CN109181695A - Terbium doped three strontium yttrium borates base green emitting phosphor of one kind and preparation method thereof - Google Patents
Terbium doped three strontium yttrium borates base green emitting phosphor of one kind and preparation method thereof Download PDFInfo
- Publication number
- CN109181695A CN109181695A CN201811117731.9A CN201811117731A CN109181695A CN 109181695 A CN109181695 A CN 109181695A CN 201811117731 A CN201811117731 A CN 201811117731A CN 109181695 A CN109181695 A CN 109181695A
- Authority
- CN
- China
- Prior art keywords
- emitting phosphor
- green emitting
- preparation
- terbium doped
- strontium yttrium
- 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.)
- Pending
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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/778—Borates
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of terbium doped three strontium yttrium borates base green emitting phosphor and preparation method thereof, chemical general formulas are as follows: Sr3Y1‑x(BO3)3: xTb, 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 terbium doped three strontium yttrium borates base green emitting phosphor 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.
The green emitting phosphor of business is mainly Zn at present2SiO4:Mn2+And BaAl12O19:Mn2+, however Mn2+Ion it is remaining
The brightness time is long, using being restricted.Therefore the green emitting phosphor that developing can effectively be excited by black light and blue light has real
Border application value.Redgreenblue fluorescent powder is coated, near ultraviolet LED chip near ultraviolet excitation blue, green, red
Fluorescent powder forms blue and green light, feux rouges combination can also issue white light.This method not only can overcome conventional white light LED to deposit
The problem of, be also easy to the luminous color of control.Tb3+It, can be near ultraviolet wave through the activator frequently as a kind of green emission
Long excitation is lower to emit green light.Therefore, research can effectively be excited by black light, terbium doped three boron that luminous intensity is high, purity is good
Sour yttrium strontium 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 terbium doped three strontium yttrium borates base green emitting phosphor 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 terbium doped three strontium yttrium borates base green emitting phosphor, the chemical general formula of the fluorescent powder are Sr3Y1-x(BO3)3: xTb,
Wherein 0.01≤x≤0.15.
The excitation spectrum of the fluorescent powder is in 325~400nm, and main excitation peak is near 376nm, and emission spectrum is 475
~650nm, main peak is near 546nm.
The fluorescent powder can be near ultraviolet excitated lower sending green light.
Terbium doped three strontium yttrium borates base green emitting phosphor of one kind 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 xTb, weigh respectively containing Sr,
Y, weighed raw material is fully ground and is uniformly mixed as raw material by the compound of B, Tb 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 Tb3+Adulterate three strontium yttrium borate fluorescence
Powder Sr3Y1-x(BO3)3: xTb, wherein 0.01≤x≤0.15.
The compound containing Sr, Y, B, Tb element, respectively SrCO3、Y2O3、H3BO3、Tb4O7。
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.Rare earth from
Son has an energy level abundant, and the luminescent material of doping shows in green illumination, short wavelength laser, information, bioluminescence mark
Know and the fields such as photoelectronics have broad application prospects.The Sr that the present invention is prepared3Y(BO3)3Base fluorescent powder chemistry
Property is stablized, good luminous performance, and luminous intensity is high, and colour rendering is good, can meet the application requirement in White-light LED illumination field.This hair
The fluorescent powder of bright preparation be suitble to it is near ultraviolet excitated, transmitting peak position be located at 490nm, 546nm, 585nm, 625nm, chromaticity coordinates position
It in green wavelength (x=0.307, y=0.479), matches, illustrates prepared by the present invention glimmering with the light emitting diode of near ultraviolet chip
Light powder is a kind of green emitting phosphor of good luminescence property.
The preparation method of terbium doped three strontium yttrium borates base green emitting phosphor 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: 0.04Tb 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 0.04Tb fluorescent powder；
Fig. 3 is the Sr that embodiment 3 is prepared3Y0.96(BO3)3: the CIE chromaticity coordinates figure of 0.04Tb fluorescent powder.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of terbium doped three strontium yttrium borates base green emitting phosphor of the 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 xTb, weigh respectively containing Sr,
Y, weighed raw material is fully ground and is uniformly mixed as raw material by the compound of B, Tb 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 Tb3+Adulterate three strontium yttrium borate fluorescence
Powder Sr3Y1-x(BO3)3: xTb, wherein 0.01≤x≤0.15.
A kind of terbium doped three strontium yttrium borates base green emitting phosphor of the 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 0.01Tb accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Tb4O7, 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 Tb3+Adulterate three strontium yttrium borate green emitting phosphors.
Embodiment 2
By chemical formula Sr3Y0.98(BO3)3: the stoichiometric of 0.02Tb accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Tb4O7, 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 Tb3+Adulterate three strontium yttrium borate green emitting phosphors.
Embodiment 3
By chemical formula Sr3Y0.96(BO3)3: the stoichiometric of 0.04Tb accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Tb4O7, 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 Tb3+Adulterate three strontium yttrium borate green emitting phosphors.
Fig. 1 is Sr prepared by the present embodiment 33Y0.96(BO3)3: 0.04Tb 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 0.04Tb fluorescent powder.It should
The excitation spectrum of fluorescent powder is in 325~400nm, and main excitation peak is near 376nm, and emission spectrum is in 475~650nm, hair
It penetrates peak position and is located at 490nm, 546nm, 585nm, 625nm, main peak is near 546nm.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 0.04Tb fluorescent powder.Chromaticity coordinates is located at
Green wavelength (x=0.307, y=0.479) 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 0.1Tb accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Tb4O7, 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 Tb3+Adulterate three strontium yttrium borate green emitting phosphors.
