CN105087006A - Samarium and europium-codoped yttrium barium phosphate fluorescent powder and preparation method thereof - Google Patents
Samarium and europium-codoped yttrium barium phosphate fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses samarium and europium-codoped yttrium barium phosphate fluorescent powder and a preparation method thereof. The chemical formula of the fluorescent powder is Ba3Y(1-x-y)SmxEuy(PO4)3, wherein the x is 0.001-0.2; the y is 0.001-0.2. The red fluorescent powder obtained through using Sm<3+> and Eu<3+> to replace Y<3+> is high in crystallization degree and luminous intensity and good in color rendering, can be effectively stimulated by purple light or ultraviolet light to emit red fluorescence with the main wavelengths of 598 nm and 610 nm, and is red fluorescent powder capable of being used for white-light LEDs or energy-saving lamps. According to the invention, the operation is easy, the production cost and equipment requirement are low, the obtained product is stable in quality, and industrial production is facilitated.
Description
Technical field
The present invention relates to ultraviolet-purple light type White-light LED illumination and display fluorescent material field, yttrium phosphate barium fluorescent material that a kind of samarium is europium-doped specifically and preparation method thereof.
Background technology
White light emitting diode (LED) is called as forth generation lighting source, as the solid light source of a new generation, except the shortcomings such as the energy consumption that traditional incandescent light and luminescent lamp exist is high, frangible except overcoming, pollution, also have that volume is little, environmental protection, speed of response is fast, the life-span is long, can planar package, luminous intensity high, efficient, energy-conservation, vibration resistance, low voltage drive and environmental pollution etc. can not be caused to have advantage.Particularly in recent years, along with developing rapidly of blueness, purple and ultraviolet LED, make white light LEDs have very large application prospect at lighting field, be acknowledged as the green illumination light source substituting luminescent lamp and incandescent light at present.
Realize white light LEDs and mainly contain three kinds of approach: one is that red, green, blue three kinds of LED combination are produced white light.But want this method complex circuit designs, cost is higher.The second realizes Single chip white light by quantum effect, but cost is higher, and technology is also immature.The third cooperatively interacts with each coloured light that the LED of blue light, purple light or UV-light excites different colours fluorescent material to send to realize white light.This method is simple, cost is lower.Reported first in 1996 coordinates YAG:Dy with blue-ray LED
3+yellow emitting phosphor realizes white light LEDs, and in development subsequently, luminous efficiency has exceeded 100lm/W.But the emissive porwer that YAG fluorescent powder is positioned at red light region is very weak, there is the phenomenon that ruddiness lacks after causing same blue-light LED chip to mix, thus affect correlated(color)temperature and the colour rendering index of white light LEDs.These deficiencies of fluorescent material have become the bottleneck improving white light LEDs development, the performance of fluorescent material determines the technical indicator such as luminous efficiency, colour temperature, colour rendering index of white light LEDs, and therefore exploitation can be become the focus of current research and urgent task by the red fluorescent powder for white radiation LED of purple light or near ultraviolet excitation.
In addition, the luminous efficiency of fluorescent material except with its chemical composition and structure mutually outside the Pass, different preparation methods causes fluorescent material to have different performances, thus can produce significantly impact to the luminescent properties of fluorescent material.Such as, the fluorescent material of phosphate system often adopts high temperature solid phase synthesis to synthesize, its temperature of reaction is high, preparation time long, require higher to experimental installation, easily agglomeration is produced owing at high temperature reacting, the particle size obtained is large, need ball milling, luminosity and the performance of fluorescent material can be had a strong impact on.And sol-gel method preparation process is difficult to realize for phosphate fluorescent.Therefore, the suitable method preparing fluorescent material is selected also to be urgent problem in the art.
Summary of the invention
For solving existing YAG:Dy
3+yellow emitting phosphor realizes that white light technology red color components is not enough, colour rendering index and colour temperature is not enough and high temperature solid-state method is easily reunited, easily affect the shortcoming of luminous efficiency after particle ball mill crushing, the invention provides europium-doped yttrium phosphate barium fluorescent material of a kind of samarium and preparation method thereof, this fluorescent material is by UV-light or near ultraviolet excitation, luminous efficiency is high, the simple and environmental protection of preparation method.
The present invention for solving the problems of the technologies described above adopted technical scheme is: the yttrium phosphate barium fluorescent material that a kind of samarium is europium-doped, and the chemical formula of this fluorescent material is: Ba
3y
(1-x-y)sm
xeu
y(PO
4)
3, in formula, x gets 0.001 ~ 0.2, y and gets 0.001 ~ 0.2.
