CN104449723B - A kind of boron phosphate luminescent powder of transmitting green fluorescence and its preparation method and application - Google Patents
A kind of boron phosphate luminescent powder of transmitting green fluorescence and its preparation method and application Download PDFInfo
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- CN104449723B CN104449723B CN201410820995.6A CN201410820995A CN104449723B CN 104449723 B CN104449723 B CN 104449723B CN 201410820995 A CN201410820995 A CN 201410820995A CN 104449723 B CN104449723 B CN 104449723B
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Abstract
The present invention relates to borate fluorescent powder of a kind of transmitting green fluorescence and its preparation method and application, the chemical composition formula of this fluorescent material is: (Ln1‑xTbx)7O6(BO3)(PO4)2, in formula, Ln is rare earth element, 0.01≤x≤0.1.The preparation method of the boron phosphate luminescent powder of this transmitting green fluorescence, comprises the following steps: (a) uses NH4H2PO4、H3BO3、Ln2O3And Tb4O7For raw material, grind be placed in the alumina crucible added a cover at 300 ~ 500 DEG C reacting by heating 6 ~ 12 hours head product；B () is pressed into the disk of a diameter of 1 ~ 5 centimetre after being ground by above-mentioned reaction head product, be placed in the platinum crucible added a cover；C platinum crucible is placed in the heating furnace containing carbon dust by (), natural cooling after calcining 12 ~ 30 hours at 1000 ~ 1500 DEG C.Due to terbium ion outer-shell electron5D4→7F5Magnetic dipole transition so that this boron phosphate luminescent powder transmitting green fluorescence.The equipment that the preparation method of the boron phosphate luminescent powder of transmitting green fluorescence of the present invention uses is simple, operation safety, condition are easily controlled, the reliable product quality prepared.
Description
Technical field
The present invention relates to a kind of boron phosphate luminescent powder, be specifically related to a kind of at X-ray, boron phosphate luminescent powder of burst of ultraviolel or vacuum ultraviolet-excited lower transmitting green fluorescence and its preparation method and application.
Background technology
Along with computer, the communication information network as core universal, and the rapid expansion in personal digital assistant device product market, the flat faced display as man-machine video clip shows good market prospect, becomes one of electronics field of attracting people's attention most.Wherein plasma flat-plate show (PDP) owing to its volume is little, light weight, ultrathin type, without x-ray radiation, be unaffected by the magnetic field, big visual angle, vertiginous picture fast response time etc. be a little subject to people's attention.Plasma flat-plate shows it is to utilize gas discharge to produce vacuum ultraviolet, excites three primary colors fluorescent powder to realize the device of display.The three primary colors fluorescent powder reaching commercial use at present mainly has: red Y2O3:Eu3+, (Y, Gd) BO3:Eu3+、Y2O2S:Eu3+, green: Zn2SiO4:Mn2+、BaAl12O19:Mn2+With blue BaAl14O23:Eu2+、BaMgAl10O17:Eu2+, the preparation method of these vacuum ultraviolet luminescent materials is always one of important directions of people's research.But blue and green emitting phosphor still uses the fluorescent material of non-rare earth, and this luminous efficiency allowing for these fluorescent material is relatively low, it is therefore necessary to develop a kind of new and effective rare earth green fluorescent material.
And for radioscopic image is converted to visual image during medical X-ray photograph, intensifying screen need to be used.The green glow intensifying screen using x-ray excited also has multiple, and wherein high sensitivity intensifying screen uses Gd2O2S∶Tb3+、GdTa04:Tb3+, Gd3GaO12: Tb3+Fluorescent material, but these fluorescent material is mainly with rare earth oxide (Gd2O3) it is raw material, this makes holding at high price of it.All of everything all make to develop a kind of reasonable price, the novel rare earth green fluorescent material again with excellent luminance performance simultaneously becomes a kind of inevitable.
