CN107652972A - A kind of self-activation long-afterglow material of Color tunable and preparation method thereof - Google Patents

A kind of self-activation long-afterglow material of Color tunable and preparation method thereof Download PDF

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CN107652972A
CN107652972A CN201711039813.1A CN201711039813A CN107652972A CN 107652972 A CN107652972 A CN 107652972A CN 201711039813 A CN201711039813 A CN 201711039813A CN 107652972 A CN107652972 A CN 107652972A
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long
glow
afterglow
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self
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CN107652972B (en
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邱忠贤
朱桂颖
廉世勋
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Hunan Normal University
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    • 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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7715—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
    • C09K11/7716—Chalcogenides
    • 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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7701—Chalogenides
    • 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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
    • C09K11/7729—Chalcogenides
    • 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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7759—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing samarium
    • C09K11/776—Chalcogenides

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  • Inorganic Chemistry (AREA)
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  • Luminescent Compositions (AREA)

Abstract

The invention provides a kind of self-activation long-afterglow material of Color tunable, its name composition can be expressed as：Na2SnO3：xRE (RE=Eu3+、Sm3+、Tm3+、Dy3+、Ce3+).When not adding rare earth ion as activator (x=0); by the glow color for changing synthesis atmosphere conditional regulatory material; respectively under air, nitrogen or argon atmosphere, carbon monoxide weakly reducing atmosphere; the self-activation fluorescent material that glow color is respectively green, blue-green and blueness can be obtained, there is blue long afterflow property.When adding a kind of above-mentioned rare earth ion therein as activator ion (x=0.0001 0.05), the long after glow luminous material of Color tunable can be obtained.RE is Eu3+Or Sm3+When, red long afterglow material can be obtained, and by adjusting Eu3+Or Sm3+Doping concentration, nearly white light emission fluorescent material can be obtained；RE is Tm3+When, glow color adjustable fluorescent material from blue light to green glow is obtained, there is blue long afterflow material；RE is Dy3+When, obtain glow color adjustable fluorescent material from green glow to warm white；RE is Ce3+When, obtain bluish-white light emitting phosphor.

