CN103897695A - Orange red rear earth long-afterglow luminescent material suitable for near ultraviolet excitation and preparation method thereof - Google Patents

Orange red rear earth long-afterglow luminescent material suitable for near ultraviolet excitation and preparation method thereof Download PDF

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CN103897695A
CN103897695A CN201410009895.5A CN201410009895A CN103897695A CN 103897695 A CN103897695 A CN 103897695A CN 201410009895 A CN201410009895 A CN 201410009895A CN 103897695 A CN103897695 A CN 103897695A
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luminescent material
orange red
afterglow luminescent
rare earth
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CN103897695B (en
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汪正良
胡芬芬
周美丽
朱怡雯
程萍
郭俊明
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Yunnan Minzu University
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Abstract

The invention relates to the field of white light emitting diodes, and discloses a method for preparing an orange red rear earth long-afterglow luminescent material suitable for near ultraviolet excitation. The chemical composition of the orange red rear earth long-afterglow luminescent material provided by the invention is M<II>3(1-x-y)M<III>2O5Cl2: xEu<2+>, yR<III>, wherein M<II> is one or two of alkaline earth metal ions Sr<2+> and Ba<2+>; M<III> is one or two of Al<3+> and B<3+>; R<III> is one of Dy<3+>, Nd<3+>, La<3+> and Pr<3+>; x and y are molar percentage coefficients of corresponding doping ions relative to M<II> ions, x is not smaller than 0.0 and not greater than 0.50, and y is not smaller than 0.0 and not greater than 0.20. The orange red rear earth long-afterglow luminescent material provided by the invention is prepared by a high-temperature solid phase method. The orange red fluorescent powder provided by the invention mainly emits orange yellow light of 600 nm under near ultraviolet excitation, so that the luminous efficiency is high; after being irradiated for 30 minutes by a 365 nm ultraviolet lamp, the orange red rear earth long-afterglow luminescent material is placed in a dark box, and the afterglow time can reach 4 hours.

