CN104212453A - Praseodymium doped oxygen yttrium silicate up-conversion luminescent material, preparation method, and applications thereof - Google Patents

Praseodymium doped oxygen yttrium silicate up-conversion luminescent material, preparation method, and applications thereof Download PDF

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Publication number
CN104212453A
CN104212453A CN201310206369.3A CN201310206369A CN104212453A CN 104212453 A CN104212453 A CN 104212453A CN 201310206369 A CN201310206369 A CN 201310206369A CN 104212453 A CN104212453 A CN 104212453A
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luminescent material
conversion luminescent
silicic acid
acid oxygen
praseodymium doped
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周明杰
陈吉星
王平
冯小明
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention discloses a praseodymium doped oxygen yttrium silicate up-conversion luminescent material, which is represented by a chemical formula Me2Y8(SiO4)6O2:xPr3+, wherein the x is in a range of 0.01 to 0.08, and the Me represents a magnesium element, a calcium element, a strontium element, or a barium element. In the photoluminescence spectrum of the up-conversion luminescent material, the excitation wavelength of the up-conversion luminescent material is at 578 nm, a luminescent peak is formed in the 483nm wavelength zone by transition radiation of Pr3+ ion from the 3P0 to 3H4, and the up-conversion luminescent material can be used as a blue light luminescent material. The invention also provides a preparation method of the up-conversion luminescent material, and an organic light emitting diode using the up-conversion luminescent material.

Description

Praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material, preparation method and application thereof
Technical field
The present invention relates to a kind of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material, preparation method and Organic Light Emitting Diode.
Background technology
Organic Light Emitting Diode (OLED) because unit construction is simple, the characteristic such as cheap, the luminous of production cost, reaction times is short, flexible, and obtain a very wide range of application.But because the OLED blue light material obtaining stability and high efficiency is at present more difficult, significantly limit the development of white light OLED device and light source industry.
Upconverting fluorescent material can launch visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in the field such as optical fiber communication technology, fibre amplifier, 3 D stereo display, biomolecules fluorescence labelling, infrared detective.But, can by infrared, the long-wave radiations such as red-green glow inspire the praseodymium doped silicic acid oxygen yttrium 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 inspire the praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material of blue light, preparation method by long-wave radiation and use the Organic Light Emitting Diode of this praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material.
A kind of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material, its chemical formula is Me 2y 8(SiO 4) 6o 2: xPr 3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
Described x is 0.05.
A preparation method for praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material, comprises the following steps:
Step one, according to Me 2y 8(SiO 4) 6o 2: xPr 3+the stoichiometric ratio of each element takes MeO, Y 2o 3, SiO and Pr 2o 3powder, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element;
Step 2, the powder taken mixed obtain presoma in described step one;
Step 3, by the calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C of the presoma in described step 2,
Step 4, the precursor after process in described step 3 is cooled to 100 DEG C ~ 300 DEG C, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is Me 2y 8(SiO 4) 6o 2: xPr 3+praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material.
Described MeO, Y 2o 3, SiO and Pr 2o 3the each component molar of powder is than being 2:4:6:(0.01 ~ 0.08).
Described MeO, Y 2o 3, SiO and Pr 2o 3the each component molar of powder is than being 2:4:6:0.05.
Described in step 2, mixing is that described powder is ground 20 minutes ~ 60 minutes in corundum alms bowl.
By the calcination 3 hours at 950 DEG C of described presoma in step 3.
Cooling temperature in step 4 is 200 DEG C, and soaking time is 2 hours.
A kind of 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, be dispersed with praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material is Me 2y 8(SiO 4) 6o 2: xPr 3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
X is 0.05.
The preparation method of above-mentioned praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material is comparatively simple, and cost is lower, produces, comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of the praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material of preparation, the excitation wavelength of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr 3+ion 3p 0→ 3h 4transition radiation formed glow peak, can as blue light emitting material.
