CN109337685A - A kind of three strontium yttrium borate base green emitting phosphor of Er ions and preparation method thereof - Google Patents
A kind of three strontium yttrium borate base green emitting phosphor of Er ions and preparation method thereof Download PDFInfo
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- CN109337685A CN109337685A CN201811108246.5A CN201811108246A CN109337685A CN 109337685 A CN109337685 A CN 109337685A CN 201811108246 A CN201811108246 A CN 201811108246A CN 109337685 A CN109337685 A CN 109337685A
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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Abstract
The invention discloses a kind of three strontium yttrium borate base green emitting phosphor of Er ions and preparation method thereof, chemical general formulas are as follows: Sr3Y1‑x(BO3)3: xEr, wherein 0.01≤x≤0.15.It can effectively be excited by black light, issue the high green light of excitation purity.The present invention is that green emitting phosphor is prepared based on solid-phase synthesis, is prepared in air atmosphere, simple process, favorable reproducibility, short preparation period, and non-pollutant discharge is environmental-friendly, easily operated and industrialized production.
Description
Technical field
The invention belongs to the phosphor technologies field LED, be related to a kind of three strontium yttrium borate base green emitting phosphor of Er ions and
Preparation method.
Background technique
Light emitting diode (Light Emitting Diode, LED) is acknowledged as the new light sources of 21st century, has
Many advantages, such as energy conservation, fast, environmentally protective, the service life is long, small in size, luminous efficiency is high response, has in illumination and display field
Huge application prospect.
Currently, the green emitting phosphor of business is mainly Zn2SiO4:Mn2+And BaAl12O19:Mn2+, however Mn2+Ion
Persistence is long, using being restricted.Therefore it develops and can be had by the green emitting phosphor that black light and blue light effectively excite
Practical application value.Redgreenblue fluorescent powder is coated near ultraviolet LED chip, it is blue near ultraviolet excitation, green, red
Color fluorescent powder forms blue and green light, feux rouges combination can also issue white light.This method can not only overcome conventional white light LED
There are the problem of, be also easy to the luminous color of control.Er3+It, can be near ultraviolet through the activator frequently as a kind of green emission
Wavelength excitation is lower to emit green light.Therefore, research can effectively be excited by black light, the Er ions three that luminous intensity is high, purity is good
Strontium yttrium borate base green light fluorescent powder has good practical application value.
Summary of the invention
The object of the present invention is to provide a kind of three strontium yttrium borate base green emitting phosphor of Er ions and preparation method thereof, solve to pass
The problems such as colour rendering index present in system white light LEDs is low, and colour temperature is high.
The technical scheme adopted by the invention is that
A kind of three strontium yttrium borate base green emitting phosphor of Er ions, the chemical general formula of the fluorescent powder are Sr3Y1-x(BO3)3: xEr,
Wherein 0.01≤x≤0.15.
The excitation spectrum of the fluorescent powder is in 300~425nm, and main excitation peak is near 376nm, and emission spectrum is 500
~600nm, main peak is near 565nm.
The fluorescent powder can be near ultraviolet excitated lower sending green light.
A kind of three strontium yttrium borate base green emitting phosphor of Er ions and preparation method thereof, comprising the following steps:
(1) according to the chemical structural formula Sr of fluorescent powder3Y1-x(BO3)3: the mol ratio amount of xEr, weigh respectively containing Sr,
Y, weighed raw material is fully ground and is uniformly mixed as raw material by the compound of B, Er element；
(2) it by uniform raw material under air atmosphere, is calcined 5-8 hours at 1200 DEG C -1300 DEG C；
(3) it after the completion of calcining, is taken out after being cooled to room temperature, is fully ground crushing, obtains Er3+Adulterate three strontium yttrium borate fluorescence
Powder Sr3Y1-x(BO3)3: xEr, wherein 0.01≤x≤0.15.
The compound containing Sr, Y, B, Er element, respectively SrCO3、Y2O3、H3BO3、Er2O3。
The calcining is to be rapidly heated in resistance furnace to carry out in SX3-10-14 type, in air atmosphere, from room temperature with 5~
The heating rate of 10 DEG C/min rises to 1200 DEG C -1300 DEG C, keeps the temperature 5-8h, later furnace cooling.