Description

A kind of orange red rare earth long-afterglow luminescent material that is applicable near ultraviolet excitation and preparation method thereof
Technical field
The present invention relates to a kind of orange red rare earth long-afterglow luminescent material and preparation method thereof, specifically, is a kind of orange red rare earth long-afterglow luminescent material that is applicable near ultraviolet excitation and preparation method thereof.Belong to rare earth material preparation field.
Background technology
The problems such as current environment pollution and energy dilemma have caused countries in the world extensive concern, and novel " energy-conservation " and " green " have become the study hotspot of material science.Long after glow luminous material (claiming again long persistence luminescent powder) is a kind of novel energy-saving and environmental protection shaped material, it does not need external power source that energy is provided, the energy of energy automatic absorption sunlight or light, and portion of energy is wherein stored in material, then the form slow release by visible ray is out the energy of storing in material.Utilize its this characteristic, long after glow luminous material beautifies with the field such as technique U.S., information storage, imaging demonstration, biological label art and is with a wide range of applications in low light level illumination, emergent Warning Mark, building.
Early stage long after glow luminous material is mainly the sulfide of mixing transition metal ion, and the luminosity of long persistence luminous sulfide material is low, and luminous time of persistence is short, can not meet whole noctilucent requirement.What current people's research was the most ripe is alkali earth metal aluminate green long afterglow luminescent material, and its luminous efficiency is high, and time of persistence is long, but meets water unstable, and color is single.In addition rare-earth activated silicate long-afterglow material is also an important subject of present long-afterglow material.Silicate compared with oxide compound, sulfide, aluminate etc., have acidproof, alkaline-resisting, water-fast, and good chemical stability.The research of silicate long-afterglow material.This type of long-afterglow material mainly comprises Sr 2mgSi 2o 7: Eu 2+, Dy 3+, Ca 2mgSi 2o 7: Eu 2+, Tb 3+, Ba 2mgSi 2o 7: Eu 2+, Tm 3+, Sr 3mgSi 2o 8: Eu 2+, Dy 3+, Ca 3mgSi 2o 8: Eu 2+, Dy 3+, Ba 3mgSi 2o 8: Eu 2+, Dy 3+deng.Although the research of silicate long-afterglow material obtains very large progress in recent years, in general, the afterglow property of silicate systems does not reach the level of aluminates system yet.
It is a kind of inorganic fluorescent powder out newly developed in recent years that alkaline-earth metal halogen aluminate is mixed rare earth luminescent material.Alkaline-earth metal halogen aluminate substrate is stable, has different crystalline structure according to their composition, proportioning difference; Rare earth ion with alkaline-earth metal ions radius (as Sr 2+) approach, be conducive to the doping of rare earth ion, therefore alkaline-earth metal halogen aluminate is suitable as the luminous host of rare earth ion.Immature for the research of current long after glow luminous material, we propose to study Novel alkali earth metals halogen aluminate and mix rare earth long-afterglow luminescent material tool and have very important significance.
Summary of the invention
The object of the invention is the deficiency for existing rare earth long-afterglow luminescent material, provide that a kind of luminous efficiency is high, good stability, be suitable for the orange red rare earth long-afterglow luminescent material of near ultraviolet excitation.
Another object of the present invention is to provide the preparation method of above-mentioned rare earth long-afterglow luminescent material.
