CN106833640B - A kind of fluorescent powder and preparation method thereof - Google Patents
A kind of fluorescent powder and preparation method thereof Download PDFInfo
- Publication number
- CN106833640B CN106833640B CN201710097233.1A CN201710097233A CN106833640B CN 106833640 B CN106833640 B CN 106833640B CN 201710097233 A CN201710097233 A CN 201710097233A CN 106833640 B CN106833640 B CN 106833640B
- Authority
- CN
- China
- Prior art keywords
- fluorescent powder
- oxide
- compound
- application according
- sintering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C09K11/7756—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing neodynium
-
- 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
-
- 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
-
- 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
Abstract
The application belongs to field of material technology, and in particular to a kind of fluorescent powder and preparation method thereof.The chemical stability of fluorescent powder provided by the present invention is good, and launching efficiency is high, can be excited within the scope of visible region.The chemical composition expression formula of the fluorescent powder is Bi2O3: xRe, wherein Re is the rare earth element being doped in basis material, is Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb or Lu；It prepares the product stability height that the prices of raw materials are cheap, and low for equipment requirements, preparation is simple, favorable repeatability, obtain, easy to promote large-scale and production application.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of fluorescent powder and preparation method thereof.
Background technique
Fluorescent powder stores luminous energy after by the irradiation such as natural light, daylight light, ultraviolet light, is stopping illumination
It after penetrating, then slowly releases in a manner of fluorescence, so at night or dark, remaining to see luminous, the duration
Up to a few houres to ten a few houres.Excitation and the design of emission band are for LED fluorescent powder, laser lighting fluorescent powder, long range
Night vision monitoring etc. be all it is particularly significant, the two is indispensable.The excitation wave band of fluorescent powder is mainly and rear-earth-doped ion is in difference
Advanced transition in matrix is related, mainly usually controls the excitation of fluorescent powder by member rare earth doped in fluorescent powder matrix at present
Wave band.
For current many fluorescent materials, those skilled in the art intentionally get using visible light as excitation light source and realize
The fluorescent material of specific emission wavelength.However, in existing fluorescent material due to the distinctive luminosity of rare earth ion and
Its higher level structure, so that realizing that excitation of the fluorescent powder within the scope of visible region becomes very difficult.
Summary of the invention
In view of this, the present invention provides the fluorescent powder that can be excited in visible light near infrared range of one kind and its
Preparation method floods partial level by using the method for the host material doping with rare-earth ions of narrow band gap, realizes fluorescent powder
Excitation wave band is moved into visual field.
The specific technical solution of the present invention is as follows:
The present invention provides a kind of fluorescent powders, as shown in formula (I):
Bi2O3:xRe (Ⅰ)；
Wherein, Re is rare earth element, one in Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Eu and Lu
Kind is a variety of；
X is the doping mole of Re, 0.001≤x≤0.1.
The present invention also provides a kind of preparation method of above-mentioned fluorescent powder, are as follows: Bi compound will be contained and compound containing Re mixes
It closes, is sintered, obtains the fluorescent powder；
Wherein, Re is selected from one of Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Eu and Lu or a variety of；
The molar ratio of Bi and Re is 2:x in the compound containing Bi and compound containing Re；0.001≤x≤0.1.
Preferably, the compound containing Bi is selected from the oxide of Bi；
The compound containing Re is selected from the oxide of Re and/or the nitrate of Re.
Preferably, the oxide of the Bi is Bi2O3。
Preferably, the temperature of the sintering is 600~1000 DEG C.
Preferably, the time of the sintering is 4~8h.
Preferably, the atmosphere of the sintering is air atmosphere.
Preferably, the sintering uses high temperature process furnances.
Preferably, the mixed container is mortar.
The present invention provides a kind of fluorescent powders, and chemical stability is good, and launching efficiency is high, can within the scope of visible region quilt
Excitation, transmitting is red to arrive a variety of coloured light of near-infrared.The chemical composition expression formula of the fluorescent powder is Bi2O3: xRe, wherein Re is doping
Rare earth element into basis material is Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb or Lu；It prepares former material
Expect cheap, low for equipment requirements, preparation is simple, favorable repeatability, and obtained product stability is high, is easy to big
Scale is promoted and production application.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the X-ray diffractogram of fluorescent powder prepared in embodiment 1；
Fig. 2 is the diffusing reflectance spectra of fluorescent powder prepared in embodiment 1；
Fig. 3 is the excitation spectrum of fluorescent powder prepared in embodiment 1；
Fig. 4 is the reflectance spectrum of fluorescent powder prepared in embodiment 1；
Fig. 5 is the diffusing reflectance spectra of fluorescent powder prepared in embodiment 2；
Fig. 6 is the excitation spectrum of fluorescent powder prepared in embodiment 2；
Fig. 7 is the reflectance spectrum of fluorescent powder prepared in embodiment 2；
Fig. 8 is the excitation spectrum of fluorescent powder prepared in embodiment 3；
Fig. 9 is the reflectance spectrum of fluorescent powder prepared in embodiment 3；
Figure 10 is the excitation spectrum of fluorescent powder prepared in embodiment 4；
Figure 11 is the emission spectrum of fluorescent powder prepared in embodiment 4；
Figure 12 is the excitation spectrum of fluorescent powder prepared in embodiment 5；
Figure 13 is the emission spectrum of fluorescent powder prepared in embodiment 5.
