CN109021976A - Three strontium yttrium borate base red fluorescent powders of a kind of europium doping and preparation method thereof - Google Patents
Three strontium yttrium borate base red fluorescent powders of a kind of europium doping and preparation method thereof Download PDFInfo
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- CN109021976A CN109021976A CN201811109213.2A CN201811109213A CN109021976A CN 109021976 A CN109021976 A CN 109021976A CN 201811109213 A CN201811109213 A CN 201811109213A CN 109021976 A CN109021976 A CN 109021976A
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- 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
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7797—Borates
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Abstract
The invention discloses a kind of europiums to adulterate three strontium yttrium borate base red fluorescent powders and preparation method thereof, chemical general formula are as follows: Sr3Y1‑x(BO3)3: xEu, wherein 0.01≤x≤0.15.It can effectively be excited by near ultraviolet or blue light, issue the high feux rouges of excitation purity.The present invention is that red fluorescence powder 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 europium adulterate three strontium yttrium borate base red fluorescent powders 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, it is mainly the blue light excitation YAG:Ce for passing through the generation of GaIn base chip that commercial white light LEDs, which generate white light,3+Fluorescence
Powder, but generate white light lack red color components, cause its color rendition index lower (Ra<80), correlated colour temperature it is higher (CCT>
7000K), common lighting requirement can only be met.Redgreenblue fluorescent powder is coated, near ultraviolet LED chip near ultraviolet
Light excitated blue, green, red fluorescence powder form blue and green light, feux rouges combination can also issue white light.This method not only may be used
To overcome the problems, such as that conventional white light LED exists, it is also easy to the luminous color of control.Eu3+Through swashing frequently as a kind of red emission
Agent living can emit feux rouges under near ultraviolet or blue light excitation.So Eu3+The transmitting light of doping fluorescent powder can be used as white light
The red color components of LED.Therefore, research can effectively be excited by near ultraviolet, blue light, and the europium that luminous intensity is high, purity is good adulterates three boron
Sour yttrium strontium base red light fluorescent powder has good practical application value.
Summary of the invention
The object of the present invention is to provide a kind of europiums to adulterate three strontium yttrium borate base red fluorescent powders and preparation method thereof, solves to pass
The problems such as red fluorescence powder 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 red fluorescent powders of europium doping, the chemical general formula of the fluorescent powder are Sr3Y1-x(BO3)3: xEu,
Wherein 0.01≤x≤0.15.
The excitation spectrum of the fluorescent powder is in 350~500nm, and main excitation peak is near 393nm, and emission spectrum is 550
~750nm, main peak is near 614nm.
The fluorescent powder can issue feux rouges under near ultraviolet or blue light excitation.
Three strontium yttrium borate base red fluorescent powders of a kind of europium doping 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 xEu, weigh respectively containing Sr,
Y, weighed raw material is fully ground and is uniformly mixed as raw material by the compound of B, Eu 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 Eu3+Adulterate three strontium yttrium borate fluorescence
Powder Sr3Y1-x(BO3)3: xEu, wherein 0.01≤x≤0.15.
The compound containing Sr, Y, B, Eu element, respectively SrCO3、Y2O3、H3BO3、Eu2O3。
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)3Belong to three borates for the fluorescent powder of matrix, it is non-containing 1 in structure
BO3 3-" free oxygen " atom, and one-dimensional energy transmission can be formed along rare earth ion chain, therefore, which can be with rare earth
Ion generates effective energy conversion.Three borate fluorescent powders have very strong excitation spectrum, and all have in ultra-violet (UV) band one very strong
Excitation peak, thus luminous intensity is higher.So Sr3Y(BO3)3Good fluorescent powder basis material can be used as.By mixing
Miscellaneous active ions Eu3+, main peak can be obtained under near ultraviolet (393nm) and blue light (465nm) excitation be located at strong light near 614nm
Degree is compared with strong, the higher feux rouges of excitation purity.The Sr that the present invention is prepared3Y(BO3)3Base fluorescent powder chemical property is stablized, photism
Can be good, luminous intensity is high, and colour rendering is good, can meet the application requirement in White-light LED illumination field.Fluorescent powder prepared by the present invention is suitable
Near ultraviolet or blue light excitation are closed, transmitting peak position is located at 593nm, 614nm, 707nm, and chromaticity coordinates is located at red light region (x=
0.635, y=0.365) it, is matched with the light emitting diode of near ultraviolet chip and blue chip, illustrates fluorescent powder prepared by the present invention
It is a kind of red fluorescence powder of good luminescence property.
Europium provided by the invention adulterates the preparation method of three strontium yttrium borate base red fluorescent powders, and preparation method is 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: 0.04Eu 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 0.04Eu fluorescent powder；
Fig. 3 is the Sr that embodiment 3 is prepared3Y0.96(BO3)3: the CIE chromaticity coordinates figure of 0.04Eu fluorescent powder.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of europium of the present invention adulterates three strontium yttrium borate base red fluorescent powders and preparation method thereof, 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 xEu, weigh respectively containing Sr,
Y, weighed raw material is fully ground and is uniformly mixed as raw material by the compound of B, Eu 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 Eu3+Adulterate three strontium yttrium borate fluorescence
Powder Sr3Y1-x(BO3)3: xEu, wherein 0.01≤x≤0.15.
A kind of europium of the present invention adulterates three strontium yttrium borate base red fluorescent powders 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 0.01Eu accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Eu2O3, 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 Eu3+Adulterate three strontium yttrium borate red fluorescence powders.
