CN108753293A - It is a kind of using niobates as white fluorescent powder of matrix and preparation method thereof - Google Patents
It is a kind of using niobates as white fluorescent powder of matrix and preparation method thereof Download PDFInfo
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- CN108753293A CN108753293A CN201810692490.4A CN201810692490A CN108753293A CN 108753293 A CN108753293 A CN 108753293A CN 201810692490 A CN201810692490 A CN 201810692490A CN 108753293 A CN108753293 A CN 108753293A
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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 using niobates as white fluorescent powder of matrix and preparation method thereof, and the chemical general formula of the fluorescent powder is Ba2LaNbO6:XDy, wherein 0≤x≤0.2, it can effectively be excited by near ultraviolet or blue light, send out the high white light of excitation purity, the present invention is a kind of to be prepared by the preparation method of the white fluorescent powder of matrix of niobates based on solid-phase synthesis, strong operability, preparation process is simple, production cost is low, it prepares in air atmosphere, temperature-rise period is simple, preparation method is simple, favorable reproducibility, short preparation period, the thermal stability and chemical stability of gained matrix are high, it is a kind of good luminous host material, stablize by the white emitting fluorescent powder chemical property of single-matrix of titanate, good luminous performance, luminous intensity is high, colour rendering is good, and preferable light intensity and colour rendering are still kept at relatively high temperatures, the application requirement in White-light LED illumination field can be met.
Description
Technical field
The invention belongs to LED fluorescent powder technical fields, are related to a kind of using niobates as the white fluorescent powder of matrix and its system
Preparation Method.
Background technology
Light emitting diode (Light Emitting Diode, LED) is acknowledged as the new light sources of 21st century, has
Energy saving, fast, the environmentally protective, long lifespan of response, it is small, luminous efficiency is high many advantages, such as, have in illumination and display field
Huge application prospect.
Currently, there are mainly three types of the forms of acquisition white light for illumination LED：First, red-green-blue LED chip is pressed one
Certainty ratio assembled package generates white light；Second, YAG fluorescent powder is coated on blue-light LED chip, chip sends out blue light excitation fluorescence
Powder generates yellow light, yellow light and remaining blue light, forms white light；Third coats three base of RGB near ultraviolet LED chip
Color fluorescent powder forms blue and green light near ultraviolet excitation blue, green, red fluorescence powder, feux rouges combines and generates white light.
The red fluorescence powder of business is mainly Y at present2O2S:Dy3+, however red fluorescence powder Y2O2S:Dy3+Its luminous intensity is about
Blue colour fluorescent powder BaMgAll0O17:Dy2+With green emitting phosphor ZnS:(Cu+, A13+) 1/8th, luminous efficiency is very low,
And red fluorescence powder Y2O2S:Dy3+It is harmful to decompose the gas generated.Therefore develop can directly by black light and
The white fluorescent powder that blue light effectively excites has actual application value.
Invention content
The object of the present invention is to provide a kind of using niobates as white fluorescent powder of matrix and preparation method thereof, solves existing
There is the problem that light-emitting phosphor efficiency is low present in technology.
The technical solution adopted in the present invention is that a kind of using niobates as the white fluorescent powder of matrix, chemical general formula is
Ba2LaNbO6:XDy, wherein 0≤x≤0.2.
The present invention is a kind of using niobates as the white fluorescent powder of matrix, and feature also resides in：
For the excitation spectrum of the white fluorescent powder in 325nm~450nm, emission peak is 475nm~650nm.
The present invention is a kind of using niobates as the preparation method of the white fluorescent powder of matrix, is specifically implemented according to the following steps：
Step 1, according to white fluorescent powder chemical general formula Ba2LaNbO6:The mol ratio amount of xDy, wherein 0≤x≤0.2,
The raw materials of compound containing Ba, La, Nb and Dy element is weighed respectively；
Step 2, it after the raw material that step 1 weighs being sufficiently mixed, is ground, obtains raw mixture；
Step 3, the raw mixture that step 2 obtains is placed under air atmosphere, be constantly warming up to temperature be 1350~
1500 DEG C, carry out high-temperature calcination；
Step 4, the raw material after step 3 being calcined takes out after being cooled to room temperature, and grinds to get using niobates as matrix
White fluorescent powder Ba2LaNbO6∶xDy。
The present invention is a kind of using niobates as the preparation method of the white fluorescent powder of matrix, it is further characterized in that,
Compound containing Ba, La, Nb and Dy element in step 1, respectively its carbonate or oxide.