Specific embodiment
It is had excellent performance to provide one kind, the fluorescent powder that can be excited in visible light near infrared range, the present invention
Flood partial level by using the method for the host material doping with rare-earth ions of narrow band gap, realize the excitation wave band of fluorescent powder to
It is moved within the scope of visual field.
The present invention provides a kind of fluorescent powders, as shown in formula (I):
Bi2O3:xRe (Ⅰ)；
Wherein, Re is rare earth element, one in Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Eu and Lu
Kind is a variety of, more preferably Nd, Sm, Er, Tm or Eu；
X is the doping mole of Re, 0.001≤x≤0.1, preferably 0.001≤x≤0.08, more preferably 0.003≤x
≤ 0.07, most preferably x=0.001,0.002,0.005 or 0.1.
The present invention also provides the preparation method of above-mentioned fluorescent powder, are as follows: Bi compound and the mixing of compound containing Re will be contained, into
Row sintering, obtains the fluorescent powder；
Wherein, Re is selected from one of Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Eu and Lu or a variety of；
The molar ratio of Bi and Re is 2:x, 0.001≤x≤0.1 in the compound containing Bi and compound containing Re.
The present invention is not particularly limited the source for preparing raw material, is commercially available.In the present invention, contain Bi
Compound is selected from the oxide of Bi, most preferably Bi2O3；Compound containing Re is selected from the oxide of Re or the nitrate of Re, most preferably
For the oxide of Re.
Further, the temperature of the sintering is 600~1000 DEG C, and the time is 4~8h.
Further, the atmosphere of the sintering is air atmosphere.
Further, the sintering uses high temperature process furnances, and the high temperature process furnances are preferably Muffle furnace.
Further, the mixed container is mortar.
Further, effect is fired to improve, mixture can also be preheated before sintering, temperature is preferably
500~600 DEG C, preheating time is preferably 2~3h.
Technical solution of the present invention is clearly and completely described below in conjunction with description of the invention attached drawing, it is clear that
Described embodiment is a part of the embodiment of the present invention, instead of all the embodiments.Those skilled in the art should manage
Solution, modifies to specific embodiments of the present invention or is replaced on an equal basis to some technical characteristics, without departing from the present invention
The spirit of technical solution should all cover in the scope of protection of the invention.
The X-ray diffraction detection of sample to be tested uses the general analysis XD-2X x ray diffractometer x in Beijing in following embodiment；Exciting light
Spectrum detection uses Edinburg FLS-980 Fluorescence Spectrometer；Diffusing reflection spectrum detection is divided using Evolution-220 UV, visible light
Photometer；Excitation spectrum detection uses Edinburg FLS-980 Fluorescence Spectrometer.
Embodiment 1
According to the chemical composition of fluorescent powder: Bi2O3:0.005Nd3+, Bi is weighed respectively2O3And Nd2O3, molar ratio 1:
0.005, it is sufficiently mixed and puts high temperature process furnances into after being ground uniformly in mortar and be sintered, at 800 DEG C in air environment
6h is fired, the fluorescent powder is obtained.
Fluorescent powder obtained in the present embodiment is analyzed, as a result as shown in Figure 1 to 4.The X-ray diffractogram of Fig. 1
Proof obtains bismuth oxide pure phase；There is apparent absorption peak at 500~850nm in the spectrogram that diffuses of Fig. 2, illustrates institute
The fluorescent powder of preparation can effectively be excited by the wavelength within the scope of this；Fig. 3 is resulting excitation spectrum under 1077nm wavelength detecting, figure
In occur obvious excitation peak in 450~650nm, illustrate that the fluorescent powder can be by excited by visible light；Fig. 4 is under 577nm wavelength
Resulting emission spectrum is excited, apparent emission peak is shown at 1077nm wavelength, illustrates that the fluorescent powder can emit near-infrared
Light.
Embodiment 2
According to the chemical composition of fluorescent powder: Bi2O3:0.005Er3+, Bi is weighed respectively2O3And Er2O3, molar ratio 1:
0.005, it is sufficiently mixed and puts high temperature process furnances into after being ground uniformly in mortar and be sintered, at 800 DEG C in air environment
6h is fired, the fluorescent powder is obtained.