Embodiment 2
By chemical formula Sr3Y0.98(BO3)3: the stoichiometric of 0.02Eu accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Eu2O3, 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
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 Eu3+Adulterate three strontium yttrium borate red fluorescence powders.
Embodiment 3
By chemical formula Sr3Y0.96(BO3)3: the stoichiometric of 0.04Eu accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Eu2O3, 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 Eu3+Adulterate three strontium yttrium borate red fluorescence powders.
Fig. 1 is Sr prepared by the present embodiment 33Y0.96(BO3)3: 0.04Eu 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 0.04Eu fluorescent powder.It should
The excitation spectrum of fluorescent powder is in 350~500nm, and main excitation peak is near 393nm, and emission spectrum is in 550~750nm, hair
It penetrates peak position and is located at 593nm, 614nm, 707nm, main peak is near 614nm.It can be seen that the fluorescent powder can be by black light
It effectively excites and issues feux rouges, 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 0.04Eu fluorescent powder.Chromaticity coordinates is located at
Red light region (x=0.635, y=0.365) illustrates that fluorescent powder prepared by the present invention is a kind of red fluorescence of good luminescence property
Powder.
Embodiment 4
By chemical formula Sr3Y0.9(BO3)3: the stoichiometric of 0.1Eu accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Eu2O3, 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 Eu3+Adulterate three strontium yttrium borate red fluorescence powders.
Embodiment 5
By chemical formula Sr3Y0.85(BO3)3: the stoichiometric of 0.15Eu accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Eu2O3, 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 Eu3+Adulterate three strontium yttrium borate red fluorescence powders.
Claims (7)
1. a kind of europium adulterates three strontium yttrium borate base red fluorescent powders, which is characterized in that the chemical general formula of the fluorescent powder is Sr3Y1-x
(BO3)3: xEu, wherein 0.01≤x≤0.15.
2. europium as described in claim 1 adulterates three strontium yttrium borate base red fluorescent powders, which is characterized in that the excitation of the fluorescent powder
Spectrum is in 350~500nm, and main excitation peak is near 393nm, and for emission spectrum in 550~750nm, main peak is attached in 614nm
Closely.
3. europium as claimed in claim 2 adulterates three strontium yttrium borate base red fluorescent powders, which is characterized in that the fluorescent powder energy
It is enough to issue feux rouges under near ultraviolet or blue light excitation.
4. the preparation method that a kind of europium adulterates three strontium yttrium borate base red fluorescent powders, which comprises the following steps:
(1) according to the chemical structural formula Sr of fluorescent powder3Y1-x(BO3)3: the mol ratio amount of xEu, weigh respectively containing Sr, Y, B,
The compound of Eu 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 Eu3+Adulterate three strontium yttrium borate fluorescent powders
Sr3Y1-x(BO3)3: xEu, wherein 0.01≤x≤0.15.
5. the preparation method that europium as claimed in claim 4 adulterates three strontium yttrium borate base red fluorescent powders, which is characterized in that described
The compound containing Sr, Y, B, Eu element, respectively SrCO3、Y2O3、H3BO3、Eu2O3。
6. the preparation method that europium as claimed in claim 4 adulterates three strontium yttrium borate base red fluorescent powders, 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 that europium as claimed in claim 4 adulterates three strontium yttrium borate base red fluorescent powders, 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 |
|---|---|---|---|---|
| CN114410301A (en) * | 2021-11-25 | 2022-04-29 | 济南鲁新新型建材股份有限公司 | Strontium-yttrium-europium borate fluorescent powder and preparation method and application thereof |
| CN115612493A (en) * | 2022-09-08 | 2023-01-17 | 上海应用技术大学 | Ultraviolet excited Eu (II) single-doped red light emitting fluorescent powder and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033900A (en) * | 2017-05-27 | 2017-08-11 | 陕西科技大学 | Three boric acid lanthanum-strontium base green light fluorescent powders of a kind of europium doping and preparation method thereof |
-
2018
- 2018-09-21 CN CN201811109213.2A patent/CN109021976A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033900A (en) * | 2017-05-27 | 2017-08-11 | 陕西科技大学 | Three boric acid lanthanum-strontium base green light fluorescent powders of a kind of europium doping and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| DAN ZHAO ET AL.: "Growth and spectral properties of Er3+/Yb3+-codoped Sr3Y(BO3)3 crystal", 《JOURNAL OF CRYSTAL GROWTH》 * |
| MIAOMIAO TIAN ET AL.: "Synthesis, color-tunable emission, thermal stability, luminescence and energy transfer of Sm3+ and Eu3+ single-doped M3Tb(BO3)3 (M = Sr and Ba) phosphors", 《CRYSTENGCOMM》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114410301A (en) * | 2021-11-25 | 2022-04-29 | 济南鲁新新型建材股份有限公司 | Strontium-yttrium-europium borate fluorescent powder and preparation method and application thereof |
| CN115612493A (en) * | 2022-09-08 | 2023-01-17 | 上海应用技术大学 | Ultraviolet excited Eu (II) single-doped red light emitting fluorescent powder and preparation method and application thereof |
| CN115612493B (en) * | 2022-09-08 | 2024-03-26 | 上海应用技术大学 | Ultraviolet excited Eu (II) single doped red light emitting fluorescent powder and preparation method and application thereof |
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