Accompanying drawing explanation
Fig. 1 is the structural representation of the Organic Light Emitting Diode of an embodiment.
Fig. 2 is the photoluminescence spectrogram of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material prepared by embodiment 1.
Fig. 3 is the XRD spectra of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material prepared by embodiment 1.
Fig. 4 is the spectrogram forming the Organic Light Emitting Diode emitted white light in the transparent encapsulated layer of embodiment 1 preparation doped with praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material material.
Embodiment
Below in conjunction with the drawings and specific embodiments, praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material and preparation method thereof is illustrated further.
The praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material of one embodiment, its chemical formula is Me 2y 8(SiO 4) 6o 2: xPr 3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
Preferably, x is 0.05.
In the photoluminescence spectra of this praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material, the excitation wavelength of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material is 578nm, when material is subject to the radiation of long wavelength (as 578nm) time, and Pr 3+ion has just been in 3p 0excited state, then to 3h 4transition, just sends the blue light of 483nm, can as blue light emitting material.
The preparation method of above-mentioned praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material, comprises the following steps:
Step S11, according to Me 2y 8(SiO 4) 6o 2: xPr 3+the stoichiometric ratio of each element takes MeO, Y 2o 3, SiO and Pr 2o 3powder, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
In this step, described MeO, Y 2o 3, SiO and Pr 2o 3the each component molar of powder is than being 2:4:6:(0.01 ~ 0.08).
In this step, preferred MeO, Y 2o 3, SiO and Pr 2o 3the each component molar of powder is than being 2:4:6:0.05.
Step S13, the powder taken mixed obtain presoma in step S11.
In this step, powder is ground in corundum alms bowl the presoma obtaining mixing for 20 minutes ~ 60 minutes, preferred grinding 40 minutes.
Step S15, by presoma calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C,
Preferably, presoma calcination 3 hours at 950 DEG C.
Step S17, be cooled to 100 DEG C ~ 500 DEG C by after the precursor after process in step S15, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is Me 2y 8(SiO 4) 6o 2: xPr 3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
Preferably, the precursor after process in step S15 is cooled to 200 DEG C, then is incubated 2 hours.
The preparation method of above-mentioned praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material is comparatively simple, and cost is lower, produces, comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of the praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material of preparation, the excitation wavelength of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material is 578nm, in 483nm wavelength zone by Pr 3+ion 3p 0→ 3h 4transition radiation formed glow peak, can as blue light emitting material.
Refer to Fig. 1, the Organic Light Emitting Diode 100 of an embodiment, this Organic Light Emitting Diode 100 comprises the substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the transparent encapsulated layer 5 that stack gradually.Be dispersed with praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material is Me 2y 8(SiO 4) 6o 2: xPr 3+wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element, the organic luminous layer 3 in this device sends red-green glow, part red-green glow excites in transparent encapsulated layer 5 and is dispersed with praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material 6 and sends blue light, and last redgreenblue just blendes together white light.
Be specific embodiment below.
Embodiment 1
Select purity be 99.99% powder, by MgO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol and 0.08mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, then 200 DEG C are cooled to be incubated 2 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Mg 2y 8(SiO 4) 6o 2: 0.08Pr 3+up-conversion phosphor.
Process prepared by Organic Light Emitting Diode:
The substrate 1 stacked gradually uses soda-lime glass, negative electrode 2 uses metal A g layer, organic luminous layer 3 uses Ir (piq) 2 (acac) Chinese name (methyl ethyl diketone) closes iridium (III), transparent anode 4 uses tin indium oxide ITO two (1-phenyl-isoquinoline 99.9), and transparent encapsulated layer 5 tetrafluoroethylene.Be dispersed with praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material 6 in transparent encapsulated layer 5, the chemical formula of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material is Mg 2y 8(SiO 4) 6o 2: 0.08Pr 3+.