Fluorescent powder obtained in the present embodiment is analyzed, as a result as shown in Fig. 5~Fig. 7.In the diffusing reflection spectrum of Fig. 5
Occur apparent absorption peak in figure at 500~850nm, illustrates that prepared fluorescent powder can effectively be swashed by the wavelength within the scope of this
Hair；Fig. 6 is resulting excitation spectrum under 1547nm wavelength, occurs obvious excitation peak at 450~700nm, illustrates the fluorescence
Powder can be by excited by visible light；Fig. 7 is that resulting emission spectrum is excited under 516nm wavelength, is shown at 1547nm wavelength in figure
Apparent emission peak out illustrates that the fluorescent powder can emit near infrared light.
Embodiment 3
According to the chemical composition of fluorescent powder: Bi2O3:0.001Tm3+, Bi is weighed respectively2O3And Tm2O3, molar ratio 1:
0.001, it is sufficiently mixed and puts high temperature process furnances into after being ground uniformly in mortar and be sintered, at 800 DEG C in air environment
6h is fired, the fluorescent powder is obtained.
Fluorescent powder obtained in the present embodiment is analyzed, as a result as shown in Figure 8 and Figure 9.Fig. 8 is under 810nm wavelength
Resulting excitation spectrum is detected, occurs obvious excitation peak at 600~750nm, illustrates that the fluorescent powder can be by excited by visible light.Figure
9, to excite resulting emission spectrum under 673nm wavelength, show apparent emission peak in figure at 810nm wavelength, illustrate this
Fluorescent powder can emit near infrared light.
Embodiment 4
According to the chemical composition of fluorescent powder: Bi2O3:0.02Eu3+, Bi is weighed respectively2O3And Eu2O3, molar ratio 1:
0.02, it is sufficiently mixed and puts high temperature process furnances into after being ground uniformly in mortar and be sintered, burnt in air environment at 800 DEG C
6h processed obtains the fluorescent powder.
Fluorescent powder obtained in the present embodiment is analyzed, as a result as shown in Figure 10 and Figure 11.Figure 10 is 612nm wavelength
It is lower to detect resulting excitation spectrum, occur obvious excitation peak in 450~550nm in figure, illustrates that the fluorescent powder can be by visible light
Excitation；Figure 11 is that resulting emission spectrum is excited under 465nm wavelength, and apparent transmitting is shown at 612nm wavelength in figure
Peak illustrates that the fluorescent powder can emit feux rouges.
Embodiment 5
According to the chemical composition of fluorescent powder: Bi2O3:0.1Sm3+, Bi is weighed respectively2O3And Sm2O3, molar ratio 1:
0.1, it is sufficiently mixed and puts high temperature process furnances into after being ground uniformly in mortar and be sintered, burnt in air environment at 800 DEG C
6h processed obtains the fluorescent powder.
Fluorescent powder obtained in the present embodiment is analyzed, as a result as shown in Figure 12 and Figure 13.Figure 12 is 653nm wavelength
It is lower to detect resulting excitation spectrum, occur obvious excitation peak in 450~550nm in figure, illustrates that the fluorescent powder can be by visible light
Excitation；Figure 13 is that resulting emission spectrum is excited under 490nm wavelength, and apparent emission peak is shown at 653nm wavelength, is said
The bright fluorescent powder can emit feux rouges.
Embodiment described above is some embodiments of the invention, but embodiments of the present invention are not by described
The limitation of embodiment, other any various modifications done without departing from spirit of the invention and basic principle, simplification, substitution,
It improves, modification and simply combination and displacement belong within the scope of the present invention.
Claims (8)
1. a kind of application of bismuth-system compound oxide in fluorescent powder, which is characterized in that in visible light near infrared range
The bismuth-system compound oxide is excited, bismuth system compound emits red light near infrared light；
The bismuth-system compound oxide is compound shown in formula (I):
Bi2O3:xRe (I)；
Wherein, Re Nd, Sm, Er, Tm or Eu；
X is the doping mole of Re, 0.001≤x≤0.1；
The bismuth-system compound oxide the preparation method comprises the following steps:
Bi compound and the mixing of compound containing Re will be contained, be sintered, obtain the fluorescent powder；
The molar ratio of Bi and Re is 2:x in the compound containing Bi and compound containing Re.
2. application according to claim 1, which is characterized in that the compound containing Bi is selected from the oxide of Bi；
The compound containing Re is selected from the oxide of Re and/or the nitrate of Re.
3. application according to claim 1, which is characterized in that the oxide of the Bi is Bi2O3。
4. application according to claim 1, which is characterized in that the temperature of the sintering is 600~1000 DEG C.
5. application according to claim 1, which is characterized in that the time of the sintering is 4~8h.
6. application according to claim 1, which is characterized in that the atmosphere of the sintering is air atmosphere.