The grinding of the raw material, calcined its milling time of grinding are 20~60min.
The beneficial effects of the present invention are:
It is provided by the invention with Sr3Y(BO3)3It is not only at low cost, stability is good, easy preparation for the fluorescent powder of matrix, but also
There is a very strong excitation peak near ultraviolet region, is suitble near ultraviolet excitation, can be applied to white LEDs.Therefore, Sr3Y(BO3)3
Good fluorescent powder basis material can be used as.By adulterating active ions Er3+, can be obtained under black light (379nm) excitation
Winner peak is located at the neighbouring luminous intensity of 565nm compared with strong, the higher green light of excitation purity.The Sr that the present invention is prepared3Y(BO3)3Base
Fluorescent powder chemical property is stablized, good luminous performance, and luminous intensity is high, and colour rendering is good, can meet the application in White-light LED illumination field
It is required that.Fluorescent powder prepared by the present invention is suitble near ultraviolet excitated, and emission peak is located at 526nm, 540nm, 554nm, 565nm,
Chromaticity coordinates is located at green wavelength (x=0.367, y=0.622), matches near ultraviolet chip light emitting diode, illustrates system of the present invention
Standby fluorescent powder is a kind of green light fluorescent powder of good luminescence property.
The preparation method of three strontium yttrium borate base green emitting phosphor of Er ions provided by the invention, preparation method are based on solid
Phase synthesi is come what is prepared, and strong operability is prepared in air atmosphere, and temperature-rise period is simple, and preparation method is simple, reappears
Good, the short preparation period of property.
Detailed description of the invention
Fig. 1 is the Sr that embodiment 3 is prepared3Y0.96(BO3)3: 0.04Er fluorescent powder and Sr3Y(BO3)3The X-ray of matrix
Diffracting spectrum and Ba3Dy(BO3)3Standard card (PDF#50-0098) comparison diagram；
Fig. 2 is the Sr that embodiment 3 is prepared3Y0.96(BO3)3: the excitation spectrum and emission spectrum of 0.04Er fluorescent powder；
Fig. 3 is the Sr that embodiment 3 is prepared3Y0.96(BO3)3: the CIE chromaticity coordinates figure of 0.04Er fluorescent powder.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of three strontium yttrium borate base green emitting phosphor of Er ions of the present invention and preparation method thereof, it is specifically real according to the following steps
It applies:
(1) according to the chemical structural formula Sr of fluorescent powder3Y1-x(BO3)3: the mol ratio amount of xEr, weigh respectively containing Sr,
Y, weighed raw material is fully ground and is uniformly mixed as raw material by the compound of B, Er element；
(2) it by uniform raw material under air atmosphere, is calcined 5-8 hours at 1200-1300 DEG C；
(3) it after the completion of calcining, is taken out after being cooled to room temperature, is fully ground crushing, obtains Er3+Adulterate three strontium yttrium borate fluorescence
Powder Sr3Y1-x(BO3)3: xEr, wherein 0.01≤x≤0.15.
A kind of three strontium yttrium borate base green emitting phosphor of Er ions of the present invention and preparation method thereof, is prepared using solid phase method,
Its luminous intensity is high, simple process, strong operability, short preparation period.
Embodiment 1
By chemical formula Sr3Y0.99(BO3)3: the stoichiometric of 0.01Er accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Er2O3, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.Above-mentioned raw materials are ground
Mill after mixing, is packed into corundum crucible, is placed in and is rapidly heated in resistance furnace, in air atmosphere with the heating rate of 5 DEG C/min
1200 DEG C are risen to, keeps the temperature 5 hours, then furnace cooling is cooled to room temperature to sample.Take out sample regrinding crush to get
To Er3+Adulterate three strontium yttrium borate green emitting phosphors.
Embodiment 2
By chemical formula Sr3Y0.98(BO3)3: the stoichiometric of 0.02Er accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Er2O3, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.Above-mentioned raw materials are ground
Mill after mixing, is packed into corundum crucible, is placed in and is rapidly heated in resistance furnace, in air atmosphere with the heating rate of 8 DEG C/min
1250 DEG C are risen to, keeps the temperature 5 hours, then furnace cooling is cooled to room temperature to sample.Take out sample regrinding crush to get
To Er3+Adulterate three strontium yttrium borate green emitting phosphors.
