CN110016343A - A kind of bismuth doped crystal and preparation method thereof having both long afterglow and mechanoluminescence - Google Patents
A kind of bismuth doped crystal and preparation method thereof having both long afterglow and mechanoluminescence Download PDFInfo
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- CN110016343A CN110016343A CN201910283072.4A CN201910283072A CN110016343A CN 110016343 A CN110016343 A CN 110016343A CN 201910283072 A CN201910283072 A CN 201910283072A CN 110016343 A CN110016343 A CN 110016343A
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Abstract
The present invention discloses a kind of bismuth doped crystal and preparation method thereof for having both long afterglow and mechanoluminescence.The chemical formula of the crystal is Sr:Y:Ge:O:Bi=3:2:3:12:x, 0 < x≤3%.Preparation method is to be weighed by each element mol ratio containing strontium, containing yttrium, germanic and bismuth-containing compound as raw material, and raw material is mixed, is calcined, cooling.Material of the present invention is with Bi3+Excitation band for active ions, ultraviolet excitation is wider, has strong absorb in 240-450nm；By changing excitation wavelength, luminescent color is adjustable to orange red region in yellow green.Material after-glow brightness of the invention is high, the time is long, it is ultraviolet to detect twilight sunset near infrared band, in addition to luminescence generated by light and it is long-persistence luminous other than, crystal of the invention has application prospect there is also mechanoluminescence phenomenon, in the detection fields such as stress intensity and its distribution.And synthetic method is simple, is convenient for large-scale production.
Description
Technical field
The invention belongs to the technical fields of luminescent material, and in particular to a kind of bismuth doping for having both long afterglow and mechanoluminescence
Crystal and preparation method thereof.
Background technique
Long after glow luminous material is otherwise known as and stores up light type luminescent material, belongs to one kind of embedded photoluminescent material.It can be by
Extraneous high-energy radiation, which excites, simultaneously gets up its energy storage, after excitaton source is closed, stored by energy it is slow in the form of light
Ground releases, and such shine can continue several seconds, a few houres even several days.For certain long-afterglow materials, also
Along with the generation of mechanoluminescence.Mechanoluminescence, i.e. material are under mechanical external force (frictional force, pressure, impact force etc.) effect
Luminescence phenomenon.With continuous exploration in recent decades, researchers have discovered that a variety of crystalline substances with mechanoluminescence property
Body material.Its with the advantages such as low in cost, stable luminescent property, luminous intensity be directly proportional to suffered stress intensity,
The fields such as stress intensity and its distribution of detection have application prospect.
The special electron configuration of trivalent bismuth ion make its be highly prone in crystal around crystalline field and coordination environment shadow
It rings, has in different substrates or environment from ultraviolet to the broad-band illumination property of feux rouges.However, being caused at present for long afterglow and power
Luminous research focuses primarily upon in transition metal and rare earth ion doped material, such as SrAl2O4:Eu2+,Dy3+、
Zn3Ga2Ge2O10:Cr3+、Ca3Ga2Ge3O12:Nd3+And CaAl2O4:Eu2+,Nd3+Deng the crystal activated about major element such as bismuth
Material is less in the report of this aspect, the application which greatly limits bismuth active material in long afterglow and mechanoluminescence field, because
This is developed is necessary with long-persistence luminous and mechanoluminescence bismuth doped crystal.
Summary of the invention
In order to overcome the disadvantages mentioned above of the prior art and insufficient, the purpose of the present invention is to provide one kind have both long afterglow and
Bismuth doped crystal of mechanoluminescence and preparation method thereof.Crystal of the invention can effectively be excited by ultraviolet light, and excitation band compares
Width has strong absorb within the scope of 240-450nm；Twilight sunset coverage area is big, ultraviolet to detect twilight sunset near infrared band；It is remaining
The brightness time is long, after 254nm exciting light irradiates 5min, remains to detect after 14h long-persistence luminous；More than luminescence generated by light and length
Except brightness shines, there is also mechanoluminescence phenomenons for bismuth doped crystal of the present invention.
The purpose of the present invention is achieved through the following technical solutions:
A kind of bismuth doped crystal having both long afterglow and mechanoluminescence, expression general formula are Sr3Y2Ge3O12:xBi3+, wherein x
For molar fraction, and 0 < x≤3%.
The bismuth doped crystal for having both long afterglow and mechanoluminescence, crystal structure belong to cubic system, and light emitting ionic is
Bi3+Ion.