7. application according to claim 1, which is characterized in that the sintering uses high temperature process furnances.
8. application according to claim 1, which is characterized in that the mixed container is mortar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710097233.1A CN106833640B (en) | 2017-02-22 | 2017-02-22 | A kind of fluorescent powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710097233.1A CN106833640B (en) | 2017-02-22 | 2017-02-22 | A kind of fluorescent powder and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106833640A CN106833640A (en) | 2017-06-13 |
| CN106833640B true CN106833640B (en) | 2019-08-09 |
Family
ID=59133276
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710097233.1A Active CN106833640B (en) | 2017-02-22 | 2017-02-22 | A kind of fluorescent powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106833640B (en) |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6503316B1 (en) * | 2000-09-22 | 2003-01-07 | Dmc2 Degussa Metals Catalysts Cerdec Ag | Bismuth-containing laser markable compositions and methods of making and using same |
| CN101670285B (en) * | 2009-09-16 | 2012-07-04 | 桂林理工大学 | Visible light responding Bi-system composite oxide photocatalyst Bi2-xRxO3 and preparation method |
| CN105206855B (en) * | 2015-09-10 | 2018-03-30 | 刘备之 | A kind of composite electrolyte membrane for oxygen processed |
-
2017
- 2017-02-22 CN CN201710097233.1A patent/CN106833640B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106833640A (en) | 2017-06-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Lovisa et al. | White photoluminescence emission from ZrO2 co-doped with Eu3+, Tb3+ and Tm3+ | |
| Ma et al. | Tunable emission, thermal stability and energy-transfer properties of SrAl2Si2O8: Ce3+/Tb3+ phosphors for w-LEDs | |
| CN105754598A (en) | Rare earth-doped nanometer spherical TiO2 up-conversion compound and preparation method thereof | |
| CN101225304A (en) | Multi-band fluorescent infrared up-conversion material based on sensitizer substrate | |
| Singh et al. | Optical properties of Sr2La8 (SiO4) 6O2 doped with Ho3+ phosphor | |
| CN107502350A (en) | A kind of praseodymium doped laminated perovskite type red long afterglow luminous material, Its Preparation Method And Use | |
| CN109666481A (en) | A kind of long after glow luminous material and preparation method thereof | |
| CN106701074B (en) | A kind of metatitanic acid alkali red up-conversion luminescent material and preparation method thereof | |
| EP2489718B1 (en) | Bismuth ion sensitized rare earth germanate luminescence materials and preparation methods thereof | |
| CN100386405C (en) | Red long afterglow luminescent material and its prepn | |
| CN114774125B (en) | Long-afterglow luminescent material and preparation method thereof | |
| Jia et al. | Synthesis and luminescence properties of orange–red phosphor Ba 2 ScNbO 6: Sm 3+ | |
| CN104531144A (en) | CaMg<2>Al<16>O<27>:Mn <4+> red fluorescent powder and preparation technology thereof | |
| CN106833640B (en) | A kind of fluorescent powder and preparation method thereof | |
| RU2390535C2 (en) | Infrared luminophor based on yttrium oxysulphide | |
| CN102181287B (en) | Ytterbium and thulium double-doped calcium tungstate polycrystalline powder blue upconversion material and preparation method thereof | |
| CN108276998A (en) | Samaric ion doping metatitanic acid gadolinium barium red fluorescence powder and preparation method thereof | |
| CN108504357A (en) | A kind of titanium aluminate-base up-conversion luminescent material, preparation method and application | |
| CN104710987B (en) | Tantalate-based up-conversion luminescent material and preparation method thereof | |
| Xiaoxia et al. | Photoluminescence characteristics of Gd2Mo3O9: Eu phosphor particles by solid state reaction method | |
| CN106867524B (en) | A kind of preparation and application of alkaline earth aluminate blue fluorescent material | |
| CN106085423A (en) | Conversion of white light material C aF in one2: Yb3+/ Eu3+/ Y3+ | |
| Jiang et al. | Investigation on the luminescent properties of a novel Bi3+ based blue long afterglow phosphor Ca14Ga10Zn6O35: Bi3+ | |
| CN105524615A (en) | Niobate red phosphor for white-light LEDs and preparation method thereof | |
| CN106147765A (en) | Infrared stealthy luminescent material of a kind of false proof molybdate and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200819 Address after: Room 410, 4th floor, Lingang logistics park office building, 612 Jianshe Road East section, Pingdingshan City, Henan Province Patentee after: Pingdingshan Lingang optoelectronic Research Institute Co., Ltd Address before: 510062, No. 729, Dongfeng East Road, Guangzhou, Guangdong, Yuexiu District Patentee before: GUANGDONG University OF TECHNOLOGY |
|
| TR01 | Transfer of patent right |