CN106398694A - Pb<2+>-doped ultraviolet long-afterglow luminescent material and preparation method thereof - Google Patents
Pb<2+>-doped ultraviolet long-afterglow luminescent material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Pb<2+>-doped ultraviolet long-afterglow luminescent material and a preparation method thereof. The luminescent material uses Sr2MgGe2O7 as a matrix and doping Pb<2+> ions as activation ions, wherein the Pb<2+> ions account for 0.05 to 2 mol% of the luminescent material. The preparation method comprises the following steps: mixing raw materials with a fluxing agent; carrying out low-temperature pre-burning at first; and then carrying out high-temperature sintering so as to obtain the ultraviolet long-afterglow luminescent material. The luminescent material prepared in the invention presents strong single-band ultraviolet long-afterglow luminescence performance. The peak of ultraviolet long-afterglow luminescence located at the position of 370 nm and afterglow time is as long as 12 h. Meanwhile, the material presents excellent photoexcitation luminescence performance. A sample having undergone high-energy ultraviolet pre-irradiation has obviously improved ultraviolet afterglow intensity after excitation by low-energy light (white light or near infrared light). The ultraviolet long-afterglow luminescent material has potential application value in fields like photochemical catalysis, disinfection and sterilization, counterfeiting prevention and medical photodynamic therapy.
Description
Technical field
The invention belongs to long after glow luminous material technical field, more particularly, to a kind of Pb2+The ultraviolet of doping is long-persistence luminous
Material and preparation method thereof.
Background technology
Luminescence band is located at ultra-violet light-emitting material between 200~400nm, because it is in photochemical catalysis, disinfection, anti-
The huge using values in field such as pseudo- and medical optical dynamic therapy, in the nearest extensive concern just causing people for several years.?
Just because of this, develop the study hotspot that new ultra-violet light-emitting material is always field of light emitting materials, current research mainly collects
In in rare earth ion doped ultra-violet light-emitting material and semi-conducting material.But, for some special applications of luminescent material, such as
Photocatalysis, optical dynamic therapy etc., if ultra-violet light-emitting material can after the external world excites stopping, luminous still be able to continue certain
Time, that is, it is long-persistence luminous to produce ultraviolet, then this special ultraviolet afterglow performance will have well
Using value.At present, the immense success acquired compared to visible ray and the research of near infrared light long after glow luminous material, ultraviolet
The R and D of long after glow luminous material are relatively backward always, also lack excellent performance in the market and chemical stability is good
The advantages of ultraviolet long-afterglow material.
The long after glow luminous material of design and exploitation function admirable needs the suitable centre of luminescence and matrix.Report at present
In the activator in road, there is 6s2The Pb of electron configuration2+It is a very promising ultra-violet light-emitting center.Have at present
Many relevant Pb2+The report of the ultra-violet light-emitting material of doping, but Pb2+As the long-afterglow material of the centre of luminescence, especially purple
Outer long-afterglow material, does not also have the report of correlation.
Content of the invention
For prior art, it is an object of the invention to provide a kind of Pb2+The ultraviolet long after glow luminous material of doping, remaining
Brightness emission peak is located at 370nm, and persistence is more than 12h.
Another object of the present invention is to providing the preparation method of the ultraviolet long after glow luminous material of above-mentioned lead ion doping.
For achieving the above object, the present invention employs the following technical solutions:
The present invention provides a kind of Pb2+The ultraviolet long after glow luminous material of doping, with Sr2MgGe2O7For matrix, Doped ions
Pb2+For active ions, wherein Pb2+Account for the 0.05mol%~2mol% of described luminescent material.
The activator of the present invention must be appropriate, and activation dosage is excessive, can cause activator ion concentration quenching;Activation dosage
When less, then do not reach preferably activation effect so that the performance of luminescent material is relatively low.
The present invention also provides a kind of Pb2+The preparation method of the ultraviolet long after glow luminous material of doping, comprises the following steps:
By material and flux mixing, carry out low temperature presintering first, then carry out high temperature sintering again, obtain ultra-violet light-emitting material
Material;Described material includes compound containing Sr, compound containing Mg, compound containing Ge and compound containing Pb.
Preferably, described compound containing Sr is strontium carbonate or strontium oxide strontia, but comes from the effect of ultraviolet long after glow luminous material
Say, further preferred for strontium carbonate.