Compound containing Ba, La, Nb, Dy element in step 1, respectively BaCO3、 La2O3、Nb2O5、Dy2O3。
In step 3, be with the heating rate of 5~10 DEG C/min,
In step 3, the time of calcining is 6~8 hours.
Beneficial effects of the present invention are, a kind of using niobates as the white fluorescent powder of matrix, by adulterating active ions Dy3 +, can be obtained under near ultraviolet and blue light excitation main peak be located near 494nm and 584nm luminous intensity compared with by force, excitation purity it is higher
White light.The CIE chromaticity coordinates of the white fluorescent powder fits like a glove with NTSC standard chromaticity coordinates, near ultraviolet chip and blue chip
Light emitting diode matches, and can be used as white light LEDs white fluorescent powder；
It is provided by the invention using niobates as the preparation method of the white fluorescent powder of matrix, preparation method be based on solid phase
Synthetic method is come what is prepared, and strong operability, calcination temperature is low, prepares in air atmosphere, and temperature-rise period is simple, and preparation method is simple
It is easy, favorable reproducibility, short preparation period.
Description of the drawings
Fig. 1 is Ba2LaNbO6The X ray diffracting spectrum and Ba of matrix2LaNbO6Standard card (PDF#37-0856) compares
Figure；
Fig. 2 is Ba2LaNbO6:The excitation spectrum and launching light spectrogram of 0.04Dy white fluorescent powders；
Fig. 3 is Ba2LaNbO6:The CIE chromaticity coordinates figures of 0.04Dy white fluorescent powders.
Specific implementation mode
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
It is provided by the invention a kind of using niobates as the white fluorescent powder of matrix, chemical general formula Ba2LaNbO6:XDy,
Wherein 0≤x≤0.2.
For the excitation spectrum of the white fluorescent powder in 325nm~450nm, emission peak is 475nm~650nm.
The present invention is a kind of using niobates as the preparation method of the white fluorescent powder of matrix, is specifically implemented according to the following steps：
Step 1, according to white fluorescent powder chemical general formula Ba2LaNbO6:The mol ratio amount of xDy, wherein 0≤x≤0.2,
The raw materials of compound containing Ba, La, Nb and Dy element is weighed respectively；
Step 2, it after the raw material that step 1 weighs being sufficiently mixed, is ground, obtains raw mixture；
Step 3, the raw mixture that step 2 obtains is placed under air atmosphere, be constantly warming up to temperature be 1350~
1500 DEG C, carry out high-temperature calcination；
Step 4, the raw material after step 3 being calcined takes out after being cooled to room temperature, and grinds to get using niobates as matrix
White fluorescent powder Ba2LaNbO6∶xDy。
Compound containing Ba, La, Nb and Dy element in step 1, respectively its carbonate or oxide.
Compound containing Ba, La, Nb, Dy element in step 1, respectively BaCO3、 La2O3、Nb2O5、Dy2O3。
In step 3, be with the heating rate of 5~10 DEG C/min,
In step 3, the time of calcining is 6~8 hours.
A kind of obtained by the present invention is the excitation spectrum of the white fluorescent powder of matrix in 325nm~450nm using niobates
It is interior, two main excitation peaks near 353nm and 365nm, emission peak in 475nm~650nm, main peak substantially in 494nm and
Near 584nm；NbO in the chemical formula6 2-Nb-O keys in group have stronger covalent bonding effect, the oxygen in polyhedron from
Son by neighbouring high-valence state niobium polarization so that the Fluorescence quenching effect of rare earth activation ion reduces, to make activation from
The doping concentration of son improves.By adulterating active ions Dy3+, main peak can be obtained under near ultraviolet and blue light excitation and be located at 494nm
With luminous intensity near 584nm compared with strong, the higher white light of excitation purity；The fluorescent powder can by the effectively excitation of black light and blue light and
White light is sent out, white light LEDs are can be applied to.