Embodiment 5
By chemical formula Sr3Y0.85(BO3)3: the stoichiometric of 0.15Tb accurately weighs SrCO with electronic balance respectively3、
Y2O3、H3BO3、Tb4O7, 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 Tb3+Adulterate three strontium yttrium borate green emitting phosphors.
Claims (7)
1. a kind of terbium doped three strontium yttrium borates base green emitting phosphor, which is characterized in that the chemical general formula of the fluorescent powder is Sr3Y1-x
(BO3)3: xTb, wherein 0.01≤x≤0.15.
2. terbium doped three strontium yttrium borates base green emitting phosphor as described in claim 1, which is characterized in that the excitation of the fluorescent powder
Spectrum is in 325~400nm, and main excitation peak is near 376nm, and for emission spectrum in 475~650nm, main peak is attached in 546nm
Closely.
3. terbium doped three strontium yttrium borates base green emitting phosphor 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 terbium doped three strontium yttrium borates base green emitting phosphor, which comprises the following steps:
(1) according to the chemical structural formula Sr of fluorescent powder3Y1-x(BO3)3: the mol ratio amount of xTb, weigh respectively containing Sr, Y, B,
The compound of Tb 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 Tb3+Adulterate three strontium yttrium borate fluorescent powders
Sr3Y1-x(BO3)3: xTb, wherein 0.01≤x≤0.15.
5. the preparation method of terbium doped three strontium yttrium borates base green emitting phosphor as claimed in claim 4, which is characterized in that described
The compound containing Sr, Y, B, Tb element, respectively SrCO3、Y2O3、H3BO3、Tb4O7。
6. the preparation method of terbium doped three strontium yttrium borates base green emitting phosphor 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 terbium doped three strontium yttrium borates base green emitting phosphor 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811117731.9A CN109181695A (en) | 2018-09-21 | 2018-09-21 | Terbium doped three strontium yttrium borates base green emitting phosphor of one kind and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811117731.9A CN109181695A (en) | 2018-09-21 | 2018-09-21 | Terbium doped three strontium yttrium borates base green emitting phosphor of one kind and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109181695A true CN109181695A (en) | 2019-01-11 |
Family
ID=64909718
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811117731.9A Pending CN109181695A (en) | 2018-09-21 | 2018-09-21 | Terbium doped three strontium yttrium borates base green emitting phosphor of one kind and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109181695A (en) |
Citations (3)
| 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 |
-
2018
- 2018-09-21 CN CN201811117731.9A patent/CN109181695A/en active Pending
Patent Citations (3)
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Sun et al. | Simultaneously enhanced far-red luminescence and thermal stability in Ca3Al4ZnO10: Mn4+ phosphor via Mg2+ doping for plant growth lighting | |
| Yu et al. | A new eulytite-type Pb3Bi (PO4) 3: Eu3+ red-emitting phosphor: synthesis, structure and photoluminescence characteristics | |
| CN111057545A (en) | Bismuth-doped gallate blue fluorescent powder and preparation method thereof | |
| Tian et al. | A new oxyapatite red phosphor Eu3+-doped Ca3Y7 (BO4)(SiO4) 5O: synthesis, structure and luminescence properties | |
| CN108690612A (en) | It is a kind of to adulterate orange red fluorescent powder and preparation method thereof by the europium of matrix of niobates | |
| CN108949175A (en) | A kind of three strontium yttrium borate base blue colour fluorescent powder of cerium dopping and preparation method thereof | |
| Jiao et al. | Color tunable Ba3Lu (PO4) 3: Tb3+, Mn2+ phosphor via Tb3+→ Mn2+ energy transfer for white LEDs | |
| CN107353900B (en) | A kind of niobates fluorescent powder, preparation method and light emitting diode | |
| CN109337685A (en) | A kind of three strontium yttrium borate base green emitting phosphor of Er ions and preparation method thereof | |
| CN109021976A (en) | Three strontium yttrium borate base red fluorescent powders of a kind of europium doping and preparation method thereof | |
| CN109021975A (en) | A kind of three strontium yttrium borate base red fluorescent powder of praseodymium doped and preparation method thereof | |
| CN109181694A (en) | Three strontium yttrium borate base blue colour fluorescent powders of a kind of divalent europium doping and preparation method thereof | |
| CN105623660B (en) | The warm white fluorescent material that a kind of ultraviolet LED excites | |
| CN104059640B (en) | A kind of borate fluorescent powder substrate and the preparation method of fluorescent material | |
| CN104830335B (en) | A kind of borate base fluorescent powder of europium doping and preparation method thereof | |
| CN107338050A (en) | Rare earth samarium activation molybdate base red fluorescent powder and preparation method thereof | |
| Hua et al. | Synthesis and emission enhancement of intrinsic green-emitting materials for versatile applications | |
| CN108690613A (en) | It is a kind of using niobates as samarium doping orange red fluorescent powder of matrix and preparation method thereof | |
| CN106833643B (en) | A kind of green emitting phosphor and preparation method thereof of ultraviolet/near ultraviolet excitation | |
| CN109054833A (en) | A kind of three strontium yttrium borate base Chinese red fluorescent powder of samarium doping and preparation method thereof | |
| CN108753293A (en) | It is a kind of using niobates as white fluorescent powder of matrix and preparation method thereof | |
| CN107033899A (en) | A kind of boric acid lanthanum-strontium base red light fluorescent powder of samarium doping three and preparation method thereof | |
| CN109181695A (en) | Terbium doped three strontium yttrium borates base green emitting phosphor of one kind and preparation method thereof | |
| CN104327852B (en) | Silicon/germinate phosphor, preparation method and application thereof | |
| Perumal et al. | Synthesis, photoluminescence properties of Sr 1.95 Ba 0.05 CeO 4: Eu 3+ for LED applications |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190111 |