To achieve these goals, the orange red rare earth long-afterglow luminescent material that is applicable near ultraviolet excitation of the present invention, its chemical constitution is:
M II 3(1-x-y)M III 2O 5Cl 2:?xEu 2+,?yR III。M iIfor alkaline-earth metal ions Sr 2+, Ba 2+in one two several; M iIIfor Al 3+, B 3+in one or both; R iIIfor Dy 3+, Nd 3+, La 3+, Pr 3+in one; X, y are the relative M of corresponding dopant ion iIthe molar percentage coefficient that ion is shared, 0.0≤x≤0.50,0.0≤y≤0.20.The quality percentage composition of raw material type used in the present invention and each raw material is respectively: Strontium carbonate powder (SrCO 3): 0 ~ 51.70 %; Barium carbonate (BaCO 3): 0 ~ 54.99 %; Six water strontium chloride (SrCl 26H 2o): 0 ~ 37.15 %; Bariumchloride (BaCl 2): 0 ~ 25.48 %; Aluminium hydroxide [Al (OH) 3]: 0 ~ 21.73 %; Boric acid (H3BO3): 0 ~ 18.04 %, europiumsesquioxide (Eu2O3): 0 ~ 21.46 %; Dysprosium trioxide (Dy2O3): 0 ~ 12.88 %; Neodymium sesquioxide (Nd2O3): 0 ~ 12.88 %; Lanthanum sesquioxide (La2O3): 0 ~ 12.88 %; Praseodymium trioxide (Pr6O11): 0 ~ 12.88 %.
Work as M iIfor alkaline-earth metal ions Sr 2+, Ba 2+in two kinds time, the emission peak half-peak width of sample can become large with respect to wherein a kind of, and and the emissive porwer of sample can be significantly improved; M iIIfor Al 3+, B 3+in two kinds time when wherein a kind of, the emissive porwer of sample and twilight sunset life time can be significantly improved.
Near-ultraviolet light of the present invention, refers to the near-ultraviolet light of sending out 380～410 nm.
The preparation method of above-mentioned rare earth orange-red long afterglow Luminescent Material, adopts high temperature solid-state method, comprises the steps: various raw materials in agate mortar, to mix in proportion, pre-burning 3～6 hours at 400～500 DEG C, be chilled to room temperature, take out and again grind evenly, in 1000～1200 DEG C of H 2in atmosphere, reduce sintering 4～10 hours, by levigate gained sinter the finished product.
Rare earth orange-red long afterglow Luminescent Material of the present invention has very strong orange red light emission (emission peak is positioned at 600 nm left and right) under near ultraviolet excitation, and luminous efficiency is high.Ultra violet lamp 30 min at 365nm are placed in camera bellows, and can reach 4 h its time of persistence.
Brief description of the drawings
Fig. 1 is room temperature excitation spectrum (monitoring wavelength is 600 nm) and the emmission spectrum (excitation wavelength is 400 nm) of orange-red long afterglow Luminescent Material of the present invention;
Fig. 2 is the decay of afterglow curve of orange-red long afterglow Luminescent Material of the present invention.
Embodiment
Embodiment 1:
Take Strontium carbonate powder (SrCO 3): 2.8 g (43.67 %), bariumchloride (BaCl 2): 2.08 g(32.44 %), aluminium hydroxide [Al (OH) 3]: 1.17 g(18.25 %), boric acid (H 3bO 3): 0.325 g(5.08 %), europiumsesquioxide (Eu 2o 3): 0.0176 g(0.27 %), Dysprosium trioxide (Dy 2o 3): 0.0187 g(0.29 %), after fully grinding in agate mortar and mixing, at 500 DEG C, pre-burning 4 hours, is chilled to room temperature, takes out and again grinds evenly, in 1200 DEG C of H 2in atmosphere, reduce sintering 4 hours, by levigate gained sinter the finished product Sr 1.9baAl 1.5b 0.5o 5cl 2: 0.05Eu 2+, 0.05Dy 3+.
The luminescent properties of this fluorescent material as shown in Figure 1, in near-ultraviolet light district, (250 nm ~ 450 nm) has the very strong broadband excitation that excites to sample. and the emmission spectrum under 400 nm optical excitation is as shown in Figure 1, the transmitting of sample be orange red light emission taking 600 about nm as main, this corresponding to Eu 2+4f 65d 1-4f 7transition.