Refer to Fig. 2, Figure 2 shows that the photoluminescence spectra figure of the praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material obtained.As seen from Figure 2, the excitation wavelength of the praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material that the present embodiment obtains is 578nm, in 483nm wavelength zone by Pr 3+ion 3p 0→ 3h 4transition radiation formed glow peak, this praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve is the XRD curve of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material prepared by enforcement 1, test comparison standard P DF card.Contrast PDF card, can find out and can find out that all diffraction peaks are all the crystallization phasess of corresponding silicic acid oxygen yttrium, and does not have doped element and other dephasign to occur, illustrates that the product that this preparation method obtains has good crystalline quality.
Refer to Fig. 4, Fig. 4 curve 1 is the spectrogram forming the Organic Light Emitting Diode emitted white light in transparent encapsulated layer doped with praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material material, and curve 2 is not doped with the contrast of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material material in transparent encapsulated layer.Can find out in figure, fluorescent material by the red light of long wave, can inspire the blue light of shortwave, blendes together white light.
Embodiment 2
Select purity be 99.99% powder, by MgO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.05mmol grinds and makes its Homogeneous phase mixing in 20 minutes in corundum mortar, then calcination 3 hours at 800 DEG C in retort furnace, be then cooled to 250 DEG C to be incubated 2 hours, then furnace cooling takes out to room temperature, obtain block materials, can obtain chemical general formula after pulverizing is Mg 2y 8(SiO 4) 6o 2: 0.05Pr 3+up-conversion phosphor.
Embodiment 3
Select purity be 99.99% powder, by MgO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.01mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, be then cooled to 250 DEG C to be incubated 2 hours, then furnace cooling takes out to room temperature, obtain block materials, can obtain chemical general formula after pulverizing is Mg 2y 8(SiO 4) 6o 2: 0.01Pr 3+up-conversion phosphor.
Embodiment 4
Select purity be 99.99% powder, by CaO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.08mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, be then cooled to 250 DEG C to be incubated 2 hours, then furnace cooling takes out to room temperature, obtain block materials, can obtain chemical general formula after pulverizing is Ca 2y 8(SiO 4) 6o 2: 0.08Pr 3+up-conversion phosphor.
Embodiment 5
Select purity be 99.99% powder, by CaO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.05mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 5 hours at 800 DEG C in retort furnace, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Ca 2y 8(SiO 4) 6o 2: 0.05Pr 3+up-conversion phosphor.
Embodiment 6
Select purity be 99.99% powder, by CaO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.01mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, be then cooled to 500 DEG C to be incubated 0.5 hour, then furnace cooling takes out to room temperature, obtain block materials, can obtain chemical general formula after pulverizing is Ca 2y 8(SiO 4) 6o 2: 0.01Pr 3+up-conversion phosphor.
Embodiment 7
Select purity be 99.99% powder, by SrO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.08mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, be then cooled to 250 DEG C to be incubated 2 hours, then furnace cooling takes out to room temperature, obtain block materials, can obtain chemical general formula after pulverizing is Sr 2y 8(SiO 4) 6o 2: 0.08Pr 3+up-conversion phosphor.
Embodiment 8
Select purity be 99.99% powder, by SrO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.05mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 5 hours at 800 DEG C in retort furnace, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Sr 2y 8(SiO 4) 6o 2: 0.05Pr 3+up-conversion phosphor.
Embodiment 9
Select purity be 99.99% powder, by SrO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.01mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, be then cooled to 500 DEG C to be incubated 0.5 hour, then furnace cooling takes out to room temperature, obtain block materials, can obtain chemical general formula after pulverizing is Sr 2y 8(SiO 4) 6o 2: 0.01Pr 3+up-conversion phosphor.
Embodiment 10
Select purity be 99.99% powder, by BaO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.08mmol grinds and makes its Homogeneous phase mixing in 40 minutes in corundum mortar, then calcination 3 hours at 950 DEG C in retort furnace, be then cooled to 250 DEG C to be incubated 2 hours, then furnace cooling takes out to room temperature, obtain block materials, can obtain chemical general formula after pulverizing is Ba 2y 8(SiO 4) 6o 2: 0.08Pr 3+up-conversion phosphor.