Description

A kind of self-activation long-afterglow material of Color tunable and preparation method thereof
Technical field
The present invention relates to a kind of long after glow luminous material of Color tunable, belong to phosphor field.
Background technology
Long-afterglow material is the luminescent material of a kind of accumulating type, can when being excited by electron storage in trap, from And the continuous illumination after excitation source stopping.Long after glow luminous material is in military project instrument, false proof, secure ID, display and medicine Tracer etc. has a wide range of applications.All the time, the research of long-afterglow material concentrates on rear-earth-doped sulfide, sulphur oxygen Compound, alkali earth metal aluminate and silicate systems, and the II-VI semi-conducting materials of doped transition metal ionses.In recent years, Researchers are found that several base metal stannate system long-afterglow materials successively, more than the green length with self-activate luminescence Brightness Mg2SnO4, rear-earth-doped red long-afterglow SrSnO3:Sm3+, white long afterglow fluorescent material CaSnO3:Eu3+,Tb3+.Alkali gold Category stannate fluorescent material and long-afterglow material have not been reported.
The content of the invention
The invention provides a kind of alkali metal stannate self-activation long-afterglow material of Color tunable, and preparation method thereof with Synthesis condition.Fluorescent material of the present invention, its name composition can be expressed as：Na2SnO3：xRE (x=0-0.05；RE= Eu3 +、Sm3+、Tm3+、Dy3+、Ce3+).The synthetic method of the luminescent material is high temperature solid-state method, with Na2CO3For sodium source, SnO2For tin Source, synthesis temperature 700-1100oC, it is characterised in that the amount ratio of the material of raw material composition is nNa : nSn = (1+m) : 1 (0 ＜ m≤4.0), i.e. Na in raw material2CO3Must be excessive.
When not adding rare earth ion as activator（x=0）, more than change synthesis atmosphere conditional regulatory self-activation length The glow color of brightness material.When it is air to synthesize atmosphere, the glow color for obtaining material is green, and transmitting main peak is located at 515 Nm, emission spectrum covering 360-750 nm wave-length coverages, has blue long afterflow property；When synthesis atmospheric condition is inert gas When nitrogen or argon gas, the glow color for obtaining material is blue-green, and emission spectrum includes two broadband emissions, and main peak is located at respectively 470 nm and 500 nm, emission spectrum covering 360-750 nm wave-length coverages, have blue long afterflow property；And when synthesis atmosphere When condition is carbon monoxide weakly reducing atmosphere, the glow color for obtaining material is blueness, and transmitting main peak is located at 469 nm, launches light Spectrum covering 360-650 nm wave-length coverages.
As addition Eu3+、Sm3+、Tm3+、Dy3+Or Ce3+In a kind of rare earth ion as activator ion when（x= 0.0001-0.05）, the long after glow luminous material of Color tunable can be obtained.When activator ion is Eu3+Or Sm3+When, in sky Under the conditions of gas, the characteristic emission spectrum of trivalent rare earth ionses can be respectively obtained, and there is red long-afterglow property；Pass through regulation Eu3+Or Sm3+Doping concentration, matrix broadband emission can also be obtained and sent out with the compound nearly white light of trivalent rare earth ionses peak emission Penetrate fluorescent material.When activator ion is Tm3+When, under air conditionses, obtain blue long afterflow material；By adjusting Tm3+Doping Concentration, it is possible to achieve controllable adjustment of the light-emitting phosphor color from blue light to green glow.When activator ion is Dy3+When, in air Under the conditions of, adjust Dy3+Doping concentration can obtain glow color adjustable fluorescent material from green glow to warm white.Work as activator ion For Ce3+When, the glow color for obtaining material is Bluish white, and emission spectrum covers 360-700 nm wave-length coverages.
Brief description of the drawings
Fig. 1：The emission spectrum of sodium stannate self-activation long lad phosphor under different atmosphere
Fig. 2：The twilight sunset launching light spectrogram of sodium stannate self-activation long lad phosphor
Fig. 3：The decay of afterglow curve map of sodium stannate self-activation long lad phosphor
Fig. 4：Na2SnO3: 0.001Eu3+Phosphor emission spectrogram
Fig. 5：Na2SnO3: 0.005Sm3+Phosphor emission spectrogram
Fig. 6：Na2SnO3: 0.01Tm3+Phosphor emission spectrogram
Fig. 7：Na2SnO3: 0.01Dy3+Phosphor emission spectrogram
Fig. 8：Na2SnO3: 0.01Ce3+Phosphor emission spectrogram
Embodiment
It is the non-limiting examples of fluorescent material synthesis of the present invention below：
Example 1：Green Na under air atmosphere2SnO3Self-activation fluorescent material
Product is synthesized using high temperature solid state reaction.Stoichiometrically weigh Na2CO34.2396 g, SnO21.5070 g, match somebody with somebody Abrasive lapping uniformly loads corundum crucible afterwards；Crucible is put into box-type high-temperature furnace, temperature programming to 1000 DEG C be incubated 6 hours；So Stop heating afterwards, cool down and produce fluorescent material product.The fluorescent material does not add Doped ions, and there is self-activating ultraviolet light to turn green Photoemissive luminosity, and there is blue long afterflow property, the characteristic emission spectrum of the fluorescent material is as shown in figure 1, after-glow light Spectrum is as shown in Fig. 2 decay of afterglow curve is as shown in Figure 3.