Figure 2 shows that the decay of afterglow curve of sample.Work as Eu 2+when ion is excited, its portions of electronics can be by RE 3+(RE=Dy 3+, Nd 3+, La 3+, Pr 3+) produce trap level capture, at room temperature enter hot activation and get back to Eu 2+ion t 2energy level or eenergy level, then produces twilight sunset phenomenon.Ultra violet lamp 30 min at 365 nm are placed in camera bellows, and can reach 4 h its time of persistence.
Embodiment 2:
Take Strontium carbonate powder (SrCO 3): 2.8 g (39.62 %), six water strontium chloride (SrCl 26H 2o): 2.67 g(37.78 %), aluminium hydroxide [Al (OH) 3]: 1.56 g(22.09 %), europiumsesquioxide (Eu 2o 3): 0.0176 g(0.25 %), Dysprosium trioxide (Dy 2o 3): 0.0187 g(0.26 %), after fully grinding in agate mortar and mixing, at 500 DEG C, pre-burning 4 hours, is chilled to room temperature, takes out and again grinds evenly, in 1200 DEG C of H 2in atmosphere, reduce sintering 6 hours, by levigate gained sinter the finished product Sr 2.9al 2o 5cl 2: 0.05Eu 2+, 0.05Dy 3+.
Embodiment 3:
Take Strontium carbonate powder (SrCO 3): 2.8 g (39.99 %), six water strontium chloride (SrCl 26H 2o): 2.67 g(38.14 %), aluminium hydroxide [Al (OH) 3]: 1.17 g(16.71 %), boric acid (H 3bO 3): 0.325 g(4.64 %), europiumsesquioxide (Eu 2o 3): 0.0176 g(0.25 %), Dysprosium trioxide (Dy 2o 3): 0.0187 g(0.27 %), after fully grinding in agate mortar and mixing, at 500 DEG C, pre-burning 4 hours, is chilled to room temperature, takes out and again grinds evenly, in 1200 DEG C of H 2in atmosphere, reduce sintering 4 hours, by levigate gained sinter the finished product Sr 2.9al 1.5b 0.5o 5cl 2: 0.05Eu 2+, 0.05Dy 3+.
Embodiment 4:
Take Strontium carbonate powder (SrCO 3): 2.8 g(40.37 %), six water strontium chlorides: (SrCl 26H 2o) 2.67 g(38.49 %), aluminium hydroxide [Al (OH) 3]: 0.78 g(11.25 %), boric acid (H 3bO 3): 0.61 g(9.37 %), europiumsesquioxide (Eu 2o 3): 0.0176 g(0.25 %), neodymium sesquioxide (Nd 2o 3): 0.0168 g(0.24 %), after fully grinding in agate mortar and mixing, at 500 DEG C, pre-burning 6 hours, is chilled to room temperature, takes out and again grinds evenly, in 1200 DEG C of H 2in atmosphere, reduce sintering 2 hours, by levigate gained sinter the finished product Sr 2.9alBO 5cl 2: 0.05Eu 2+, 0.05Nd 3+.
Embodiment 5:
Take Strontium carbonate powder (SrCO 3): 2.66 g (38.22 %), six water strontium chlorides: (SrCl 26H 2o) 2.67 g(38.37 %), aluminium hydroxide [Al (OH) 3]: 1.56 g(22.42 %), europiumsesquioxide (Eu 2o 3): 0.0352 g(0.51 %), neodymium sesquioxide (Nd 2o 3): 0.0336 g(0.48 %), after fully grinding in agate mortar and mixing, at 500 DEG C, pre-burning 4 hours, is chilled to room temperature, takes out and again grinds evenly, in 1200 DEG C of H 2in atmosphere, reduce sintering 8 hours, by levigate gained sinter the finished product Sr 2.8al 2o 5cl 2: 0.1Eu 2+, 0.1Nd 3+.
Embodiment 6:
Take Strontium carbonate powder (SrCO 3): 2.66 g (38.24 %), six water strontium chlorides: (SrCl 26H 2o) 2.67 g(38.37 %), aluminium hydroxide [Al (OH) 3]: 1.56 g(22.42 %), europiumsesquioxide (Eu 2o 3): 0.0352 g(0.51 %), lanthanum sesquioxide (Nd 2o 3): 0.0325 g(0.46 %), after fully grinding in agate mortar and mixing, at 500 DEG C, pre-burning 4 hours, is chilled to room temperature, takes out and again grinds evenly, in 1200 DEG C of H 2in atmosphere, reduce sintering 8 hours, by levigate gained sinter the finished product Sr 2.8al 2o 5cl 2: 0.1Eu 2+, 0.1La 3+.
Embodiment 7:
Take Strontium carbonate powder (SrCO 3): 2.66 g (38.23 %), six water strontium chlorides: (SrCl 26H 2o) 2.67 g(38.37 %), aluminium hydroxide [Al (OH) 3]: 1.56 g(22.42 %), europiumsesquioxide (Eu 2o 3): 0.0352 g(0.51 %), Praseodymium trioxide (Pr 6o 11): 0.0340 g(0.47 %), after fully grinding in agate mortar and mixing, at 500 DEG C, pre-burning 4 hours, is chilled to room temperature, takes out and again grinds evenly, in 1200 DEG C of H 2in atmosphere, reduce sintering 10 hours, by levigate gained sinter the finished product Sr 2.8al 2o 5cl 2: 0.1Eu 2+, 0.1Pr 3+.