A kind of preparation method for the bismuth doped crystal having both long afterglow and mechanoluminescence, comprising the following steps:
It (1) is Sr:Y:Ge:O:Bi=3:2:3:12:x by each element mol ratio, wherein x is molar fraction, and 0 < x≤
3%；It is weighed respectively containing strontium compound, containing yttrium compound, germanium-containing compound and bismuth-containing compound as raw material；
(2) it by after the weighed raw material grinding uniformly of step (1), in 1473~1573K, 4~8h of pre-burning, is cooled to room temperature, grinds
Mill mixes, up to the bismuth doped crystal for having both long afterglow and mechanoluminescence after grinding.
Preferably, step (1) carbonate containing oxide or strontium that strontium compound is strontium.
It preferably, is the oxide of yttrium containing yttrium compound described in step (1).
Preferably, step (1) germanium-containing compound is the oxide of germanium.
Preferably, step (1) bismuth-containing compound is bismuth oxide or bismuth nitrate.
Compared with prior art, the present invention has the following advantages and beneficial effects:
(1) the bismuth doped crystal of the present invention for having both long afterglow and mechanoluminescence is with Bi3+Ion is active ions, its energy
Enough effectively to be excited by ultraviolet light, excitation band is wider, has strong absorb within the scope of 240-450nm.
(2) of the present invention to have both long afterglow and the bismuth doped crystal twilight sunset coverage area of mechanoluminescence is big, it is ultraviolet to close
Infrared band detects twilight sunset.
(3) 14h is still after the closing of 254nm excitaton source for the bismuth doped crystal of the present invention for having both long afterglow and mechanoluminescence
It can detect luminous, after-glow brightness is high, the time is long.
(4) bismuth doped crystal of the invention in addition to luminescence generated by light and it is long-persistence luminous other than, there is also mechanoluminescence phenomenons.
(5) stable structure of the bismuth doped crystal of the present invention for having both long afterglow and mechanoluminescence, synthetic method is simple,
Convenient for large-scale production.
Detailed description of the invention
Fig. 1 is proportion (1)-(7) the bismuth doped crystal sample obtained for having both long afterglow and mechanoluminescence of embodiment 1
The comparison diagram of X-ray powder diffraction pattern and standard diffraction card figure.
Fig. 2 is the excitation-emission spectrum of proportion (4) sample of embodiment 1.
Fig. 3 is proportion (1)-(7) the bismuth doped crystal sample obtained for having both long afterglow and mechanoluminescence of embodiment 1
Emission spectrum, excitation wavelength 362nm.
Fig. 4 is the fluorescence of proportion (4) the bismuth doped crystal sample obtained for having both long afterglow and mechanoluminescence of embodiment 1
Life diagram, excitation wavelength 362nm, launch wavelength 465nm.
Fig. 5 is that the bismuth doped crystal of long afterglow and mechanoluminescence is had both made from embodiment 2 in the irradiation of 254nm excitation light source
Die-away time is the twilight sunset spectrum of 1min-20min after 5min.
Fig. 6 is that the bismuth doped crystal of long afterglow and mechanoluminescence is had both made from embodiment 2 in the irradiation of 254nm excitation light source
Die-away time is the twilight sunset spectrum of 60-360min after 5min.
Fig. 7 is that the bismuth doped crystal of long afterglow and mechanoluminescence is had both made from embodiment 2 in the irradiation of 254nm excitation light source
Die-away time is the twilight sunset spectrum of 14h after 5min.
Fig. 8 is the sample tribo-luminescence spectrum and twilight sunset spectrum comparison diagram of embodiment 3.
Specific embodiment
Below with reference to examples and drawings, the present invention is described in further detail, but embodiments of the present invention are not
It is limited to this, for not specifically specified technological parameter, can refer to routine techniques progress.
Embodiment 1
Strontium carbonate, yttrium oxide, germanium oxide, bismuth oxide are chosen as initial compounds raw material, based on each element chemistry
Ratio is measured, weighs four kinds of raw materials of compound respectively, totally 7 groups, is matched as follows:
(1) Sr:Y:Ge:O:Bi=3:2:3:12:0, corresponding x=0%；
(2) Sr:Y:Ge:O:Bi=3:2:3:12:0.0005, corresponding x=0.05%；
(3) Sr:Y:Ge:O:Bi=3:2:3:12:0.001, corresponding x=0.10%；
(4) Sr:Y:Ge:O:Bi=3:2:3:12:0.005, corresponding x=0.50%；
(5) Sr:Y:Ge:O:Bi=3:2:3:12:0.01, corresponding x=1.00%；
(6) Sr:Y:Ge:O:Bi=3:2:3:12:0.02, corresponding x=2.00%；
(7) Sr:Y:Ge:O:Bi=3:2:3:12:0.03, corresponding x=3.00%；
Mixture is ground after mixing, is packed into corundum crucible；Corundum crucible is placed in corundum boat, high-temperature cabinet is put into
Formula electric furnace.Strict control heating rate calcines 6h in 1523K, is cooled to room temperature, is ground, has both after grinding up to described
The bismuth doped crystal of long afterglow and mechanoluminescence.