Example 2：Blue-green Na under inert gas shielding atmosphere2SnO3Self-activation fluorescent material
Product is synthesized using high temperature solid state reaction.Stoichiometrically weigh Na2CO31.9078 g, SnO22.2609 g, match somebody with somebody Abrasive lapping uniformly loads corundum crucible afterwards；Crucible is pushed into tube type high-temperature furnace, is continually fed into N2Stream, temperature programming is to 900 DEG C Insulation 6 hours；Then stop heating, be cooled to room temperature, produce fluorescent material product.There is the fluorescent material self-activating ultraviolet light to turn Bluish-green photoemissive luminosity, its characteristic emission spectrum as shown in figure 1, its persistent quality with being made in example 1 under air atmosphere Standby sample is consistent.
Example 3：Blue Na under CO weakly reducing atmospheres2SnO3Self-activation fluorescent material
Product is synthesized using high temperature solid state reaction.Stoichiometrically weigh Na2CO33.1797 g, SnO22.2605 g, match somebody with somebody Abrasive lapping uniformly loads corundum crucible afterwards；Crucible is put into the large size crucible equipped with carbon dust, is capped, is sent into box-type high-temperature furnace In, temperature programming to 950 DEG C be incubated 6 hours；Then heating is stopped, taking-up is cooled to room temperature, produces fluorescent material product.This is glimmering Light powder has the luminosity that self-activating ultraviolet light turns blue emission, and its characteristic emission spectrum is as shown in Figure 1.
Example 4：Na2SnO3: 0.001Eu3+Fluorescent material
Product is synthesized using high temperature solid state reaction.Stoichiometrically weigh Na2CO31.9078 g, SnO21.8084 g, Eu2O30.0021 g, uniformly load corundum crucible afterwards with abrasive lapping；Crucible is put into box-type high-temperature furnace, temperature programming is extremely 1000 DEG C are incubated 6 hours；Then stop heating, cool down and produce fluorescent material product.Fluorescent material characteristic emission spectrum as shown in figure 4, In the case where the nm of substrate fluorescent powder excitation wavelength 277 is excited, the broadband emission and Eu of host material can be obtained simultaneously3+Feature it is red Light is launched, therefore can pass through Eu3+Nearly white light emission is realized in the regulation and control of doping concentration, and the fluorescent material has red long-afterglow Matter.
Example 5：Na2SnO3: 0.005Sm3+Fluorescent material
Product is synthesized using high temperature solid state reaction.Stoichiometrically weigh Na2CO32.0668 g, SnO22.2605 g, Sm2O30.0131 g, load corundum crucible after dispensing mill is even；Crucible is put into box-type high-temperature furnace, temperature programming is to 1000 DEG C Insulation 6 hours；Then stop heating, cool down and produce fluorescent material product.The fluorescent material characteristic emission spectrum is as shown in figure 5, in base The nm of matter fluorescent material excitation wavelength 277 is excited down, can obtain the broadband emission and Sm of host material simultaneously3+Feature orange light Transmitting, therefore Sm can be passed through3+Nearly white light emission is realized in the regulation and control of doping concentration, and the fluorescent material has red long-afterglow Matter.
Example 6：Na2SnO3: 0.01Tm3+Fluorescent material
Product is synthesized using high temperature solid state reaction.Stoichiometrically weigh Na2CO32.4802g SnO21.9591 g, Tm2O30.0251 g, uniformly load corundum crucible afterwards with abrasive lapping；Crucible is put into box-type high-temperature furnace, temperature programming is extremely 1000 DEG C are incubated 6 hours；Then stop heating, cool down and produce fluorescent material product.The fluorescent material characteristic emission spectrum such as Fig. 6 institutes Show, can be by adjusting Tm3+Doping concentration realizes controllable adjustment of the light-emitting phosphor color from blue light to green glow, and with blueness Long afterglow qualities.
Example 7：Na2SnO3: 0.01Dy3+Fluorescent material
Product is synthesized using high temperature solid state reaction.Stoichiometrically weigh Na2CO31.6322 g, SnO22.1098 g, Dy2O30.0261 g, uniformly load corundum crucible afterwards with abrasive lapping；Crucible is put into box-type high-temperature furnace, temperature programming is extremely 1000 DEG C are incubated 6 hours；Then stop heating, cool down and produce fluorescent material product.The fluorescent material characteristic emission spectrum such as Fig. 7 institutes Show, it is observed that Dy under burst of ultraviolel3+Feature white light emission peak, by adjusting Dy3+Doping concentration can realize luminous face Controllable adjustment of the color from green glow to warm white.
Example 8：Na2SnO3: 0.01Ce3+Fluorescent material
Product is synthesized using high temperature solid state reaction.Stoichiometrically weigh Na2CO32.9147 g, SnO21.6577 g, Ce2O30.0180g, uniformly load corundum crucible afterwards with abrasive lapping；Crucible is put into box-type high-temperature furnace, temperature programming to 1000 DEG C insulation 6 hours；Then stop heating, cool down and produce fluorescent material product.The fluorescent material characteristic emission spectrum is as shown in figure 8, purple Outer light, which excites down, is shown as blue or green white light emission, emission spectrum covering 360-700 nm wave-length coverages.