Summary of the invention
The invention aims to overcome the deficiencies in the prior art to provide one to be applicable in X-ray, burst of ultraviolel or the boron phosphate luminescent powder of vacuum ultraviolet-excited lower transmitting green fluorescence.
For reaching above-mentioned purpose, the technical solution used in the present invention is: the boron phosphate luminescent powder of a kind of transmitting green fluorescence, and its chemical composition formula is:
(Ln1-xTbx)7O6(BO3)(PO4)2, in formula, Ln is rare earth element, 0.01≤x≤0.1.
Optimally, one or several the combination during described Ln is La, Gd, Yb and Lu.
Optimally, described x is 0.05 ~ 0.08.
It is a further object of the present invention to provide the preparation method of the boron phosphate luminescent powder of a kind of transmitting green fluorescence, it comprises the following steps:
A () uses NH4H2PO4、H3BO3、Ln2O3And Tb4O7For raw material, press (Ln1-xTbx)7O6(BO3)(PO4) dispensing, grind be placed in the alumina crucible added a cover at 300 ~ 500 DEG C reacting by heating 6 ~ 12 hours head product；
B () is pressed into the disk of a diameter of 1 ~ 5 centimetre after being ground by the head product obtained in step (a), be placed in the platinum crucible added a cover；
C platinum crucible in step (b) is placed in the heating furnace containing carbon dust by (), natural cooling after calcining 12 ~ 30 hours at 1000 ~ 1500 DEG C.
Optimally, in described step (b), the pressure of head product tabletted is 150 ~ 200Mpa.
Optimally, in described step (c), carbon dust excess.
Another object of the present invention is to provide the application in plasma flat-plate shows of the boron phosphate luminescent powder of a kind of transmitting green fluorescence, can be used for plasma panel display, room lighting daylight lamp, lampion, black light lamp and as aspects such as x-ray excited intensifying screens.
Owing to technique scheme is used, the present invention compared with prior art has the advantage that green emitting phosphor prepared by the present invention is rare earth luminous preferable substrate due to many rare earth-boron phosphate, and easily realize the doping of other rare earth, provide conveniently for the luminescent material that exploration discovery is novel, so the present invention select rare earth-boron phosphate as substrate, with Tb3+Part replacement rare earth ion is as activator, it is achieved thereby that the guarantee of luminescent properties.
The preparation method of the boron phosphate luminescent powder of transmitting green fluorescence of the present invention compared with prior art has the advantage that (1) equipment is simple, and conveniently, safely, condition is easily controlled, and raw material is easy to get, and cost is relatively low, it is simple to produce in a large number in operation；(2) method using the carbon reduction of original creation can go back raw sample effectively, it is thus achieved that efficient luminescent material, moreover it is possible to avoids using tradition H2The potential safety hazard that reduction brings.
Accompanying drawing explanation
Accompanying drawing 1 is the green emitting phosphor that provides of present invention emission spectrum under x-ray excited.
Accompanying drawing 2 is green emitting phosphor the exciting (λ em=544nm) and launching (λ exc=172 nm) spectrum and vacuum ultraviolet-excited fluorescence spectrum at VUV wave band that the present invention provides；
Accompanying drawing 3 is green emitting phosphor the exciting (λ em=544nm) and launching (λ exc=172 nm) spectrum and vacuum ultraviolet-excited fluorescence spectrum at ultraviolet band that the present invention provides；
Accompanying drawing 4 is that the green emitting phosphor that provides of the present invention is at different Tb3+Emission spectrum under doping content compares；
Accompanying drawing 5 is relative luminance and the Tb of the green emitting phosphor that the present invention provides3+The graph of relation of doping, abscissa is Tb3+Priority doping, vertical coordinate is relative luminance.
Detailed description of the invention
Below will the present invention is described in detail by specific embodiment.