Preferably, described compound containing Mg is magnesia or magnesium carbonate, but comes from the effect of ultraviolet long after glow luminous material
Say, further preferred for magnesium carbonate.
Preferably, described compound containing Ge is germanium oxide.
Preferably, described compound containing Pb is lead oxide.
Preferably, described Sr compound, compound containing Mg, the molar ratio containing Ge compound are 2:1:2.
Preferably, described flux is H3BO3Or B2O3;The addition of flux is compound containing Sr, compound containing Mg,
Compound containing Ge and 0.1~1wt% of the gross mass of compound containing Pb.Flux can make sintering temperature decrease, and closes
The quality that the flux of adaptation proportion enables to the luminescent material of the present invention is preferable, high yield rate, improves sending out of luminescent material
Luminous intensity and persistence.
Preferably, material and flux are ground mixing, material and flux are entered preferably in mortar by the present invention
Row ground and mixed, obtains mixture.
Preferably, described calcined temperature is 800~900 DEG C, and burn-in time is 1~3h;It is further preferred that calcined temperature
For 900 DEG C, burn-in time is 2h.Pre-burning can effectively remove the volatile components in raw material, thus the sintering activity height obtaining, one-tenth
Divide uniform and stable ceramic powder.Therefore, in high-temperature sintering process, it is possible to reduce the shrinkage factor of material simultaneously effectively improves material
Luminescent properties.
Preferably, carry out compressing tablet after described low temperature presintering.It is further preferred that before compressing tablet after low temperature presintering, low temperature is pre-
Material after burning carries out regrinding into powder.The consistency of powder body material can be made after compressing tablet to greatly increase, contribute to powder
Crystal boundary between particle is mobile and crystal grain is grown up, and therefore can effectively reduce sintering temperature, thus improving the crystal property of material
And luminescent properties.
Preferably, described high temperature sintering temperature is 1250~1350 DEG C, and sintering time is 2~4h;It is further preferred that institute
State high temperature sintering temperature and be 1320 DEG C, sintering time is 3h.
Preferably, described pre-burning and high temperature sintering are all to carry out the protection it is not necessary to reducing atmosphere in air atmosphere.
One of technique scheme technical scheme has the advantages that:
(1) design and the ultraviolet long after glow luminous material of exploitation function admirable needs suitable ultra-violet light-emitting center and base
Matter, they will determine launch wavelength and the persistence of ultraviolet afterglow materials respectively.The active ions that the present invention selects
Pb2+Due to its sp → s2(3P0,1→1S0) electron transition it will usually produce a broadband emission, and, Pb2+Launch wavelength exist
Different parent lattices can produce change, and light emitting region is adjustable in the range of ultraviolet region and visible region.In addition, the present invention with
Sr2MgGe2O7As matrix, the chemical stability of luminescent material can be made good, ultraviolet twilight sunset emission peak is located at 370nm, twilight sunset
Time is more than 12h.
(2) material of present invention preparation shows the strong long-persistence luminous performance of single tape ultraviolet.Meanwhile, this material also has
Excellent light stimulus afterglow performance.Through high energy UV pre-irradiation sample through low energy light (white light or closely red
Outer light) excitation after, ultraviolet afterglow intensity is remarkably reinforced.This ultraviolet long after glow luminous material is in photochemical catalysis, disinfection, anti-
There is potential using value in the fields such as pseudo- and medical optical dynamic therapy.
(3) preparation method that the present invention adopts, its raw material drawing extensive, cheap, simple to operate it is not necessary to atmosphere
Protection, suitable large-scale industrial production.
Brief description
Fig. 1 is the X ray diffracting spectrum of the ultraviolet long after glow luminous material of preparation in the present invention.
Fig. 2 is the excitation spectrum of ultraviolet long after glow luminous material of preparation and emission spectrum in the present invention.
Fig. 3 is that the ultraviolet long after glow luminous material of preparation in the present invention obtains after 15 minutes in 254nm ultraviolet light irradiation
Long afterglow attenuation curve.
Fig. 4 be the present invention in preparation ultraviolet long after glow luminous material after 254nm ultraviolet light irradiation 15 minutes, in difference
The ultraviolet twilight sunset emission spectrum that attenuation initiation obtains.
