CN105969350A - Blue-green long-afterglow luminescent material and preparation method thereof - Google Patents

Blue-green long-afterglow luminescent material and preparation method thereof Download PDF

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CN105969350A
CN105969350A CN201610385593.7A CN201610385593A CN105969350A CN 105969350 A CN105969350 A CN 105969350A CN 201610385593 A CN201610385593 A CN 201610385593A CN 105969350 A CN105969350 A CN 105969350A
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luminescent material
blue
solution
green long
green
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CN105969350B (en
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郑子山
林秋惠
王华根
陈国良
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Minnan Normal University
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Minnan Normal University
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus

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Abstract

The invention discloses a blue-green long-afterglow luminescent material and a preparation method thereof. The chemical expression of the material is MnxZr1-0.5xP2O7, wherein x is equal to 0.005-0.12, raw materials of the luminescent material include ZrOC12.8H2O, (NH4)2HPO4, MnCO3, H3BO3, citric acid and polyethylene glycol 4000. The luminescent center of the prepared luminescent material is Zr<4+> and Mn<2+>, wherein the blue luminescent part comes from Zr<4+>, and the green luminescent part comes from Mn<2+>. After irradiation for 15 min under lamplight, a light source is removed, and it can be observed in darkness that the material can emit blue-green light continuously for 10 h or longer. Moreover, the material is low in synthesis cost and high in chemical stability.