The boron phosphate luminescent powder of transmitting green fluorescence of the present invention, its chemical composition formula is: (Ln1-xTbx)7O6(BO3)(PO4)2, in formula, Ln is rare earth element, 0.01≤x≤0.1.Owing to this borate fluorescent powder with the addition of borate and phosphate simultaneously so that boron element and P elements produce cooperative effect；And rare earth element ion and Tb3+Corresponding Resonance energy transfer can be produced, be so conducive to terbium ion outer-shell electron5D4→7F5Magnetic dipole transition so that this borate fluorescent powder transmitting green fluorescence.Ln is preferably the combination of one or several in Gd, La, Yb and Lu, thus improves itself and Tb3+Suitability.Tb3+Content x be 0.05 ~ 0.08 because working as Tb as can see from Figure 53+Content x when being 0.05 ~ 0.08, the relative luminous intensity of boron phosphate luminescent powder is the highest.
The preparation method of above-mentioned boron phosphate luminescent powder, it comprises the following steps:
Initially with NH4H2PO4、H3BO3、Ln2O3(Ln is one or several the combination in La, Gd, Yb and Lu) and Tb4O7For raw material, press (Ln1-xTbx)7O6(BO3)(PO4)2(0.01≤x≤0.1) stoichiometric proportion carries out dispensing, grinds and is placed in the alumina crucible added a cover reacting by heating at 300 ~ 500 DEG C and obtains head product in 6 ~ 12 hours；NH4H2PO4、H3BO3、Ln2O3And Tb4O7These costs of material are relatively low and are easily obtained, and this step reaction condition is easily controlled.
Then it is pressed into the disk (head product is pressed into the pressure of disk and is preferably 150 ~ 200Mpa) of a diameter of 1 ~ 5 centimetre after being ground by the head product obtained in the first step, is placed in the platinum crucible added a cover；It is pressed into disk after being ground by head product, it is possible to reduce the response time, uses platinum crucible can be prevented effectively from the pollution of carbon dust, prepared reliable product quality.
The platinum crucible that finally will be equipped with disk is placed in the heating furnace containing carbon dust (excessive), natural cooling after calcining 12 ~ 30 hours at 1000 ~ 1500 DEG C.
The boric acid microcosmic salt fluorescent material of above-mentioned transmitting green fluorescence can be used for plasma panel display, room lighting daylight lamp, lampion, black light lamp and as aspects such as medical X-ray intensifying screens.
Below in conjunction with accompanying drawing, by specific embodiment, the present invention is described in detail.
Embodiment 1
The present embodiment provides a kind of boron phosphate luminescent powder, and its chemical formula is: Gd6.3Tb0.7O6(BO3)(PO4)2, in order to prepare this fluorescent material, concrete operations are: weigh NH4H2PO4(analytical pure) 1.38g, H3BO3(analytical pure) 0.37g, Gd2O3(99.99%) 6.85g and Tb4O7(99.99%) 0.785g, is fully ground mix homogeneously in agate mortar, is subsequently placed in alumina crucible and close the cover is put in Muffle furnace and heated 6 hours at 500 DEG C；Subsequently the head product after reacting by heating is placed in agate mortar and is fully ground, pour the disk being pressed into a diameter of 5 centimetres in tablet machine under 150MPa again into, disk is placed in the platinum crucible added a cover, subsequently platinum crucible is placed in the Muffle furnace containing a large amount of carbon dusts, it is warming up to 1000 DEG C with the speed of 5 DEG C per minute, after calcining 30 hours, naturally cools to room temperature.
Embodiment 2
The present embodiment provides a kind of boron phosphate luminescent powder, and its chemical formula is: Gd6.93Tb0.07O6(BO3)(PO4)2, in order to prepare this fluorescent material, concrete operations are: weigh NH4H2PO4(analytical pure) 1.38 g, H3BO3(analytical pure) 0.37 g, Gd2O3(99.99%) 7.53 g and Tb4O7(99.99%) 0.079 g, is fully ground mix homogeneously in agate mortar, is subsequently placed in alumina crucible and close the cover is put in Muffle furnace and heated 12 hours at 300 DEG C；Subsequently the head product after reacting by heating is placed in agate mortar and is fully ground, pour the disk being pressed into a diameter of 1 centimetre in tablet machine under 200MPa again into, disk is placed in the platinum crucible added a cover, subsequently platinum crucible is placed in the Muffle furnace containing a large amount of carbon dusts, it is warming up to 1500 DEG C with the speed of 10 DEG C per minute, after calcining 12 hours, naturally cools to room temperature.