Fig. 1 is the X that embodiment 1 matches (1)-(7) the bismuth doped crystal sample obtained for having both long afterglow and mechanoluminescence
Ray powder diffraction.It is measured using German Brooker company (Bruker) D8ADVANCE type x-ray powder diffraction instrument.Spoke
Penetrating source is Cu target K alpha ray test voltage 40kV, tests electric current 40mA, 0.02 °/step of scanning step, scanning speed: 0.12s/
step.XRD spectrum is analysis shows the sample obtained at 1523K is mutually Sr3Y2Ge3O12Phase belongs to cubic system, dopping effect
Other object phases or impurity are not introduced.
Fig. 2 is the excitation-emission spectrum of proportion (4) sample of embodiment 1.Using Edinburgh, Britain company (Edinburgh)
The measurement of FLS920 type stable state moment Fluorescence Spectrometer.Using the xenon lamp of 450W as excitation light source, it is equipped with time adjustment single photon counting
Block (TCSPC), the red quick photomultiplier tube (PMT) of thermoelectric cold, TM300 excitation monochromator and double TM300 and emits monochromator.By Fig. 2
It is found that under 362nm ultraviolet excitation, sample all can produce center be located at~465nm shines.
Fig. 3 is proportion (1)-(7) sample emission spectrum of embodiment 1, excitation wavelength 362nm.Test condition and Fig. 2
It is identical.As shown in figure 3, proportion (1) sample does not shine under 362nm excitation, (2)-(7) electromagnetic radiation spectrum is matched in 425-
Within the scope of 550nm, with Bi3+Ion concentration increases luminous intensity and changes therewith, shines in x=3.00% most strong.
Fluorescence lifetime figure of the Fig. 4 for proportion (4) sample of embodiment 1, excitation wavelength 362nm, launch wavelength are
465nm, it is possible to find fluorescence lifetime is 663.34ns, fitting parameter 99.76% under this condition.
Embodiment 2
Strontium carbonate, yttrium oxide, germanium oxide, bismuth oxide are chosen as initial compounds raw material, is matched by each element mole
Than Sr:Y:Ge:O:Bi=3:2:3:12:0.005, corresponding x=0.50% weighs four kinds of raw materials of compound, mixture warp respectively
After grinding uniformly, it is packed into corundum crucible, crucible is placed in corundum boat, high-temperature box type electric furnace is put into.Strict control heating rate
6h is calcined in 1523K, is cooled to room temperature, is ground, up to the bismuth doping for having both long afterglow and mechanoluminescence after grinding
Crystal.XRD spectrum is analysis shows it is Sr3Y2Ge3O12Phase, belongs to cubic system, and dopping effect does not introduce other object phases or miscellaneous
Matter.The photoluminescence spectra property of material is similar with embodiment 1.In addition, sample after 254nm ultraviolet excitation, emits indigo color
Long afterglow, Fig. 5 and Fig. 6 are the twilight sunset spectrum after its differential declines time.Fig. 7 is sample in 254nm excitation light source irradiation 5min
Afterwards, decay 14 hours after twilight sunset spectrum, from figure 7 it can be seen that 254nm excitaton source closing after 14h remain to detect it is luminous.
Embodiment 3
Strontium carbonate, yttrium oxide, germanium oxide, bismuth oxide are chosen as initial compounds raw material, is matched by each element mole
Than Sr:Y:Ge:O:Bi=3:2:3:12:0.005, corresponding x=0.50% weighs four kinds of raw materials of compound, raw material is through grinding respectively
After mill mixes, the PVA for taking the raw material addition of half quality to account for raw material 5wt% is granulated, and the raw material after taking 5g to be granulated is pressed
Piece takes semi-automatic tablet press machine to keep 2min under 10Mpa, obtains the cylindrical sheets of 25 × 10mm.Thin slice is placed in corundum
In boat, it is put into high-temperature box type electric furnace.Strict control heating rate calcines 6h in 1523K, is cooled to room temperature.After roasting
Sr3Y2Ge3O12: 0.50%Bi3+Sample is fixed on sample stage, is rubbed using the corundum rod with sharp tip, simultaneously
Luminous signal of the sample under frictional force excitation is collected using ocean fiber spectrometer.Keep friction tips and fibre-optical probe distance
For 8mm.When carrying out tribo-luminescence experiment in darkroom, eye-observation to stronger luminous signal.Fig. 8 is shown as the friction of sample
The comparison diagram of luminescent spectrum, long-persistence luminous spectrum, it is obvious that the master of tribo-luminescence spectrum and long-persistence luminous spectrum
Peak is consistent with luminescence generated by light in 465nm.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Any change made without departing from the spirit and principles of the present invention of limitation, such as others, substitution, combines, is simple at modification
Change, should be equivalent substitute mode, be included within the scope of the present invention.