Description

A kind of blue-green long persistence luminescent material and preparation method thereof
Technical field
The invention belongs to field of light emitting materials, be specifically related to a kind of blue-green long persistence luminescent material and preparation method thereof.
Background technology
Long-afterglow material is embedded photoluminescent material, ambient light irradiation energy can be stored, under the disturbance of temperature, lentamente with the form of visible ray discharge storage energy, the various fields such as the instrument at road safety marker, the lighting installation of urgent accident, aviation and automobile shows, anti-counterfeiting technology, building decoration, industrial art coating has purposes widely.Long after glow luminous material is mainly made up of substrate, activator (centre of luminescence) and auxiliary activator.Existing patented technology and document report are all with rare earth ion or some transition metal ionss as the centre of luminescence, such as Eu2+、Eu3+、Tb3+、Nd3+、Mn2+、Cu+Deng.As patent of invention " a kind of red long afterglow luminous material and preparation method thereof " (ZL200910112064.X) discloses material (Zn1- α - βMnαLnβ)3(P1-0.8 γSiγO4)2Technology of preparing；Patent of invention " a kind of overlength afterglow long persistence luminescent silicate material and preparation method thereof " (CN201010516567) discloses material Ba3.992-xSi6O16:Eu0.008,RxTechnology of preparing；Patent of invention " a kind of method of quickly synthesizing long-persistence luminescent material " (CN101899298A) discloses material C a(0.8-2x) Zn0.2TiO3:xPr3+, xNa+Technology of preparing；Patent of invention " a kind of manganese ion-activated red long-afterglow luminescent material and preparation method thereof " (CN102719243A) discloses materials A lN:Mn2+Technology of preparing；Patent of invention " a kind of red long afterglow luminous material and preparation method thereof " (CN103160278A) material ZnGa is disclosed2O4: aCr3+,bDy3+, its luminescent center ion is respectively Eu2+, Eu3+, Pr3+, Mn2+And Cr3+.In addition some documents (see Mater. Chem. Phys. 99 (2006) 494, J. Lumin. 156 (2014) 25 and J. Electrochem. Soc. 158 (2011) H697) also report with Ag+, Cu+, Ce3+Transition metal ions is as the centre of luminescence etc..Document J. Rare Earths 22 (1) (2004) 83 reports β-Zn3(PO4)2:Zr4+Blue-green long persistence luminescent material, Zr4+As the centre of luminescence.Existing technology uses expensive rare earth element as the centre of luminescence of luminescent material or to also tend to introduce the rare earth element of some costlinesses as sensitizer, luminescent material Ba as disclosed in patent of invention patent of invention (CN201010516567) to improve the luminescent properties of material3.992-xSi6O16:Eu0.008,RxWith patent of invention (CN101899298A) disclosed in luminescent material Ca(0.8-2x) Zn0.2TiO3:xPr3+, xNa+, invention disclosed technology and the document reported use transition metal ions or Zr4+Afterglow property as the luminescent material of the centre of luminescence is the most bad, and document J. Rare Earths 22 (1) (2004) 83 reports β-Zn3(PO4)2:Zr4+The persistence of blue-green long persistence luminescent material only has half an hour, and it is the shortest for persistence, such as document (Zhangzhou Normal College's journal (natural science edition), 4(2006) P93 to make the long after glow luminous material of the centre of luminescence with transition metal ions) Cu that reports+Sr as the centre of luminescence2ZnSi2O7 :Cu+Only have 2 hours persistence.Therefore, prepare and a kind of there is length persistence, stable performance, the rare earth element of other costliness that need not to adulterate and the luminescent material that the cost of material is low is significantly.
Summary of the invention
Present invention aims to prior art not enough, it is provided that a kind of blue-green long persistence luminescent material and preparation method thereof.The centre of luminescence of obtained luminescent material is Zr4+And Mn2+, wherein blue-light-emitting part comes from Zr4+And green emitting comes from Mn2+, through light-illuminating 15 After min, remove light source, material be can be observed in the dark and can persistently turn blue green glow 10 more than h, and materials synthesis low cost, chemical stability are high.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of blue-green long persistence luminescent material, with Zr4+And Mn2+The centre of luminescence, its chemical expression is MnxZr1-0.5xP2O7, wherein x=0.005 ~ 0.12.
The preparation method of a kind of blue-green long persistence luminescent material as above, specifically includes following steps:
(1) raw material ZrOCl is the most accurately weighed2·8H2O、(NH4)2HPO4And MnCO3；
(2) H is then weighed3BO3And citric acid；
(3) ZrOCl2·8H2O、(NH4)2HPO4、H3BO3Add water with citric acid and be configured to the mixture solution A that mass percent concentration is 15 ~ 30wt%；At MnCO3The nitric acid of middle addition 3mol/L also makes it be completely dissolved, then adds distilled water and be configured to the settled solution B that mass percent concentration is 15 ~ 30wt%；
(4) solution A step (3) prepared and solution B mix homogeneously, with the pH value of 25wt% ammonia or 65wt% nitre acid-conditioning solution to 2 ~ 5；Macrogol 4000 is added subsequently, till continuing stirring until formation gel under the water-bath of 65 ~ 85 DEG C in the mixed solution of A and B；
(5) gel that step (4) is formed is put and be dried 12 h in 110 DEG C in an oven, by in the crucible loading jacketed after dried gel abrasive, interior crucible setting-out product outer crucible is put activated carbon and builds lid, it is placed in Muffle furnace, calcination 2 ~ 5 h at 950 ~ 1100 DEG C, naturally cool to room temperature, obtain blue-green long persistence luminescent material.
H in step (2)3BO3Being 0.2 ~ 1.2:1 with the mol ratio of luminescent material, citric acid is 0.8 ~ 3.5:1 with the mol ratio of luminescent material.
In step (4), the mixed solution of A and B and the weight ratio of Macrogol 4000 are 1000:0.5 ~ 5.
The beneficial effects of the present invention is:
The centre of luminescence of the luminescent material obtained by the present invention is Zr4+And Mn2+, wherein blue-light-emitting part comes from Zr4+And green emitting comes from Mn2+, through light-illuminating 15 After min, remove light source, material be can be observed in the dark and can persistently turn blue green glow 10 more than h, and the chemical ten of materials synthesis low cost, material of main part is stable.Mn2+For the centre of luminescence, the significant contributor of material emission performance, and Zr4+Can be used as the centre of luminescence and as sensitized ions, the luminescent properties of material can be had good improvement result again.