Embodiment 11
Select purity be 99.99% powder, by BaO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.05mmol, in corundum mortar, grinding makes its Homogeneous phase mixing in 20 minutes, then calcination 5 hours at 800 DEG C in retort furnace, then 100 DEG C are cooled to be incubated 3 hours, furnace cooling takes out to room temperature again, and obtain block materials, can obtain chemical general formula after pulverizing is Ba 2y 8(SiO 4) 6o 2: 0.05Pr 3+up-conversion phosphor.
Embodiment 12
Select purity be 99.99% powder, by BaO, Y 2o 3, SiO and Pr 2o 3the each component of powder is 2mmol by mole number, 4mmol, 6mmol, 0.01mmol grinds and makes its Homogeneous phase mixing in 60 minutes in corundum mortar, then calcination 3 hours at 1000 DEG C in retort furnace, be then cooled to 500 DEG C to be incubated 0.5 hour, then furnace cooling takes out to room temperature, obtain block materials, can obtain chemical general formula after pulverizing is Ba 2y 8(SiO 4) 6o 2: 0.01Pr 3+up-conversion phosphor.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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 praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material, is characterized in that: its chemical general formula is Me 2y 8(SiO 4) 6o 2: xPr 3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
2. praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material according to claim 1, it is characterized in that, described x is 0.05.
3. a preparation method for praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material, is characterized in that, comprise the following steps:
Step one, according to Me 2y 8(SiO 4) 6o 2: xPr 3+the stoichiometric ratio of each element takes MeO, Y 2o 3, SiO and Pr 2o 3powder, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element;
Step 2, the powder taken mixed obtain presoma in described step one;
Step 3, by the calcination 0.5 hour ~ 5 hours at 800 DEG C ~ 1000 DEG C of described presoma,
Step 4, the precursor after process in described step 3 is cooled to 100 DEG C ~ 300 DEG C, then be incubated 0.5 hour ~ 3 hours, cool to room temperature, obtaining chemical general formula is Me 2y 8(SiO 4) 6o 2: xPr 3+praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material.
4. the preparation method of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material according to claim 3, is characterized in that, described MeO, Y 2o 3, SiO and Pr 2o 3the each component molar of powder is than being 2:4:6:(0.01 ~ 0.08).
5. the preparation method of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material according to claim 3, is characterized in that, described MeO, Y 2o 3, SiO and Pr 2o 3the each component molar of powder is than being 2:4:6:0.05.
6. the preparation method of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material according to claim 3, is characterized in that, described in step 2, mixing is that described powder is ground 20 minutes ~ 60 minutes in corundum alms bowl.
7. the preparation method of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material according to claim 3, is characterized in that, by the calcination 3 hours at 950 DEG C of described presoma in step 3.
8. the preparation method of praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material according to claim 3, it is characterized in that, the cooling temperature in step 4 is 200 DEG C, and soaking time is 2 hours.
9. an Organic Light Emitting Diode, this Organic Light Emitting Diode comprises the substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, it is characterized in that, be dispersed with praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material in described transparent encapsulated layer, the chemical formula of described praseodymium doped silicic acid oxygen yttrium up-conversion luminescent material is Me 2y 8(SiO 4) 6o 2: xPr 3+, wherein, x is 0.01 ~ 0.08, Me is magnesium elements, calcium constituent, the one in strontium element and barium element.
10. Organic Light Emitting Diode according to claim 9, is characterized in that, described x is 0.05.
CN201310206369.3A 2013-05-29 2013-05-29 Praseodymium doped oxygen yttrium silicate up-conversion luminescent material, preparation method, and applications thereof Pending CN104212453A (en)

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Application publication date: 20141217