Specific embodiment
In order to the present invention is expanded on further, with reference to embodiment, the preparation method of ultraviolet long after glow luminous material is carried out
Describe in detail.
Embodiment 1
According to following component:Ultraviolet long after glow luminous material Sr2MgGe2O7:Pb2+, with Sr2MgGe2O7For matrix, adulterate from
Sub- Pb2+For active ions, wherein Pb2+Doping (accounting for described luminescent material) be 0.5mol%.Accurately weigh strontium carbonate
(SrCO3) 1.7716g, magnesia (MgO) 0.24g, germanium oxide (GeO2) 1.26g, lead oxide (PbO) 0.0067g and boron oxide
(B2O3)0.0165g.Above-mentioned raw materials are placed in agate mortar and grind 1 hour about, make raw material after being sufficiently mixed, move to corundum earthenware
In crucible, pre-burning 2h at 900 DEG C.Powder after pre-burning after re-grinding, using powder compressing machine by 1g about powder
It is pressed into diameter and is about 15mm, thickness is about the disk of 1mm.Finally, by the disk after shaping, at 1320 DEG C, high temperature sintering 3h obtains
To Sr2MgGe2O7:Pb2+Ultraviolet long after glow luminous material.
Prepare sample to embodiment to detect:
The X-ray diffractogram of sample referring to Fig. 1, with Sr2MgGe2O7Standard diffraction spectrum (JCPDS 38-1080) consistent.
The sample of Fig. 1 explanation synthesis is pure tetragonal phase structure, and chemical stability is good.
The excitation spectrum of sample and emission spectrum referring to Fig. 2, under 280nm high energy UV excites, sample have one
Individual wide transmitting band, this transmitting band covers the broad area from 300nm to 650nm, and emission peak is located at 370nm.Excite
The wave-length coverage of spectrum is located between 250nm to 320nm.
, referring to Fig. 3, sample is after 254nm high energy UV excites 15min, permissible for the ultraviolet long afterglow attenuation curve of sample
Produce the ultraviolet long afterglow transmitting up to 12 hours.The twilight sunset launch wavelength of monitoring is 370nm.
The ultraviolet twilight sunset emission spectrum in the differential declines moment for the sample participates in Fig. 4, excites stopping in extraneous high energy UV
Afterwards, the spectrum of the photoluminescence emission spectrum in the ultraviolet twilight sunset emission spectrum that sample records in 0.5h, 1h, 3h and 6h, with Fig. 2
Wire shaped is consistent, and the shape of twilight sunset emission spectrum and emission peak positions do not change with the increase of die-away time.
Embodiment 2
According to following component:Ultraviolet long after glow luminous material Sr2MgGe2O7:Pb2+, with Sr2MgGe2O7For matrix, adulterate from
Sub- Pb2+For active ions, wherein Pb2+Doping (accounting for described luminescent material) be 1mol%;Accurately weigh strontium carbonate (SrCO3)
1.7672g, magnesia (MgO) 0.24g, germanium oxide (GeO2) 1.26g, lead oxide (PbO) 0.0134g and boron oxide (B2O3)
0.0165g.Above-mentioned raw materials are placed in agate mortar and grind 1 hour about, so that raw material is moved to after being sufficiently mixed in corundum crucible,
Pre-burning 2h at 800 DEG C.Powder after pre-burning after re-grinding, using powder compressing machine by 1g about the powder sample arriving
It is pressed into diameter and is about 15mm, thickness is about the disk of 1mm.Finally, by the disk after shaping, at 1350 DEG C, high temperature sintering 2h obtains
To Sr2MgGe2O7:Pb2+Ultraviolet long after glow luminous material.
Embodiment 3
According to following component:Ultraviolet long after glow luminous material Sr2MgGe2O7:Pb2+, with Sr2MgGe2O7For matrix, adulterate from
Sub- Pb2+For active ions, wherein Pb2+Doping (accounting for described luminescent material) be 0.1mol%;Accurately weigh strontium carbonate
(SrCO3) 1.7751g, magnesia (MgO) 0.24g, germanium oxide (GeO2) 1.26g, lead oxide (PbO) 0.0014g and boron oxide
(B2O3)0.0165g.Above-mentioned raw materials are placed in agate mortar and grind 1 hour about, make raw material after being sufficiently mixed, move to corundum earthenware
In crucible, pre-burning 3h at 800 DEG C.Powder after pre-burning after re-grinding, using powder compressing machine by 1g about the powder arriving
Last sample is pressed into diameter and is about 15mm, and thickness is about the disk of 1mm.Finally, by the disk after shaping, at 1300 DEG C, high temperature burns
Knot 3h obtains Sr2MgGe2O7:Pb2+Ultraviolet long after glow luminous material.