The preparation method of the yttrium phosphate barium fluorescent material that above-mentioned samarium is europium-doped, comprises the following steps:
1) barium source, yttrium source, samarium source, europium source and phosphorus source is taken according to above-mentioned stoichiometric ratio, and with deionized water, phosphorus source is dissolved completely, be prepared into phosphorus source solution, and in the solution of phosphorus source, phosphate radical or equivalent phosphate concentration be 0.05mol/l to saturation concentration, for subsequent use;
Saturation concentration refers to that maxima solubility is in deionized water dissolved in phosphorus source under normal temperature;
2) get nitrosonitric acid, add deionized water wherein and regulate its concentration to be 15 ~ 20mol/l, obtained reaction system, for subsequent use;
Wherein, the amount of nitric acid will ensure that it can dissolving step 1 completely) in weigh barium source, yttrium source, samarium source and europium source;
3) to step 2) in add the load weighted barium source of step 1) in obtained reaction system, add the load weighted yttrium source of step 1) until completely dissolved, the load weighted samarium source of step 1) is added again after yttrium source is dissolved completely, the load weighted europium source of step 1) is added again after samarium source is dissolved completely, finally dripping ammoniacal liquor adjust ph is 1 ~ 2, in the process, keeps the temperature of reaction system to remain on 85 ~ 90 DEG C while stirring by heating, finally obtain transparent settled solution, for subsequent use;
4) the phosphorus source solution that step 1) prepares is added in the transparent settled solution obtained in step 3), drip ammoniacal liquor after abundant stirring, to make it, precipitin reaction occurs, temperature of reaction system is kept to be 85 ~ 90 DEG C, pH >=8.0, and constantly stir, until precipitation capacity no longer increases, then filter and obtain white precipitate, white precipitate is dried and namely obtains precursors, for subsequent use;
5) precursors step 4) obtained in air atmosphere, be heated to 1000 ~ 1350 DEG C with the temperature rise rate of 4 ~ 15 DEG C/min, and sinter 2 ~ 8h at this temperature, pulverize after naturally cooling, and use deionized water ultrasonic cleaning, namely obtain product after drying.
Described barium source is one or more mixing in barium carbonate, nitrate of baryta, barium sulfate, bariumchloride.
Described yttrium source is one or more mixing in yttrium oxide, yttrium carbonate, Yttrium trinitrate.
Described samarium source is one or more mixing of Samarium trioxide, samaric nitrate, samarium trichloride.
Described europium source is one or more mixing in europium sesquioxide, europium nitrate, Europium trichloride.
Described phosphorus source is one or more mixing in Secondary ammonium phosphate, primary ammonium phosphate, ammonium phosphate.
Beneficial effect: the present invention compared with prior art, has the following advantages:
1) the yttrium phosphate barium red fluorescence powder of the samarium ion prepared of the present invention and europium ion codoped effectively can be excited by purple light or UV-light, and main exciting light is 360 ± 1nm, 374 ± 1nm, 393 ± 1nm, 402 ± 1nm, 462 ± 1nm;
2) the transmitting peak wavelength of the yttrium phosphate barium red fluorescence powder of the samarium ion prepared of the present invention and europium ion codoped is the ruddiness of 598nm and 610nm, and luminous efficiency is high, and luminous intensity is large, and colourity is pure;
3) the present invention utilizes solution preparation, reaction is mixed under ionic condition, stoichiometric temperature and the pH value simultaneously controlling reaction system of accurate control, thus make it can be able to synthesize under lower sintering temperature, obtain the red fluorescence powder that crystal property is good, emissive porwer is higher, and short texture, particle is tiny, be evenly distributed, there is good coating property;
4) the yttrium phosphate barium red fluorescence powder abundant raw material source of the samarium ion prepared of the present invention and europium ion codoped, cheap, and preparation technology is simple, easy handling, requirement for equipment is low, and final product quality is stablized and good process repeatability, suitability for scale production; ;
5) the yttrium phosphate barium red fluorescence powder of the samarium ion prepared of the present invention and europium ion codoped has good thermostability, compared with other sulfide, halogenide, borate, high temperature resistant, and humidity is environmentally friendly.
