent is 0.005mol/L ~ 0.05mol/L.In present embodiment, dispersion agent is polyoxyethylene glycol.
Refer to Fig. 1, the spray pyrolysis equipment 100 shown in Fig. 1 comprises container for storing liquid 10, gas-holder 20, spraying gun 30, silica tube 40 and collector 50.
In present embodiment, solution prepared by step S102 is deposited in container for storing liquid 10.
S103, solution mist is changed into after mist to carrier gas, to pass into temperature be that the silica tube 40 of 100 ℃ ~ 220 ℃ generates presomas, wherein the diameter of silica tube 40 is 30mm ~ 150mm, and length is 0.5m ~ 3m, and the flow of carrier gas is 1L/min ~ 15L/min.
Preferably, the diameter of silica tube is 95mm, and length is 1.4m.
In present embodiment, use spraying gun 30 by solution atomization, spraying gun 30 is compression atomizing device.Concrete, the solution of the carrier gas of gas-holder 20 interior storages and container for storing liquid 10 interior storages is together passed into spraying gun 30 and make solution mist change into mist.Carrier gas is rare gas element or reducing gas, as: at least one in nitrogen, argon gas and hydrogen, the flow of carrier gas is 5L/min ~ 8L/min.
Silica tube 40 outer walls are being wound around resistance wire 42.
Solution mist passes into from one end of silica tube 40 after changing into mist, and at the interior generation presoma of silica tube 40, presoma is trickle powder, and pulverous presoma is the other end ejection from silica tube with carrier gas.Further, presoma is used collector 50 to collect after silica tube 40 flows out.In present embodiment, collector 50 is the acidproof filtration funnel of micropore.
S104, presoma is calcined at 600 ℃ ~ 1000 ℃ within 2 hours ~ 5 hours, to obtain chemical formula be GeS
2-Ga
2s
3: xTm
3+thulium doping chalcogenide glass up-conversion luminescent material.
Preferably, presoma is placed in the calcination 3 hours at 800 ℃ of temperature programmed control stove.
The preparation method of above-mentioned thulium doping chalcogenide glass up-conversion luminescent material is spray pyrolysis, and raw material mixes under solution state, can guarantee uniform component distribution, and technological process is simple, component loss is few, can accurately control stoichiometric ratio, is especially applicable to preparing polycomponent composite powder; Micro mist is by being suspended in airborne droplet drying, and particle is generally the spherical of rule, and few reunion, without follow-up washing, grinds, and guarantees the high purity of product, high reactivity; Whole process completed rapidly in short several seconds, so drop has little time to occur solute segregation in reaction process, further guaranteed the homogeneity that component distributes; Reaction process is simple, and a step obtains finished product, and without filtration, washing, dry, crushing process, simple to operation, production process is continuous, and production capacity is large, and production efficiency is high, is very beneficial for large suitability for industrialized production; In the photoluminescence spectra of the thulium doping chalcogenide glass up-conversion luminescent material of preparation, the excitation wavelength 796nm of thulium doping chalcogenide glass up-conversion luminescent material, corresponding respectively at the glow peak of 475nm is Tm
3+ion
1g
4→
3h
6transition radiation form glow peak, by red-green glow, excite and can launch blue light, realized that by the infrared long-wave radiation to green glow, to inspire blue light shortwave luminous.
Refer to Fig. 2, the Organic Light Emitting Diode 100 of one embodiment, this Organic Light Emitting Diode 100 comprises that the substrate 1, metal A g layer negative electrode 2, Ir (piq) 2 (acac) Chinese name that stack gradually close iridium (III) organic luminous layer 3, tin indium oxide ITO transparent anode 4 and tetrafluoroethylene transparent encapsulated layer 5 two (1-phenyl-isoquinoline 99.9) (methyl ethyl diketones).In transparent encapsulated layer 5, be dispersed with thulium doping chalcogenide glass up-conversion luminescent material 6, the chemical formula of thulium doping chalcogenide glass up-conversion luminescent material is GeS
2-Ga
2s
3: xTm
3+, wherein, x is 0.002 ~ 0.06.
In the transparent encapsulated layer 5 of Organic Light Emitting Diode 100, be dispersed with thulium doping chalcogenide glass up-conversion luminescent material 6, the excitation wavelength of thulium doping chalcogenide glass up-conversion luminescent material is 796nm, and corresponding respectively at the glow peak of 475nm is Tm
3+ion
1g
4→
3h
6transition radiation form glow peak, by red-green glow, excite and can launch blue light, blue light mixes the Organic Light Emitting Diode that formation emits white light afterwards with red-green glow.