Claims (6)

1. an orange red rare earth long-afterglow luminescent material that is applicable near ultraviolet excitation, its chemical constitution is: M iI 3 (1-x-y)m iII 2o 5cl 2: xEu 2+, yR iII, M iIfor alkaline-earth metal ions Sr 2+, Ba 2+in one or both; M iIIfor Al 3+, B 3+in one or both; R iIIfor Dy 3+, Nd 3+, La 3+, Pr 3+in one; X, y are the relative M of corresponding dopant ion iIthe molar percentage coefficient that ion is shared, 0.0≤x≤0.50,0.0≤y≤0.20.
2. the orange red rare earth long-afterglow luminescent material that is applicable near ultraviolet excitation as claimed in claim 1, is characterized in that described near-ultraviolet light refers to that wavelength is the light of 380～410nm.
3. the orange red rare earth long-afterglow luminescent material that is applicable near ultraviolet excitation as claimed in claim 1, it is characterized in that described orange red rare earth long-afterglow luminescent material is placed in camera bellows at ultra violet lamp 30 min of 365nm, can reach 4 h its time of persistence.
4. the preparation method of an orange red rare earth long-afterglow luminescent material as claimed in claim 1, it is characterized in that preparation method comprises the steps: various raw materials in agate mortar, to mix in proportion, pre-burning 3～6 hours at 400～500 DEG C, be cooled to room temperature, take out and again grind evenly, at 1000～1200 DEG C, in reducing atmosphere, reduce sintering 4～10 hours, by levigate gained sinter the finished product.
5. the preparation method of orange red rare earth long-afterglow luminescent material as claimed in claim 4, is characterized in that described reducing atmosphere is H 2atmosphere.
6. the preparation method of orange red rare earth long-afterglow luminescent material as claimed in claim 4, is characterized in that the kind of used raw material and the quality percentage composition of each raw material are respectively: the quality percentage composition of raw material type used in the present invention and each raw material is respectively: Strontium carbonate powder (SrCO 3): 0 ~ 51.70 %; Barium carbonate (BaCO 3): 0 ~ 54.99 %; Six water strontium chloride (SrCl 26H 2o): 0 ~ 37.15 %; Bariumchloride (BaCl 2): 0 ~ 25.48 %; Aluminium hydroxide [Al (OH) 3]: 0 ~ 21.73 %; Boric acid (H 3bO 3): 0 ~ 18.04 %, europiumsesquioxide (Eu 2o 3): 0 ~ 21.46 %; Dysprosium trioxide (Dy 2o 3): 0 ~ 12.88 %; Neodymium sesquioxide (Nd 2o 3): 0 ~ 12.88 %; Lanthanum sesquioxide (La 2o 3): 0 ~ 12.88 %; Praseodymium trioxide (Pr 6o 11): 0 ~ 12.88 %.
CN201410009895.5A 2014-01-09 2014-01-09 A kind of orange red rare earth long-afterglow luminescent material being applicable near ultraviolet excitation and preparation method thereof Expired - Fee Related CN103897695B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101689989B1 (en) * 2016-01-27 2016-12-26 티오켐 주식회사 Process for Producing Phosphorescent Pigments Having Excellent Afterglow
CN107353894A (en) * 2016-05-09 2017-11-17 云南民族大学 Microwave synthesizes a kind of white rare earth long-afterglow luminescent material of ultraviolet excitation
CN107746708A (en) * 2017-11-02 2018-03-02 杭州显庆科技有限公司 A kind of red long-afterglow phosphor and preparation method thereof
CN112143491A (en) * 2020-10-21 2020-12-29 岭南师范学院 Long-afterglow light conversion agent and application thereof
CN113999672A (en) * 2021-11-22 2022-02-01 厦门理工学院 Stress luminescent material with orange-yellow afterglow and preparation thereof

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Publication number Priority date Publication date Assignee Title
CN101191253A (en) * 2006-11-27 2008-06-04 中国科学院理化技术研究所 Alkali metal borate compounds, single-crystal and preparation method thereof
CN101899297A (en) * 2010-07-15 2010-12-01 兰州大学 Orange-yellow long-afterglow luminescent material and preparation method thereof
CN102191045A (en) * 2011-03-28 2011-09-21 彩虹集团公司 Preparation method of nitrogen oxide green fluorescent powder material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101191253A (en) * 2006-11-27 2008-06-04 中国科学院理化技术研究所 Alkali metal borate compounds, single-crystal and preparation method thereof
CN101899297A (en) * 2010-07-15 2010-12-01 兰州大学 Orange-yellow long-afterglow luminescent material and preparation method thereof
CN102191045A (en) * 2011-03-28 2011-09-21 彩虹集团公司 Preparation method of nitrogen oxide green fluorescent powder material

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101689989B1 (en) * 2016-01-27 2016-12-26 티오켐 주식회사 Process for Producing Phosphorescent Pigments Having Excellent Afterglow
CN107353894A (en) * 2016-05-09 2017-11-17 云南民族大学 Microwave synthesizes a kind of white rare earth long-afterglow luminescent material of ultraviolet excitation
CN107746708A (en) * 2017-11-02 2018-03-02 杭州显庆科技有限公司 A kind of red long-afterglow phosphor and preparation method thereof
CN108659829A (en) * 2017-11-02 2018-10-16 王小琴 A kind of mark of dangerous display
CN107746708B (en) * 2017-11-02 2018-12-04 宁波朗格照明电器有限公司 A kind of red long-afterglow phosphor and preparation method thereof
CN112143491A (en) * 2020-10-21 2020-12-29 岭南师范学院 Long-afterglow light conversion agent and application thereof
CN113999672A (en) * 2021-11-22 2022-02-01 厦门理工学院 Stress luminescent material with orange-yellow afterglow and preparation thereof

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