Embodiment 3
By chemical formula Sr3Y0.96(BO3)3: the stoichiometric of 0.04Er accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Er2O3, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.Above-mentioned raw materials are ground
Mill after mixing, is packed into corundum crucible, is placed in and is rapidly heated in resistance furnace, in air atmosphere with the heating rate of 10 DEG C/min
1250 DEG C are risen to, keeps the temperature 5 hours, then furnace cooling is cooled to room temperature to sample.Take out sample regrinding crush to get
To Er3+Adulterate three strontium yttrium borate green emitting phosphors.
Fig. 1 is Sr prepared by the present embodiment 33Y0.96(BO3)3: 0.04Er fluorescent powder and Sr3Y(BO3)3The X-ray of matrix is spread out
Penetrate map and Ba3Dy(BO3)3Standard card (PDF#50-0098) comparison diagram.At present without discovery Sr in PDF card base3Y
(BO3)3Standard card, but find compared with the crystal structure of this substance similar Ba3Dy(BO3)3Standard card PDF#
Standard card of the 50-0098 as sample diffraction atlas analysis.It can be found that main diffraction peak all with Ba3Dy(BO3)3Standard
Card is corresponding, but all has to big angle of diffraction direction and a little deviate.Reason is that the ionic radius of Sr and Ba is differentCause to deviate to wide-angle；The ionic radius of Y and Dy is very closeInfluence very little to the angle of diffraction.It is seen that object is mutually with high purity, crystallinity
Good, significant change does not occur for doping front and back principal crystalline phase.
Fig. 2 is Sr prepared by the present embodiment 33Y0.96(BO3)3: the excitation spectrum and emission spectrum of 0.04Er fluorescent powder.It should
The excitation spectrum of fluorescent powder is in 300~425nm, and main excitation peak is near 379nm, and emission spectrum is in 500~600nm, hair
It penetrates peak position and is located at 526nm, 540nm, 554nm, 565nm, main peak is near 565nm.It can be seen that the fluorescent powder can be close
Ultraviolet light effectively excites and issues green light, can be applied to white light LEDs.
Fig. 3 is Sr prepared by the present embodiment 33Y0.96(BO3)3: the CIE chromaticity coordinates figure of 0.04Er fluorescent powder.Chromaticity coordinates is located at
Green wavelength (x=0.367, y=0.622) illustrates that fluorescent powder prepared by the present invention is a kind of green fluorescence of good luminescence property
Powder.
Embodiment 4
By chemical formula Sr3Y0.9(BO3)3: the stoichiometric of 0.1Er accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Er2O3, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.Above-mentioned raw materials are ground
Mill after mixing, is packed into corundum crucible, is placed in and is rapidly heated in resistance furnace, in air atmosphere with the heating rate of 10 DEG C/min
1250 DEG C are risen to, keeps the temperature 7 hours, then furnace cooling is cooled to room temperature to sample.Take out sample regrinding crush to get
To Er3+Adulterate three strontium yttrium borate green emitting phosphors.
Embodiment 5
By chemical formula Sr3Y0.85(BO3)3: the stoichiometric of 0.15Er accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Er2O3, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.Above-mentioned raw materials are ground
Mill after mixing, is packed into corundum crucible, is placed in and is rapidly heated in resistance furnace, in air atmosphere with the heating rate of 10 DEG C/min
1300 DEG C are risen to, keeps the temperature 8 hours, then furnace cooling is cooled to room temperature to sample.Take out sample regrinding crush to get
To Er3+Adulterate three strontium yttrium borate green emitting phosphors.
Claims (7)
1. a kind of three strontium yttrium borate base green emitting phosphor of Er ions, which is characterized in that the chemical general formula of the fluorescent powder is Sr3Y1-x
(BO3)3: xEr, wherein 0.01≤x≤0.15.