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
According to chemical formula Ba2LaNbO6:The stoichiometric of 0Dy accurately weighs raw material respectively using electronic balance
Ba2CO3、La2O3、Nb2O5、Dy2O3, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.By above-mentioned raw materials
It is ground after mixing, is packed into corundum crucible, is placed in and is rapidly heated in resistance furnace, in air atmosphere with the liter of 10 DEG C/min
Warm rate rises to 1350 DEG C, keeps the temperature 6 hours, then furnace cooling waits for that sample is cooled to room temperature.It takes out sample and regrinds powder
It is broken to get to mix dysprosium using niobates as the white fluorescent powder Ba of matrix2LaNbO6。
Fig. 1 is Ba prepared by the present embodiment 12LaNbO6The X ray diffracting spectrum and Ba of white fluorescent powder2LaNbO6Standard
Card (PDF#37-0856) comparison diagram.It is seen that object phase purity is relatively high, better crystallinity degree.
Embodiment 2
According to chemical formula Ba2LaNbO6:The stoichiometric of 0.04Dy accurately weighs raw material respectively using electronic balance
Ba2CO3、La2O3、Nb2O5、Dy2O3, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.By above-mentioned raw materials
It is ground after mixing, is packed into corundum crucible, is placed in and is rapidly heated in resistance furnace, in air atmosphere with the liter of 10 DEG C/min
Warm rate rises to 1400 DEG C, keeps the temperature 6.5 hours, then furnace cooling waits for that sample is cooled to room temperature.It takes out sample and regrinds powder
It is broken to get to mix dysprosium using niobates as matrix white fluorescent powder Ba2LaNbO6:0.04Dy。
Fig. 1 is Ba2LaNbO6The X ray diffracting spectrum and Ba of matrix2LaNbO6Standard card (PDF#37-0856) compares
Figure.It is seen that object phase purity is relatively high, better crystallinity degree.
Fig. 2 is Ba prepared by the present embodiment 22LaNbO6:The excitation spectrum and emission spectrum of 0.04Dy white fluorescent powders.Two
A main emission peak is located near 494nm and 584nm, and two main excitation peaks are located at 353nm nearby and near 365nm.Thus
As it can be seen that the fluorescent powder can send out white light by black light and blue light effectively excitation, white light LEDs are can be applied to.
Fig. 3 is the Ba prepared by the present embodiment 22LaNbO6:The CIE chromaticity coordinates figures of 0.04Dy red fluorescence powders.It can from figure
Find out, the CIE chromaticity coordinates of the red fluorescence powder is (x=0.321, y=0.361), with NTSC standard chromaticity coordinates (x=0.330, y
=0.330) substantially close to therefore wherein can be used to directly emit white light.
Embodiment 3
By chemical formula Ba2LaNbO6:The stoichiometric of 0.1Dy accurately weighs raw material respectively using electronic balance
Ba2CO3、La2O3、Nb2O5、Dy2O3, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.By above-mentioned original
Material is ground after mixing, is packed into corundum crucible, is placed in and is rapidly heated in resistance furnace, in air atmosphere with 10 DEG C/min's
Heating rate rises to 1450 DEG C, keeps the temperature 7 hours, then furnace cooling waits for that sample is cooled to room temperature.It takes out sample and regrinds powder
It is broken to get to mix dysprosium using niobates as the white fluorescent powder Ba of matrix2LaNbO6:0.1Dy。
Embodiment 4
According to chemical formula Ba2LaNbO6:The stoichiometric of 0.1Dy accurately weighs raw material respectively using electronic balance
Ba2CO3、La2O3、Nb2O5、Dy2O3, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.By above-mentioned raw materials
It is ground after mixing, is packed into corundum crucible, is placed in and is rapidly heated in resistance furnace, in air atmosphere with the liter of 10 DEG C/min
Warm rate rises to 1480 DEG C, keeps the temperature 7.5 hours, then furnace cooling waits for that sample is cooled to room temperature.It takes out sample and regrinds powder
It is broken to get to the niobates white fluorescent powder Ba for mixing dysprosium2LaNbO6:0.1Dy。
Embodiment 5
According to chemical formula Ba2LaNbO6:The stoichiometric of 0.2Dy accurately weighs raw material respectively using electronic balance
Ba2CO3、La2O3、Nb2O5、Dy2O3, the purity of middle rare earth is 99.99%, remaining is that analysis is pure.By above-mentioned raw materials
It is ground after mixing, is packed into corundum crucible, is placed in and is rapidly heated in resistance furnace, in air atmosphere with the liter of 10 DEG C/min