Embodiment 4
According to following component:Ultraviolet long after glow luminous material Sr2MgGe2O7:Pb2+, with Sr2MgGe2O7For matrix, adulterate from
Sub- Pb2+For active ions, wherein Pb2+Doping (accounting for described luminescent material) be 2mol%;Accurately weigh strontium carbonate (SrCO3)
1.7583g, magnesia (MgO) 0.24g, germanium oxide (GeO2) 1.26g, lead oxide (PbO) 0.0268g and boron oxide (B2O3)
0.0165g.Above-mentioned raw materials are placed in agate mortar and grind 1 hour about, so that raw material is moved to after being sufficiently mixed in corundum crucible,
Pre-burning 2h at 900 DEG C.Powder after pre-burning after re-grinding, using powder compressing machine by 1g about the powder sample arriving
It is pressed into diameter and is about 15mm, thickness is about the disk of 1mm.Finally, by the disk after shaping, at 1250 DEG C, high temperature sintering 4h obtains
To Sr2MgGe2O7:Pb2+Ultraviolet long after glow luminous material.
Comparative example 1
According to following component:Long after glow luminous material Sr3MgGe2O8:Pb2+, with Sr3MgGe2O8For matrix, Doped ions
Pb2+For active ions, wherein Pb2+Doping be 0.5mol%;Accurately weigh strontium carbonate (SrCO3) 1.9947g, magnesia
(MgO) 0.18g, germanium oxide (GeO2) 0.945g, lead oxide (PbO) 0.005g and boron oxide (B2O3)0.0156g.Will be above-mentioned
Raw material is placed in agate mortar and grinds 1 hour about, so that raw material is moved to after being sufficiently mixed in corundum crucible, pre-burning at 900 DEG C
2h.Powder after pre-burning after re-grinding, using powder compressing machine by 1g about to powder sample be pressed into diameter and be about
15mm, thickness is about the disk of 1mm.Finally, by the disk after shaping, at 1350 DEG C, high temperature sintering 3h obtains Sr3MgGe2O7:
Pb2+Long after glow luminous material.Sr3MgGe2O7:Pb2+The twilight sunset emission peak of long after glow luminous material is located at 350nm, but
It is that initial afterglow intensity is very weak, and persistence is also very short, only about a few minutes.
Comparative example 2
According to following component:Long after glow luminous material Ba2MgGe2O7:Pb2+, with Ba2MgGe2O7For matrix, Doped ions
Pb2+For active ions, wherein Pb2+Doping be 0.5mol%;Accurately weigh brium carbonate (BaCO3) 1.8865g, magnesia
(MgO) 0.192g, germanium oxide (GeO2) 1.008g, lead oxide (PbO) 0.0053g and boron oxide (B2O3)0.01545g.Will be upper
State raw material and be placed in grinding 1 hour about in agate mortar, so that raw material is moved to after being sufficiently mixed in corundum crucible, pre- at 800 DEG C
Burn 2h.Powder after pre-burning after re-grinding, using powder compressing machine by 1g about to powder sample be pressed into diameter about
For 15mm, the thickness about disk of 1mm.Finally, by the disk after shaping, at 1200 DEG C, high temperature sintering 3h obtains
Ba2MgGe2O7:Pb2+Long after glow luminous material.Ba2MgGe2O7:Pb2++The twilight sunset emission peak of long after glow luminous material is located at
380nm about, but, initial afterglow intensity is very weak, and persistence is also very short, only about a few minutes.