Be specific embodiment below.
Embodiment 1
Take GeS
2, Ga
2s
3and Tm
2s
3powder, GeS
2, Ga
2s
3and Tm
2s
3the mol ratio of powder is 0.6:0.37:0.03, is dissolved in the solution that is mixed with 1.5mol/L in hydrogen sulfide, and adds the polyoxyethylene glycol additive of 0.01mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 5L/min.It is that the silica tube of 180 ℃ generates presoma that solution presoma enters temperature with argon carrier, and wherein the diameter of silica tube is 95mm, and length is 1.4m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 3 hours, and 800 ℃ of calcining temperatures, obtain 0.6GeS
2-0.37Ga
2s
3: 0.03Tm
3+up-conversion phosphor.
Refer to Fig. 3, the photoluminescence spectra of the thulium doping chalcogenide glass up-conversion luminescent material that in Fig. 3, curve 1 obtains for the present embodiment.As seen from Figure 3, the excitation wavelength of thulium that embodiment 1 obtains doping chalcogenide glass up-conversion luminescent material is 796nm, when material is subject to long wavelength's (as 796nm) radiation, and Tm now
3+ion
1g
4→
3h
6transition, just sends the blue light of 475nm, can be used as blue light emitting material.
Refer to Fig. 4, in Fig. 4, curve is for implementing the Raman spectrum of the thulium doping chalcogenide glass up-conversion luminescent material of 1 preparation, Raman peaks in figure is depicted as germanium sulfide gallium glass characteristic peak, the peak that does not occur doped element and other impurity, illustrates that doped element and substrate material have formed good bonding.
Fig. 5 is the spectrogram that has the Organic Light Emitting Diode comparative example that thulium doping chalcogenide glass up-conversion luminescent material forms in the transparent encapsulated layer of embodiment 1 preparation, and curve 2 is not for adding the fluorescent material in embodiment 1.In figure, can find out, thulium doping chalcogenide glass up-conversion luminescent material can inspire the blue light of shortwave by the red-green glow of long wave, after blue light mixes with red-green glow, forms white light.
Embodiment 2
Take GeS
2, Ga
2s
3and Tm
2s
3powder, GeS
2, Ga
2s
3and Tm
2s
3the mol ratio of powder is 0.4:0.598:0.002, is dissolved in the solution that is mixed with 0.3mol/L in hydrogen sulfide, and adds the polyoxyethylene glycol additive of 0.05mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 15L/min.It is that the silica tube of 220 ℃ generates presoma that solution presoma enters temperature with argon carrier, and wherein the diameter of silica tube is 150mm, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 5 hours, and 1000 ℃ of calcining temperatures, obtain 0.4GeS
2-0.598Ga
2s
3: 0.002Tm
3+up-conversion phosphor.
Embodiment 3
Take GeS
2, Ga
2s
3and Tm
2s
3powder, GeS
2, Ga
2s
3and Tm
2s
3the mol ratio of powder is 0.5:0.44:0.06, is dissolved in the solution that is mixed with 0.05mol/L in hydrogen sulfide, and adds the polyoxyethylene glycol additive of 0.005mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 1L/min.It is that the silica tube of 150 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 2 hours, and 600 ℃ of calcining temperatures, obtain 0.5GeS
2-0.44Ga
2s
3: 0.06Tm
3+up-conversion phosphor.
Embodiment 4
Take GeS
2, Ga
2s
3and Tm
2s
3powder, GeS
2, Ga
2s
3and Tm
2s
3the mol ratio of powder is 0.45:0.54:0.01, is dissolved in the solution that is mixed with 1.5mol/L in hydrogen sulfide, and adds the polyoxyethylene glycol additive of 0.01mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 5L/min.It is that the silica tube of 180 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 3 hours, and 1100 ℃ of calcining temperatures, obtain 0.45GeS
2-0.54Ga
2s
3: 0.01Tm
3+up-conversion phosphor.
Embodiment 5
Take GeS
2, Ga
2s
3and Tm
2s
3powder, GeS
2, Ga
2s
3and Tm
2s
3the mol ratio of powder is 0.46:0.5:0.04, is dissolved in the solution that is mixed with 3mol/L in hydrogen sulfide, and adds the polyoxyethylene glycol additive of 0.05mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 15L/min.It is that the silica tube of 220 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 5 hours, and 1300 ℃ of calcining temperatures, obtain 0.46GeS
2-0.5Ga
2s
3: 0.04Tm
3+up-conversion phosphor.
