CN109337684A - A kind of three strontium yttrium borate base white fluorescent powder of dysprosium doped and preparation method thereof - Google Patents
A kind of three strontium yttrium borate base white fluorescent powder of dysprosium doped and preparation method thereof Download PDFInfo
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- CN109337684A CN109337684A CN201811108229.1A CN201811108229A CN109337684A CN 109337684 A CN109337684 A CN 109337684A CN 201811108229 A CN201811108229 A CN 201811108229A CN 109337684 A CN109337684 A CN 109337684A
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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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/778—Borates
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Abstract
The invention discloses a kind of three strontium yttrium borate base white fluorescent powder of dysprosium doped and preparation method thereof, chemical general formulas are as follows: Sr3Y1‑x(BO3)3: xDy, wherein 0.01≤x≤0.15.It can effectively be excited by black light, issue the high white light of excitation purity.The present invention is that white fluorescent 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 three strontium yttrium borate base white fluorescent powder of dysprosium doped 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, commercial white light LEDs generate white light, mainly passing through blue light excites YAG:Ce3+Fluorescent powder, but generate white
Light lacks red color components, causes its color rendition index lower, colour temperature is higher.Redgreenblue is coated near ultraviolet LED chip
Fluorescent powder, forms feux rouges near ultraviolet excitation three primary colors fluorescent powder, green light, blue light combination can also issue white light, but this
There are still many problems in proportion regulation for kind method, and luminous efficiency and color reducibility is caused to be greatly affected.Therefore,
It is badly in need of studying a kind of white emitting fluorescent powder that can be effectively excited, solves the proportion regulation between three primary colors fluorescent powder, energy damages
The problems such as consumption, color reabsorb.Rare earth ion Dy3+Since the white light emission of itself is (by positioned at 470~500nm's4F9/2→6H15/2Transition and positioned at 570~600nm's4F9/2→6H13/2Transition composition) and be concerned.Therefore, research can be by black light
Effectively excitation, the three strontium yttrium borate base white emitting fluorescent powder of dysprosium doped that luminous intensity is high, purity is good have good practical application valence
Value.
Summary of the invention
The object of the present invention is to provide a kind of three strontium yttrium borate base white fluorescent powders of dysprosium doped and preparation method thereof, solve three
Primary colours fluorescent powder is in problem present on proportion regulation.
The technical scheme adopted by the invention is that
A kind of three strontium yttrium borate base white fluorescent powder of dysprosium doped, the chemical general formula of the fluorescent powder are Sr3Y1-x(BO3)3: xDy,
Wherein 0.01≤x≤0.15.
The excitation spectrum of the fluorescent powder is in 275~450nm, and main excitation peak is near 351nm, and emission spectrum is 470
~650nm, main peak is near 484nm.
The fluorescent powder can issue white light under near ultraviolet excitation.
A kind of three strontium yttrium borate base white fluorescent powder of dysprosium doped 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 xDy, weigh respectively containing Sr,
Y, weighed raw material is fully ground and is uniformly mixed as raw material by the compound of B, Dy 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 Dy3+Adulterate three strontium yttrium borate fluorescence
Powder Sr3Y1-x(BO3)3: xDy, wherein 0.01≤x≤0.15.
The compound containing Sr, Y, B, Dy element, respectively SrCO3、Y2O3、H3BO3、Dy2O3。
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 to UV excitation, can be applied to white LEDs.Therefore, Sr3Y(BO3)3It can make
For good fluorescent powder basis material.Rare earth ion has good physical and chemical stability and the characteristics of luminescence, the hair of doping
Luminescent material green illumination, short wavelength laser, information are shown, bioluminescence identifies and the fields such as photoelectronics have it is wide
Application prospect.The Sr that the present invention is prepared3Y(BO3)3Base fluorescent powder chemical property is stablized, good luminous performance, luminous intensity
Height, colour rendering is good, can meet the application requirement in White-light LED illumination field.Fluorescent powder prepared by the present invention be suitble to it is near ultraviolet excitated,
Transmitting peak position is located at 484nm, 577nm, and chromaticity coordinates is located at white light field (x=0.334, y=0.371), this shines with the world
The chromaticity coordinates (x=0.33, y=0.33) for the white light that the bright committee provides is close, matches with the light emitting diode of near ultraviolet chip,
Illustrate that fluorescent powder prepared by the present invention is a kind of single-matrix white fluorescent powder of good luminescence property.
The preparation method of three strontium yttrium borate base white fluorescent powder of dysprosium doped 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: 0.04Dy 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 0.04Dy fluorescent powder；
Fig. 3 is the Sr that embodiment 3 is prepared3Y0.96(BO3)3: the CIE chromaticity coordinates figure of 0.04Dy 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 white fluorescent powder of dysprosium doped 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 xDy, weigh respectively containing Sr,
Y, weighed raw material is fully ground and is uniformly mixed as raw material by the compound of B, Dy 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 Dy3+Adulterate three strontium yttrium borate fluorescence
Powder Sr3Y1-x(BO3)3: xDy, wherein 0.01≤x≤0.15.