Compared with the long after glow luminous material in comparative example 1 and comparative example 2, the better performances of the material of the present invention, be by
More special in the matrix selected and active ions.Sr2MgGe2O7It is one kind of cubic non-centrosymmetrical melilite compound,
There is special crystal structure.Wherein, Sr2+Radius with as activator Pb2+Very much like, Pb in sintering process2+Easily
In replacement Sr2+Enter parent lattice and form more centres of luminescence, thus being conducive to the long-persistence luminous of material.Meanwhile, Pb2 +It is with s2The ion of electron configuration, the crystalline field of surrounding lattice ion is very big on their luminous impact.In different matrix
In material, due to the difference of crystalline field, Pb2+Luminescent properties can produce obvious change.
The explanation of above example is only to aid in understanding the method for the present invention and its core concept.It should be pointed out that for this
For the those of ordinary skill in field, without departing from the present invention away from the premise of, some improvement can also be carried out to the present invention
And modification, these improve and modify and also fall in the protection domain of the claims in the present invention.
Claims (10)
1. a kind of Pb2+The ultraviolet long after glow luminous material of doping, with Sr2MgGe2O7For matrix, Doped ions Pb2+For activation from
Son, wherein Pb2+Account for the 0.05mol%~2mol% of described luminescent material.
2. the Pb described in claim 12+The preparation method of the ultraviolet long after glow luminous material of doping, is characterized in that, including following
Step:
By material and flux mixing, carry out low temperature presintering first, then carry out high temperature sintering again, obtain ultra-violet light-emitting material;
Described material includes compound containing Sr, compound containing Mg, compound containing Ge and compound containing Pb.
3. preparation method as claimed in claim 2, is characterized in that:Described compound containing Sr is strontium carbonate or strontium oxide strontia;Described
Compound containing Mg is magnesia or magnesium carbonate;Described compound containing Ge is germanium oxide;Described compound containing Pb is lead oxide.
4. preparation method as claimed in claim 2, is characterized in that:Described flux is H3BO3Or B2O3;The addition of flux
It is compound containing Sr, compound containing Mg, compound containing Ge and the gross mass 0.1~1wt% of compound containing Pb.
5. preparation method as claimed in claim 2, is characterized in that:Described calcined temperature is 800~900 DEG C, and burn-in time is 1
~3h.
6. preparation method as claimed in claim 5, is characterized in that:Calcined temperature is 900 DEG C, and burn-in time is 2h.
7. preparation method as claimed in claim 2, is characterized in that:Carry out compressing tablet after described low temperature presintering.
8. preparation method as claimed in claim 2, is characterized in that:Described high temperature sintering temperature is 1250~1350 DEG C, sintering
Time is 2~4h.
9. preparation method as claimed in claim 8, is characterized in that:Described high temperature sintering temperature is 1320 DEG C, and sintering time is
3h.
10. preparation method as claimed in claim 2, is characterized in that:Described pre-burning and high temperature sintering are all in air atmosphere
Carry out.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107367449A (en) * | 2017-07-28 | 2017-11-21 | 山东大学 | Traceable PM2.5 particulate composites and preparation method thereof |
CN109825292A (en) * | 2019-03-21 | 2019-05-31 | 江南大学 | A kind of preparation method and application for the inorganic microparticle having both photoresponse and green long-persistence luminous effect |
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JP2014523945A (en) * | 2011-06-29 | 2014-09-18 | コーニンクレッカ フィリップス エヌ ヴェ | Luminescent substance particles comprising a coating and lighting unit comprising said luminescent substance |
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2016
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JPH10172459A (en) * | 1996-12-12 | 1998-06-26 | Samsung Display Devices Co Ltd | Projector system |
WO2004099341A1 (en) * | 2003-05-06 | 2004-11-18 | Philips Intellectual Property & Standards Gmbh | Fluorescent lamp having a uvb phosphor |
JP2014523945A (en) * | 2011-06-29 | 2014-09-18 | コーニンクレッカ フィリップス エヌ ヴェ | Luminescent substance particles comprising a coating and lighting unit comprising said luminescent substance |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107367449A (en) * | 2017-07-28 | 2017-11-21 | 山东大学 | Traceable PM2.5 particulate composites and preparation method thereof |
CN109825292A (en) * | 2019-03-21 | 2019-05-31 | 江南大学 | A kind of preparation method and application for the inorganic microparticle having both photoresponse and green long-persistence luminous effect |
CN109825292B (en) * | 2019-03-21 | 2021-10-26 | 江南大学 | Preparation method and application of inorganic microparticles with photoresponse and green long-afterglow luminescence effects |
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