Accompanying drawing explanation
The X-ray powder diffraction pattern of Fig. 1 sample obtained by embodiment 3;
The abosrption spectrogram of Fig. 2 sample obtained by embodiment 3;
Fig. 3 is the luminescent spectrum figure of sample under 374nm wavelength excites obtained by embodiment 3.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, barium source used in various embodiments of the present invention is one or more mixing in barium carbonate, nitrate of baryta, barium sulfate, bariumchloride, yttrium source is one or more mixing in yttrium oxide, yttrium carbonate, Yttrium trinitrate, samarium source is one or more mixing of Samarium trioxide, samaric nitrate, samarium trichloride, europium source is one or more mixing in europium sesquioxide, europium nitrate, Europium trichloride, and phosphorus source is one or more mixing in Secondary ammonium phosphate, primary ammonium phosphate, ammonium phosphate.
Embodiment 1
The yttrium phosphate barium fluorescent material that samarium is europium-doped, the chemical formula of this fluorescent material is: Ba
3y
0.799sm
0.2eu
0.001(PO
4)
3.
The preparation method of the yttrium phosphate barium fluorescent material that above-mentioned samarium is europium-doped, comprises the following steps:
1) take barium source, yttrium source, samarium source, europium source and phosphorus source according to above-mentioned stoichiometric ratio, and with deionized water, phosphorus source is dissolved completely, be prepared into phosphorus source solution, and in the solution of phosphorus source, phosphate radical or equivalent phosphate concentration are 0.05mol/l, for subsequent use;
2) get nitrosonitric acid, add deionized water wherein and regulate its concentration to be 15mol/l, obtained reaction system, for subsequent use;
Wherein, the amount of nitric acid will ensure that it can dissolving step 1 completely) in weigh barium source, yttrium source, samarium source and europium source;
3) to step 2) in add the load weighted barium source of step 1) in obtained reaction system, add the load weighted yttrium source of step 1) until completely dissolved, the load weighted samarium source of step 1) is added again after yttrium source is dissolved completely, after samarium source is dissolved completely, add the load weighted europium source of step 1) again, finally dripping ammoniacal liquor adjust ph is 1, in the process, in the process, keep the temperature of reaction system to remain on 85 ~ 90 DEG C by heating while stirring, finally obtain transparent settled solution, for subsequent use;
4) the phosphorus source solution that step 1) prepares is added in the transparent settled solution obtained in step 3), drip ammoniacal liquor after abundant stirring, to make it, precipitin reaction occurs, temperature of reaction system is kept to be 85 ~ 90 DEG C, pH is 8.0, and constantly stir, until precipitation capacity no longer increases, then filter and obtain white precipitate, white precipitate is dried and namely obtains precursors, for subsequent use;
5) precursors step 4) obtained in air atmosphere, is heated to 1000 DEG C with the temperature rise rate of 4 DEG C/min, and sinters 8h at this temperature, pulverize after naturally cooling, and uses deionized water ultrasonic cleaning, namely obtains product after drying.
Embodiment 2
The yttrium phosphate barium fluorescent material that samarium is europium-doped, the chemical formula of this fluorescent material is: Ba
3y
0.799sm
0.001eu
0.2(PO
4)
3.
The preparation method of the yttrium phosphate barium fluorescent material that above-mentioned samarium is europium-doped, comprises the following steps:
1) take barium source, yttrium source, samarium source, europium source and phosphorus source according to above-mentioned stoichiometric ratio, and with deionized water, phosphorus source is dissolved completely, be prepared into phosphorus source solution (phosphate radical or equivalent phosphate concentration are 0.05mol/l ~ saturated), for subsequent use;
2) get nitrosonitric acid, add deionized water wherein and regulate its concentration to be 20mol/l, obtained reaction system, for subsequent use;
Wherein, the amount of nitric acid will ensure that it can dissolving step 1 completely) in weigh barium source, yttrium source, samarium source and europium source;
3) to step 2) in add the load weighted barium source of step 1) in obtained reaction system, add the load weighted yttrium source of step 1) until completely dissolved, the load weighted samarium source of step 1) is added again after yttrium source is dissolved completely, after samarium source is dissolved completely, add the load weighted europium source of step 1) again, finally dripping ammoniacal liquor adjust ph is 2.0, in the process, in the process, keep the temperature of reaction system to remain on 85 ~ 90 DEG C by heating while stirring, finally obtain transparent settled solution, for subsequent use;
4) the phosphorus source solution that step 1) prepares is added in the transparent settled solution obtained in step 3), drip ammoniacal liquor after abundant stirring, to make it, precipitin reaction occurs, temperature of reaction system is kept to be 85 ~ 90 DEG C, pH is 9.0, and constantly stir, until precipitation capacity no longer increases, then filter and obtain white precipitate, white precipitate is dried and namely obtains precursors, for subsequent use;
5) precursors step 4) obtained in air atmosphere, is heated to 1350 DEG C with the temperature rise rate of 15 DEG C/min, and sinters 2 at this temperature, pulverize after naturally cooling, and uses deionized water ultrasonic cleaning, namely obtains product after drying.