Accompanying drawing explanation
Fig. 1 is the Mn that embodiment 1 prepares0.1Zr0.95P2O7XRD figure and standard spectrogram PDF49-1079；
Fig. 2 is the Mn that embodiment 1 prepares0.1Zr0.95P2O7Excitation and emission spectra figure；
Fig. 3 is the Mn that embodiment 1 prepares0.1Zr0.95P2O7Thermoluminescence；
Fig. 4 is Mn0.1Zr0.95P2O7Material decay of afterglow curve under different synthesis temperatures.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
Embodiment 1
A kind of blue-green long persistence luminescent material, its chemical expression is Mn0.1Zr0.95P2O7, preparation method comprises the following steps:
(1) raw material ZrOCl is the most accurately weighed2·8H2O、(NH4)2HPO4And MnCO3；
(2) H is then weighed3BO3And citric acid, H3BO3Being 0.6:1 with the mol ratio of luminescent material, citric acid is 2.5:1 with the mol ratio of luminescent material；
(3) ZrOCl2·8H2O、(NH4)2HPO4、H3BO3Add water with citric acid and be configured to the mixture solution A that mass percent concentration is 22wt%；At MnCO3The nitric acid of middle addition 3mol/L also makes it be completely dissolved, then adds distilled water and be configured to the settled solution B that mass percent concentration is 22wt%；
(4) solution A step (3) prepared and solution B mix homogeneously, with the pH value of 65wt% nitre acid-conditioning solution to 2；Adding Macrogol 4000 subsequently in the mixed solution of A and B, the mixed solution of A and B and the weight ratio of Macrogol 4000 are 1000:2.5, till continuing stirring until formation gel under the water-bath of 75 DEG C；
(5) gel that step (4) is formed is put and be dried 12 h in 110 DEG C in an oven, by in the crucible loading jacketed after dried gel abrasive, interior crucible setting-out product outer crucible is put activated carbon and builds lid, it is placed in Muffle furnace, calcination 4h at 1000 DEG C, naturally cool to room temperature, obtain blue-green long persistence luminescent material.
By prepared luminescent material after light-illuminating 15 min, remove light source, material be can be observed in the dark and can persistently turn blue more than green glow 10h.
Embodiment 2
A kind of blue-green long persistence luminescent material, its chemical expression is Mn0.005Zr0.9975P2O7, preparation method comprises the following steps:
(1) raw material ZrOCl is the most accurately weighed2·8H2O、(NH4)2HPO4And MnCO3；
(2) H is then weighed3BO3And citric acid, H3BO3Being 0.2:1 with the mol ratio of luminescent material, citric acid is 0.8:1 with the mol ratio of luminescent material；
(3) ZrOCl2·8H2O、(NH4)2HPO4、H3BO3Add water with citric acid and be configured to the mixture solution A that mass percent concentration is 15wt%；At MnCO3The nitric acid of middle addition 3mol/L also makes it be completely dissolved, then adds distilled water and be configured to the settled solution B that mass percent concentration is 15wt%；
(4) solution A step (3) prepared and solution B mix homogeneously, with the pH value of 65wt% nitre acid-conditioning solution to 3；Adding Macrogol 4000 subsequently in the mixed solution of A and B, the mixed solution of A and B and the weight ratio of Macrogol 4000 are 1000:0.5, till continuing stirring until formation gel under the water-bath of 65 DEG C；
(5) gel that step (4) is formed is put and be dried 12 h in 110 DEG C in an oven, by in the crucible loading jacketed after dried gel abrasive, interior crucible setting-out product outer crucible is put activated carbon and builds lid, it is placed in Muffle furnace, calcination 5 h at 950 DEG C, naturally cool to room temperature, obtain blue-green long persistence luminescent material.
By prepared luminescent material after light-illuminating 15 min, remove light source, material be can be observed in the dark and can persistently turn blue more than green glow 8.5h.
Embodiment 3
A kind of blue-green long persistence luminescent material, its chemical expression is Mn0.12Zr0.94P2O7, preparation method comprises the following steps:
(1) raw material ZrOCl is the most accurately weighed2·8H2O、(NH4)2HPO4And MnCO3；
(2) H is then weighed3BO3And citric acid, H3BO3Being 1.2:1 with the mol ratio of luminescent material, citric acid is 3.5:1 with the mol ratio of luminescent material；
(3) ZrOCl2·8H2O、(NH4)2HPO4、H3BO3Add water with citric acid and be configured to the mixture solution A that mass percent concentration is 30wt%；At MnCO3The nitric acid of middle addition 3mol/L also makes it be completely dissolved, then adds distilled water and be configured to the settled solution B that mass percent concentration is 30wt%；
(4) solution A step (3) prepared and solution B mix homogeneously, with the pH value of 65wt% nitre acid-conditioning solution to 2；Adding Macrogol 4000 subsequently in the mixed solution of A and B, the mixed solution of A and B and the weight ratio of Macrogol 4000 are 1000:5, till continuing stirring until formation gel under the water-bath of 85 DEG C；
(5) gel that step (4) is formed is put and be dried 12 h in 110 DEG C in an oven, by in the crucible loading jacketed after dried gel abrasive, interior crucible setting-out product outer crucible is put activated carbon and builds lid, it is placed in Muffle furnace, calcination 3 h at 1100 DEG C, naturally cool to room temperature, obtain blue-green long persistence luminescent material.
By prepared luminescent material after light-illuminating 15 min, remove light source, material be can be observed in the dark and can persistently turn blue more than green glow 7h.
Mn synthesized by the present inventionxZr1-0.5xP2O7Long after glow luminous material, its X-ray diffraction data (see figure 1) consistent with the 49-1079 in PDF standard card, emission peak is one and is positioned at 471nm(Fig. 2 from 420 to 550 the widest bands of a spectrum, main peak), for blue green light.The centre of luminescence of luminescent material is Zr4+And Mn2+, wherein blue-light-emitting part comes from Zr4+And green emitting comes from Mn2+.Oxygen defect can be produced, in the thermoluminescence from Fig. 3, it can be clearly seen that having the strongest heat to release peak at 358K, this peak belongs to oxygen defect in reducing atmosphere.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent and modification, all should belong to the covering scope of the present invention.