A kind of three strontium yttrium borate base white fluorescent powder of dysprosium doped 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 0.01Dy accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Dy2O3, 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 Dy3+Adulterate three strontium yttrium borate white fluorescent powders.
Embodiment 2
By chemical formula Sr3Y0.98(BO3)3: the stoichiometric of 0.02Dy accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Dy2O3, 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 Dy3+Adulterate three strontium yttrium borate white fluorescent powders.
Embodiment 3
By chemical formula Sr3Y0.96(BO3)3: the stoichiometric of 0.04Dy accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Dy2O3, 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 Dy3+Adulterate three strontium yttrium borate white fluorescent powders.
Fig. 1 is Sr prepared by the present embodiment 33Y0.96(BO3)3: 0.04Dy 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 0.04Dy fluorescent powder.It should
The excitation spectrum of fluorescent powder is in 275~450nm, and main excitation peak is near 351nm, and emission spectrum is in 470~650nm, hair
It penetrates peak position and is located at 484nm, 577nm, main peak is near 484nm.It can be seen that the fluorescent powder can effectively be swashed by black light
It sends out and issues white 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 0.04Dy fluorescent powder.Chromaticity coordinates is located at
Red light region (x=0.334, y=0.371) illustrates that fluorescent powder prepared by the present invention is a kind of white fluorescent of good luminescence property
Powder.
Embodiment 4
By chemical formula Sr3Y0.9(BO3)3: the stoichiometric of 0.1Dy accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Dy2O3, 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 Dy3+Adulterate three strontium yttrium borate white fluorescent powders.
Embodiment 5
By chemical formula Sr3Y0.85(BO3)3: the stoichiometric of 0.15Dy accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Dy2O3, 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 Dy3+Adulterate three strontium yttrium borate white fluorescent powders.
Claims (7)
1. a kind of three strontium yttrium borate base white fluorescent powder of dysprosium doped, which is characterized in that the chemical general formula of the fluorescent powder is Sr3Y1-x
(BO3)3: xDy, wherein 0.01≤x≤0.15.
2. three strontium yttrium borate base white fluorescent powder of dysprosium doped as described in claim 1, which is characterized in that the excitation of the fluorescent powder
Spectrum is in 275~450nm, and main excitation peak is near 351nm, and for emission spectrum in 470~650nm, main peak is attached in 484nm
Closely.
3. three strontium yttrium borate base white fluorescent powder of dysprosium doped as claimed in claim 2, which is characterized in that the fluorescent powder energy
It is enough to issue white light under near ultraviolet excitation.
4. a kind of preparation method of three strontium yttrium borate base white fluorescent powder of dysprosium doped, which comprises the following steps:
(1) according to the chemical structural formula Sr of fluorescent powder3Y1-x(BO3)3: the mol ratio amount of xDy, weigh respectively containing Sr, Y, B,
The compound of Dy 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 Dy3+Adulterate three strontium yttrium borate fluorescent powders
Sr3Y1-x(BO3)3: xDy, wherein 0.01≤x≤0.15.
5. the preparation method of three strontium yttrium borate base white fluorescent powder of dysprosium doped as claimed in claim 4, which is characterized in that described
The compound containing Sr, Y, B, Dy element, respectively SrCO3、Y2O3、H3BO3、Dy2O3。
6. the preparation method of three strontium yttrium borate base white fluorescent powder of dysprosium doped 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 white fluorescent powder of dysprosium doped 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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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4926091A (en) * | 1988-09-07 | 1990-05-15 | U.S. Philips Corporation | Luminescent terbium-activated borate, luminescent screen provided with such a borate and low-pressure mercury vapor discharge lamp provided with such a screen |
| 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 |
| CN102191052A (en) * | 2010-03-15 | 2011-09-21 | 海洋王照明科技股份有限公司 | Borate red luminescent material and preparation method thereof |
| CN108342193A (en) * | 2018-04-27 | 2018-07-31 | 京东方科技集团股份有限公司 | A kind of fluorescent powder and preparation method thereof |
-
2018
- 2018-09-21 CN CN201811108229.1A patent/CN109337684A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4926091A (en) * | 1988-09-07 | 1990-05-15 | U.S. Philips Corporation | Luminescent terbium-activated borate, luminescent screen provided with such a borate and low-pressure mercury vapor discharge lamp provided with such a screen |
| 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 |
| CN102191052A (en) * | 2010-03-15 | 2011-09-21 | 海洋王照明科技股份有限公司 | Borate red luminescent material and preparation method thereof |
| CN108342193A (en) * | 2018-04-27 | 2018-07-31 | 京东方科技集团股份有限公司 | A kind of fluorescent powder and preparation method thereof |
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