Claims (7)
1. a kind of bismuth doped crystal for having both long afterglow and mechanoluminescence, which is characterized in that its chemical general formula is Sr3Y2Ge3O12:
xBi3+, wherein x is molar fraction, and 0 < x≤3%.
2. having both the bismuth doped crystal of long afterglow and mechanoluminescence according to claim 1, which is characterized in that crystal structure category
In anorthic system, light emitting ionic Bi3+Ion.
3. the preparation method of the bismuth doped crystal as claimed in claim 1 or 2 for having both long afterglow and mechanoluminescence, which is characterized in that
The following steps are included:
(1) it weighs by each element mol ratio containing strontium compound, containing yttrium compound, germanium-containing compound and bismuth-containing compound and makees respectively
For raw material；Each element mol ratio is Sr:Y:Ge:O:Bi=3:2:3:12:x, and wherein x is molar fraction, and 0 < x≤3%；
(2) after grinding raw material, 4-8h is calcined in 1473~1573K, is cooled to room temperature, has both length described in acquisition after grinding uniformly
The bismuth doped crystal of twilight sunset and mechanoluminescence.
4. having both the preparation method of the bismuth doped crystal of long afterglow and mechanoluminescence according to claim 3, which is characterized in that
Step (1) carbonate containing oxide or strontium that strontium compound is strontium.
5. having both the preparation method of the bismuth doped crystal of long afterglow and mechanoluminescence according to claim 3 or 4, feature exists
In, step (1) it is described containing yttrium compound be yttrium oxide.
6. having both the preparation method of the bismuth doped crystal of long afterglow and mechanoluminescence according to claim 3 or 4, feature exists
In step (1) germanium-containing compound is the oxide of germanium.
7. having both the preparation method of the bismuth doped crystal of long afterglow and mechanoluminescence according to claim 3 or 4, feature exists
In step (1) bismuth-containing compound is bismuth oxide or bismuth nitrate.
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| CN111378445A (en) * | 2020-03-19 | 2020-07-07 | 北京科技大学 | Cr (chromium)3+Preparation and application method of doped near-infrared broad-spectrum luminescent material |
| CN113278418A (en) * | 2021-04-25 | 2021-08-20 | 鲁东大学 | Novel orange long-afterglow luminescent material and preparation method thereof |
| CN113667472A (en) * | 2021-07-12 | 2021-11-19 | 广东工业大学 | Bi3+Doped ultraviolet long-afterglow luminescent material and preparation method and application thereof |
| CN113667472B (en) * | 2021-07-12 | 2022-06-10 | 广东工业大学 | Bi3+Doped ultraviolet long-afterglow luminescent material and preparation method and application thereof |
| CN113980680A (en) * | 2021-11-25 | 2022-01-28 | 厦门稀土材料研究所 | Ion-codoped ultraviolet long-afterglow luminescent material, and preparation method and application thereof |
| CN115926793A (en) * | 2022-11-24 | 2023-04-07 | 中国科学院上海光学精密机械研究所 | Multi-response anti-counterfeiting germanate fluorescent powder with adjustable luminescence color as well as preparation method and application thereof |
| CN115926793B (en) * | 2022-11-24 | 2023-12-01 | 中国科学院上海光学精密机械研究所 | Multi-response anti-counterfeiting germanate fluorescent powder with adjustable luminous color, and preparation method and application thereof |
| CN116120927A (en) * | 2022-12-27 | 2023-05-16 | 中山大学 | Bi (Bi) 3+ Cyan-doped fluorescent powder and preparation method and application thereof |
| CN116120927B (en) * | 2022-12-27 | 2024-03-15 | 中山大学 | Bi (Bi) 3+ Cyan-doped fluorescent powder and preparation method and application thereof |
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