Embodiment 3
The present embodiment provides a kind of boron phosphate luminescent powder, and its chemical formula is: Gd6.65Tb0.35O6(BO3)(PO4)2, in order to prepare this fluorescent material, concrete operations are: weigh NH4H2PO4(analytical pure) 1.38 g, H3BO3(analytical pure) 0.37 g, Gd2O3(99.99%) 7.23 g and Tb4O7(99.99%) 0.39 g, is fully ground mix homogeneously in agate mortar, is subsequently placed in alumina crucible and close the cover is put in Muffle furnace and heated 10 hours at 400 DEG C；Subsequently the head product after reacting by heating is placed in agate mortar and is fully ground, then pour in tablet machine 180
It is pressed into the disk of a diameter of 2 centimetres under MPa, disk is placed in the platinum crucible added a cover, subsequently platinum crucible is placed in the Muffle furnace containing a large amount of carbon dusts, is warming up to 1200 DEG C with the speed of 15 DEG C per minute, after calcining 20 hours, naturally cool to room temperature.
Embodiment 4
The present embodiment provides a kind of boron phosphate luminescent powder, and its chemical formula is: Yb6.65Tb0.35O6(BO3)(PO4)2, its preparation method is roughly the same with the preparation method in embodiment 3, except for the difference that have employed Yb2O3(99.99%) 7.23 g.
Embodiment 5
The present embodiment provides a kind of boron phosphate luminescent powder, and its chemical formula is: La6.65Tb0.35O6(BO3)(PO4)2, its preparation method is roughly the same with the preparation method in embodiment 3, except for the difference that have employed La2O3(99.99%) 7.23 g.
Embodiment 6
The present embodiment provides a kind of boron phosphate luminescent powder, and its chemical formula is: Lu6.65Tb0.35O6(BO3)(PO4)2, its preparation method is roughly the same with the preparation method in embodiment 3, except for the difference that have employed Lu2O3(99.99%) 7.23 g.
Embodiment 7
The present embodiment provides a kind of boron phosphate luminescent powder, and its chemical formula is: Gd6.79Tb0.21O6(BO3)(PO4)2, in order to prepare this fluorescent material, concrete operations are: weigh NH4H2PO4(analytical pure) 1.38g, H3BO3(analytical pure) 0.37 g, Gd2O3(99.99%) 7.38 g and Tb4O7(99.99%) 0.235 g, is fully ground mix homogeneously in agate mortar, is subsequently placed in alumina crucible and close the cover is put in Muffle furnace and heated 10 hours at 400 DEG C；Subsequently the head product after reacting by heating is placed in agate mortar and is fully ground, then pour in tablet machine 180
It is pressed into the disk of a diameter of 2 centimetres under MPa, disk is placed in the platinum crucible added a cover, subsequently platinum crucible is placed in the Muffle furnace containing a large amount of carbon dusts, is warming up to 1200 DEG C with the speed of 15 DEG C per minute, after calcining 20 hours, naturally cool to room temperature.
Embodiment 8
The present embodiment provides a kind of boron phosphate luminescent powder, and its chemical formula is: Gd6.44Tb0.56O6(BO3)(PO4)2, in order to prepare this fluorescent material, concrete operations are: weigh NH4H2PO4(analytical pure) 1.38 g, H3BO3(analytical pure) 0.37 g, Gd2O3(99.99%) 7.00 g and Tb4O7(99.99%) 0.628 g, is fully ground mix homogeneously in agate mortar, is subsequently placed in alumina crucible and close the cover is put in Muffle furnace and heated 10 hours at 400 DEG C；Subsequently head product after reacting by heating is placed in agate mortar and is fully ground, then pour in tablet machine 180
It is pressed into the disk of a diameter of 2 centimetres under MPa, disk is placed in the platinum crucible added a cover, subsequently platinum crucible is placed in the Muffle furnace containing a large amount of carbon dusts, is warming up to 1200 DEG C with the speed of 15 DEG C per minute, after calcining 20 hours, naturally cool to room temperature.