Warm rate rises to 1500 DEG C, keeps the temperature 8 hours, then furnace cooling waits for that sample is cooled to room temperature.It takes out sample and regrinds powder
It is broken to get to the niobates white fluorescent powder Ba for mixing dysprosium2LaNbO6:0.2Dy。
It is provided by the invention using niobates as the preparation method of the white fluorescent powder of matrix, preparation method be based on solid phase
Synthetic method is come what is prepared, and strong operability, preparation process is simple, production cost is low, prepares in air atmosphere, temperature-rise period letter
Single, preparation method is simple, favorable reproducibility, short preparation period, and the thermal stability and chemical stability of gained matrix are high, are one
The good luminous host material of kind.Trivalent rare earth ions have abundant energy level, and the luminescent material of doping is in green illumination, life
The fields such as object fluorescence labelling, short wavelength laser, presentation of information and photoelectronics have broad application prospects, so this hair
It is bright be prepared using titanate as the white emitting fluorescent powder chemical property of single-matrix stable, good luminous performance, luminous intensity is high,
Colour rendering is good, and still keeps preferable light intensity and colour rendering at relatively high temperatures, can meet the application in White-light LED illumination field
It is required that.
Claims (7)
1. a kind of using niobates as the white fluorescent powder of matrix, which is characterized in that chemical general formula Ba2LaNbO6:XDy, wherein 0
≤x≤0.2。
2. as described in claim 1 using niobates as the white fluorescent powder of matrix, which is characterized in that the white fluorescent powder
For excitation spectrum in 325nm~450nm, emission peak is 475nm~650nm.
3. a kind of using niobates as the preparation method of the white fluorescent powder of matrix, which is characterized in that specifically real according to the following steps
It applies：
Step 1, according to white fluorescent powder chemical general formula Ba2LaNbO6:The mol ratio amount of xDy, wherein 0≤x≤0.2, claims respectively
Take the raw materials of compound containing Ba, La, Nb and Dy element；
Step 2, it after the raw material that step 1 weighs being sufficiently mixed, is ground, obtains raw mixture；
Step 3, the raw mixture that step 2 obtains is placed under air atmosphere, it is 1350~1500 DEG C to be constantly warming up to temperature,
Carry out high-temperature calcination；
Step 4, the raw material after step 3 being calcined takes out after being cooled to room temperature, and grinds to get using niobates as the white of matrix
Color fluorescent powder Ba2LaNbO6∶xDy。
4. according to claim 3 a kind of using niobates as the preparation method of the white fluorescent powder of matrix, which is characterized in that
Compound containing Ba, La, Nb and Dy element in step 1, respectively its carbonate or oxide.
5. as claimed in claim 4 using niobates as the preparation method of the white fluorescent powder of matrix, it is characterised in that described
Compound containing Ba, La, Nb, Dy element, respectively BaCO3、La2O3、Nb2O5、Dy2O3。
6. according to claim 5 a kind of using niobates as the preparation method of the white fluorescent powder of matrix, which is characterized in that
In step 3, heating rate is 10 DEG C/min.
7. according to claim 3 a kind of using niobates as the preparation method of the white fluorescent powder of matrix, which is characterized in that
In step 3, the time of calcining is 6~8 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116903366A (en) * | 2023-07-14 | 2023-10-20 | 昆明理工大学 | Preparation method of double perovskite doped silver ion photochromic ceramic powder |
| CN116948644A (en) * | 2023-07-25 | 2023-10-27 | 昆明理工大学 | Preparation method of rare earth ion doped photochromic fluorescent powder |
-
2018
- 2018-06-29 CN CN201810692490.4A patent/CN108753293A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116903366A (en) * | 2023-07-14 | 2023-10-20 | 昆明理工大学 | Preparation method of double perovskite doped silver ion photochromic ceramic powder |
| CN116948644A (en) * | 2023-07-25 | 2023-10-27 | 昆明理工大学 | Preparation method of rare earth ion doped photochromic fluorescent powder |
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Application publication date: 20181106 |