2. three strontium yttrium borate base green emitting phosphor of Er ions as described in claim 1, which is characterized in that the excitation of the fluorescent powder
Spectrum is in 300~425nm, and main excitation peak is near 379nm, and for emission spectrum in 500~600nm, main peak is attached in 565nm
Closely.
3. three strontium yttrium borate base green emitting phosphor of Er ions as claimed in claim 2, which is characterized in that the fluorescent powder energy
It is enough to issue green light under near ultraviolet excitation.
4. a kind of preparation method of three strontium yttrium borate base green emitting phosphor of Er ions, which comprises the following steps:
(1) according to the chemical structural formula Sr of fluorescent powder3Y1-x(BO3)3: the mol ratio amount of xEr, weigh respectively containing Sr, Y, B,
The compound of Er element is fully ground and is uniformly mixed as raw material, by weighed raw material；
(2) it by uniform raw material under air atmosphere, is calcined 5-8 hours at 1200 DEG C -1300 DEG C；
(3) it after the completion of calcining, is taken out after being cooled to room temperature, is fully ground crushing, obtains Er3+Adulterate three strontium yttrium borate fluorescent powders
Sr3Y1-x(BO3)3: xEr, wherein 0.01≤x≤0.15.
5. the preparation method of three strontium yttrium borate base green emitting phosphor of Er ions as claimed in claim 4, which is characterized in that described
The compound containing Sr, Y, B, Er element, respectively SrCO3、Y2O3、H3BO3、Er2O3。
6. the preparation method of three strontium yttrium borate base green emitting phosphor of Er ions as claimed in claim 4, which is characterized in that described
Calcining, is carried out being rapidly heated in resistance furnace, in air atmosphere, is risen to from room temperature with the heating rate of 5~10 DEG C/min
1200 DEG C -1300 DEG C, keep the temperature 5-8h, later furnace cooling.
7. the preparation method of three strontium yttrium borate base green emitting phosphor of Er ions as claimed in claim 4, which is characterized in that described
The grinding of raw material and the grinding of post-calcination sample, milling time are 20~60min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110846035A (en) * | 2019-11-28 | 2020-02-28 | 云南大学 | Erbium ion activated fluorescent powder and preparation method thereof |
| CN116814264A (en) * | 2023-06-28 | 2023-09-29 | 南京信息工程大学 | Europium and erbium single-doped and europium and erbium co-doped strontium yttrium indium acid polycrystalline fluorescent powder and preparation method thereof |
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| JP2010285596A (en) * | 2009-03-27 | 2010-12-24 | Tohoku Univ | Oxide crystal for neutron scintillator and neutron scintillator using the same |
| CN102115667A (en) * | 2009-12-30 | 2011-07-06 | 海洋王照明科技股份有限公司 | Borate green luminescent material and preparation method thereof |
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2018
- 2018-09-21 CN CN201811108246.5A patent/CN109337685A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010285596A (en) * | 2009-03-27 | 2010-12-24 | Tohoku Univ | Oxide crystal for neutron scintillator and neutron scintillator using the same |
| CN102115667A (en) * | 2009-12-30 | 2011-07-06 | 海洋王照明科技股份有限公司 | Borate green luminescent material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| DAN ZHAO, GUOFUWANG: "Growth and spectroscopic characterization of Er3+: Sr3Y(BO3)3 crystal", 《JOURNAL OF LUMINESCENCE》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110846035A (en) * | 2019-11-28 | 2020-02-28 | 云南大学 | Erbium ion activated fluorescent powder and preparation method thereof |
| CN110846035B (en) * | 2019-11-28 | 2022-09-13 | 云南大学 | Erbium ion activated fluorescent powder and preparation method thereof |
| CN116814264A (en) * | 2023-06-28 | 2023-09-29 | 南京信息工程大学 | Europium and erbium single-doped and europium and erbium co-doped strontium yttrium indium acid polycrystalline fluorescent powder and preparation method thereof |
| CN116814264B (en) * | 2023-06-28 | 2024-03-15 | 南京信息工程大学 | Europium and erbium single-doped and europium and erbium co-doped strontium yttrium indium acid polycrystalline fluorescent powder and preparation method thereof |
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Application publication date: 20190215 |