Claims (10)

  1. A kind of 1. self-activation long after glow luminous material, consisting of Na2SnO3, it is characterised in that：Using high temperature solid-state method, synthesis Temperature is 700-1100 DEG C, uses the amount ratio of material of raw material as nNa : nSn= (1+m) :1, wherein sodium source is Na2CO3, Tin source is SnO2, 0 ＜ m≤4.0.
  2. 2. the self-activation long-afterglow material described in claim 1, when it is air to synthesize atmospheric condition, obtain the luminous face of material Color is green, and transmitting main peak is located at 515 nm, emission spectrum covering 360-750 nm wave-length coverages, has blue long afterflow Matter.
  3. 3. the self-activation long-afterglow material described in claim 1, when it is inert nitrogen gas or argon gas to synthesize atmospheric condition, obtain Glow color to material is blue-green, and emission spectrum includes two broadband emissions, and main peak is located at 470 nm and 500 nm respectively, Emission spectrum covers 360-750 nm wave-length coverages, has blue long afterflow property.
  4. 4. the self-activation long-afterglow material described in claim 1, when it is carbon monoxide weakly reducing atmosphere to synthesize atmospheric condition, obtain Glow color to material is blueness, and transmitting main peak is located at 469 nm, emission spectrum covering 360-650 nm wave-length coverages.
  5. A kind of 5. long-afterglow material of Color tunable, consisting of Na2SnO3:XRE, wherein RE are Eu3+、Sm3+、Tm3+、Dy3+、 Ce3+In one kind, x molal quantity is 0.0001-0.05.
  6. 6. the long-afterglow material described in claim 5, when RE is Eu3+When, synthesis atmospheric condition is air, can obtain Eu3+'s Feature red emission, main peak are located at 611 nm, have red long-afterglow property；And by adjusting Eu3+Ion doping concentration x values, Matrix broadband emission and Eu can be obtained3+Compound nearly white light emission fluorescent material.
  7. 7. the long-afterglow material described in claim 5, when RE is Sm3+When, synthesis atmospheric condition is air, can obtain Sm3+'s Feature orange light is launched, and emission spectrum main peak is located at 568,579,605,620,650,724 nm, has red long-afterglow property； And by adjusting Sm3+Ion doping concentration x values, can obtain matrix broadband emission and Sm3+Compound nearly white light emission fluorescence Powder.
  8. 8. the long-afterglow material described in claim 5, when RE is Tm3+When, synthesis atmospheric condition is air, Tm3+Emission spectrum Main peak is located at 480,490 nm, by adjusting Tm3+Doping concentration can obtain glow color adjustable fluorescence from blue light to green glow Powder, there is blue long afterflow property.
  9. 9. the long-afterglow material described in claim 5, when RE is Dy3+When, synthesis atmospheric condition is air, adjusts Dy3+Adulterate dense Degree can obtain glow color adjustable fluorescent material from green glow to warm white.
  10. 10. the long-afterglow material described in claim 5, when RE is Ce3+When, the glow color for obtaining material is Bluish white, transmitting Spectrum covers 360-700 nm wave-length coverages.
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Publication number Priority date Publication date Assignee Title
CN114231278A (en) * 2021-12-17 2022-03-25 厦门稀土材料研究所 Self-activatable ultraviolet long-afterglow luminescent material and preparation method thereof
CN114231278B (en) * 2021-12-17 2023-04-18 厦门稀土材料研究所 Self-activatable ultraviolet long-afterglow luminescent material and preparation method thereof

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