Embodiment 6
Take GeS
2, Ga
2s
3and Tm
2s
3powder, GeS
2, Ga
2s
3and Tm
2s
3the mol ratio of powder is 0.765:0.2:0.035, is dissolved in the solution that is mixed with 0.5mol/L in hydrogen sulfide, and adds the polyoxyethylene glycol additive of 0.005mol/L.Then solution is put into atomisation unit, to atomisation unit, pass into afterwards the argon gas of 1L/min.It is that the silica tube of 150 ℃ generates presoma that solution presoma enters temperature with argon carrier, the diameter 30mm of silica tube wherein, and length is 3m.Then fluorescent material enters condenser with air-flow, finally collected by the acidproof filtration funnel of micropore.The presoma of collecting fluorescent material, is placed in temperature programmed control stove and calcines 2 hours, and 600 ℃ of calcining temperatures, obtain 0.765GeS
2-0.2Ga
2s
3: 0.035Tm
3+up-conversion phosphor.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a thulium doping chalcogenide glass up-conversion luminescent material, is characterized in that: its chemical formula is GeS
2-Ga
2s
3: xTm
3+, wherein, x is 0.002 ~ 0.06.
2. thulium doping chalcogenide glass up-conversion luminescent material according to claim 1, is characterized in that, x is 0.03.
3. a preparation method for thulium doping chalcogenide glass up-conversion luminescent material, is characterized in that, comprises the following steps:
According to GeS
2-Ga
2s
3: xTm
3+the stoichiometric ratio of each element takes GeS
2, Ga
2s
3and Tm
2s
3powder, wherein, x is 0.002 ~ 0.06;
The powder taking is dissolved in and in hydrogen sulfide, is mixed with the solution that the concentration of metallic cation is 0.05mol/L ~ 3mol/L;
Described solution mist is changed into after mist to carrier gas, to pass into temperature be that the silica tube of 100 ℃ ~ 220 ℃ generates presoma, wherein, the diameter of silica tube is 30mm ~ 150mm, and length is 0.5m ~ 3m, and the flow of carrier gas is 1L/min ~ 15L/min;
Described presoma is calcined at 600 ℃ ~ 1000 ℃ and within 2 hours ~ 5 hours, obtained chemical formula GeS
2-Ga
2s
3: xTm
3+thulium doping chalcogenide glass up-conversion luminescent material.
4. the preparation method of thulium doping chalcogenide glass up-conversion luminescent material according to claim 3, is characterized in that, x is 0.03.
5. the preparation method of thulium according to claim 3 doping chalcogenide glass up-conversion luminescent material, it is characterized in that, the powder taking is dissolved in to the step that is mixed with solution in hydrogen sulfide also to be comprised: in described solution, add dispersion agent, the concentration of described dispersion agent is 0.005mol/L ~ 0.05mol/L.
6. the preparation method of thulium doping chalcogenide glass up-conversion luminescent material according to claim 5, is characterized in that, described dispersion agent is polyoxyethylene glycol.
7. the preparation method of thulium according to claim 3 doping chalcogenide glass up-conversion luminescent material, it is characterized in that, the step that described solution mist is changed into mist is, carrier gas and described solution are passed into together in spraying gun and makes described solution mist change into mist, and described carrier gas is rare gas element or reducing gas.
8. the preparation method of thulium doping chalcogenide glass up-conversion luminescent material according to claim 7, is characterized in that, the flow of described carrier gas is 5L/min ~ 8L/min.
9. an Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, it is characterized in that, in described transparent encapsulated layer, doped with thulium doping chalcogenide glass up-conversion luminescent material, the chemical general formula of described thulium doping chalcogenide glass up-conversion luminescent material is GeS
2-Ga
2s
3: xTm
3+, wherein, x is 0.002 ~ 0.06.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, x is 0.03.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353578A (en) * | 2008-09-05 | 2009-01-28 | 浙江大学 | Upconversion luminescent material |
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2013
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353578A (en) * | 2008-09-05 | 2009-01-28 | 浙江大学 | Upconversion luminescent material |
Non-Patent Citations (1)
| Title |
|---|
| JAY HYOK SONG ET AL: "Effect of CsBr addition on the emission properties of Tm3+ ion in Ge-Ga-S glass", 《JOURNAL OF MATERIALS RESEARCH》 * |
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Application publication date: 20140716 |