Claims (4)

1. a blue-green long persistence luminescent material, it is characterised in that: the centre of luminescence of described luminescent material is Zr4+And Mn2+, its chemical expression is MnxZr1-0.5xP2O7, wherein x=0.005 ~ 0.12.
2. the method preparing blue-green long persistence luminescent material as claimed in claim 1, it is characterised in that: specifically include following steps:
(1) raw material ZrOCl is the most accurately weighed2·8H2O、(NH4)2HPO4And MnCO3；
(2) H is then weighed3BO3And citric acid；
(3) ZrOCl2·8H2O、(NH4)2HPO4、H3BO3Add water with citric acid and be configured to the mixture solution A that mass percent concentration is 15 ~ 30wt%；At MnCO3The nitric acid of middle addition 3mol/L also makes it be completely dissolved, then adds distilled water and be configured to the settled solution B that mass percent concentration is 15 ~ 30wt%；
(4) solution A step (3) prepared and solution B mix homogeneously, with the pH value of 25wt% ammonia or 65wt% nitre acid-conditioning solution to 2 ~ 5；Macrogol 4000 is added subsequently, till continuing stirring until formation gel under the water-bath of 65 ~ 85 DEG C in the mixed solution of A and B；
(5) gel that step (4) is formed is put and be dried 12 h in 110 DEG C in an oven, by in the crucible loading jacketed after dried gel abrasive, interior crucible setting-out product outer crucible is put activated carbon and builds lid, it is placed in Muffle furnace, calcination 2 ~ 5 h at 950 ~ 1100 DEG C, naturally cool to room temperature, obtain blue-green long persistence luminescent material.
The preparation method of blue-green long persistence luminescent material the most according to claim 2, it is characterised in that: H in step (2)3BO3Being 0.2 ~ 1.2:1 with the mol ratio of luminescent material, citric acid is 0.8 ~ 3.5:1 with the mol ratio of luminescent material.
The preparation method of blue-green long persistence luminescent material the most according to claim 2, it is characterised in that: in step (4), the mixed solution of A and B and the weight ratio of Macrogol 4000 are 1000:0.5 ~ 5.
CN201610385593.7A 2016-06-03 2016-06-03 A kind of blue-green long persistence luminescent material and preparation method thereof Expired - Fee Related CN105969350B (en)

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CN107722978A (en) * 2017-10-30 2018-02-23 闽南师范大学 A kind of multi-component oxide long after glow luminous material and preparation method thereof
CN108569902A (en) * 2018-06-12 2018-09-25 闽南师范大学 A kind of blue-green accumulating type luminous stone and preparation method thereof
CN108892504A (en) * 2018-06-12 2018-11-27 闽南师范大学 A kind of blue-green multicomponent light storage ceramic material and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107722978A (en) * 2017-10-30 2018-02-23 闽南师范大学 A kind of multi-component oxide long after glow luminous material and preparation method thereof
CN107722978B (en) * 2017-10-30 2020-11-06 闽南师范大学 Multi-component oxide long-afterglow luminescent material and preparation method thereof
CN108569902A (en) * 2018-06-12 2018-09-25 闽南师范大学 A kind of blue-green accumulating type luminous stone and preparation method thereof
CN108892504A (en) * 2018-06-12 2018-11-27 闽南师范大学 A kind of blue-green multicomponent light storage ceramic material and preparation method thereof
CN108892504B (en) * 2018-06-12 2020-12-29 闽南师范大学 Blue-green multi-component light-storing ceramic material and preparation method thereof
CN108569902B (en) * 2018-06-12 2021-01-29 闽南师范大学 Blue-green energy storage type luminous stone and preparation method thereof

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