Borate fluorescent powder in embodiment 1, embodiment 2, embodiment 3, embodiment 7 and embodiment 8 is excited under VUV 172nm generation fluorescence, and its relative luminance is listed in Fig. 5.When curve from Fig. 5 is it can be seen that the content y of Tb is gradually increased in the range of 0.01 ~ 0.08, the relative luminance of borate fluorescent powder is also gradually increased；And the content y of Tb by 0.08 to 0.1 be gradually increased again time, the relative luminance of borate fluorescent powder is gradually lowered.
Above-described embodiment only for technology design and the feature of the present invention are described, its object is to allow person skilled in the art will appreciate that present disclosure and to implement according to this, can not limit the scope of the invention with this.All equivalence changes made according to spirit of the invention or modification, all should contain within protection scope of the present invention.
Claims (6)
1. the boron phosphate luminescent powder of a transmitting green fluorescence, it is characterised in that its chemical composition formula is:
(Ln1-xTbx)7O6(BO3)(PO4)2, in formula, Ln is Lu, 0.01≤x≤0.1.
The boron phosphate luminescent powder of transmitting green fluorescence the most according to claim 1, it is characterised in that: described x is 0.05 ~ 0.08.
3. the preparation method of the boron phosphate luminescent powder of arbitrary described transmitting green fluorescence in claim 1 to 2, it is characterised in that it comprises the following steps:
A () uses NH4H2PO4、H3BO3、Ln2O3And Tb4O7For raw material, press (Ln1-xTbx)7O6(BO3)(PO4)2Dispensing, grind be placed in the alumina crucible added a cover at 300 ~ 500 DEG C reacting by heating 6 ~ 12 hours head product；
B () is pressed into the disk of a diameter of 1 ~ 5 centimetre after being ground by the head product obtained in step (a), be placed in the platinum crucible added a cover；
C platinum crucible in step (b) is placed in the heating furnace containing carbon dust by (), natural cooling after calcining 12 ~ 30 hours at 1000 ~ 1500 DEG C.
The preparation method of the boron phosphate luminescent powder of transmitting green fluorescence the most according to claim 3, it is characterised in that: in described step (b), it is 150 ~ 200Mpa that head product is pressed into the pressure of disk.
The preparation method of the boron phosphate luminescent powder of transmitting green fluorescence the most according to claim 3, it is characterised in that: in described step (c), carbon dust excess.
6. the boron phosphate luminescent powder of transmitting green fluorescence described in claim 1 is at plasma panel display, room lighting daylight lamp, lampion, black light lamp and as the application in terms of medical X-ray degree intensifying screen.
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| CN109929555B (en) * | 2018-12-25 | 2022-01-18 | 云南大学 | White boron phosphate fluorescent powder and preparation method and application thereof |
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| CN110003904A (en) * | 2019-04-04 | 2019-07-12 | 云南大学 | A kind of Ce boron phosphorus doped hydrochlorate ultraviolet fluorescence powder and preparation method thereof |
| CN110003905A (en) * | 2019-04-04 | 2019-07-12 | 云南大学 | A kind of Pr activation borophosphate red fluorescence powder and preparation method thereof |
| CN110846034B (en) * | 2019-11-22 | 2022-09-09 | 云南大学 | Dy 3+ Activated fluorescent powder and preparation method thereof |
| CN113999676A (en) * | 2021-11-25 | 2022-02-01 | 济南鲁新新型建材股份有限公司 | Boron-doped calcium phosphate cerium fluorescent powder and preparation method and application thereof |
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