Embodiment 3
The yttrium phosphate barium fluorescent material that samarium is europium-doped, the chemical formula of this fluorescent material is: Ba
3y
0.88sm
0.06eu
0.06(PO
4)
3.
The preparation method of the yttrium phosphate barium fluorescent material that above-mentioned samarium is europium-doped, comprises the following steps:
1) take barium source, yttrium source, samarium source, europium source and phosphorus source according to stoichiometric ratio according to claim 1, and with deionized water, phosphorus source is dissolved completely, be prepared into phosphorus source solution (phosphate radical or equivalent phosphate concentration are 0.05mol/l ~ saturated), for subsequent use;
2) get nitrosonitric acid, add deionized water wherein and regulate its concentration to be 18mol/l, obtained reaction system, for subsequent use;
Wherein, the amount of nitric acid will ensure that it can dissolving step 1 completely) in weigh barium source, yttrium source, samarium source and europium source;
3) to step 2) in add the load weighted barium source of step 1) in obtained reaction system, add the load weighted yttrium source of step 1) until completely dissolved, the load weighted samarium source of step 1) is added again after yttrium source is dissolved completely, after samarium source is dissolved completely, add the load weighted europium source of step 1) again, finally dripping ammoniacal liquor adjust ph is 1, in the process, in the process, keep the temperature of reaction system to remain on 85 ~ 90 DEG C by heating while stirring, finally obtain transparent settled solution, for subsequent use;
4) the phosphorus source solution that step 1) prepares is added in the transparent settled solution obtained in step 3), drip ammoniacal liquor after abundant stirring, to make it, precipitin reaction occurs, temperature of reaction system is kept to be 85 ~ 90 DEG C, pH is 11.0, and constantly stir, until precipitation capacity no longer increases, then filter and obtain white precipitate, white precipitate is dried and namely obtains precursors, for subsequent use;
5) precursors step 4) obtained in air atmosphere, is heated to 1200 DEG C with the temperature rise rate of 10 DEG C/min, and sinters 6h at this temperature, pulverize after naturally cooling, and uses deionized water ultrasonic cleaning, namely obtains product after drying.
Embodiment 4
The yttrium phosphate barium fluorescent material that samarium is europium-doped, the chemical formula of this fluorescent material is: Ba
3y
0.8sm
0.1eu
0.1(PO
4)
3.
The preparation method of the yttrium phosphate barium fluorescent material that above-mentioned samarium is europium-doped, comprises the following steps:
1) take barium source, yttrium source, samarium source, europium source and phosphorus source according to stoichiometric ratio according to claim 1, and with deionized water, phosphorus source is dissolved completely, be prepared into phosphorus source solution (phosphate radical or equivalent phosphate concentration are 0.05mol/l ~ saturated), for subsequent use;
2) get nitrosonitric acid, add deionized water wherein and regulate its concentration to be 19mol/l, obtained reaction system, for subsequent use;
Wherein, the amount of nitric acid will ensure that it can dissolving step 1 completely) in weigh barium source, yttrium source, samarium source and europium source;
3) to step 2) in add the load weighted barium source of step 1) in obtained reaction system, add the load weighted yttrium source of step 1) until completely dissolved, the load weighted samarium source of step 1) is added again after yttrium source is dissolved completely, after samarium source is dissolved completely, add the load weighted europium source of step 1) again, finally dripping ammoniacal liquor adjust ph is 2, in the process, in the process, keep the temperature of reaction system to remain on 85 ~ 90 DEG C by heating while stirring, finally obtain transparent settled solution, for subsequent use;
4) the phosphorus source solution that step 1) prepares is added in the transparent settled solution obtained in step 3), drip ammoniacal liquor after abundant stirring, to make it, precipitin reaction occurs, temperature of reaction system is kept to be 85 ~ 90 DEG C, pH is 12.0, and constantly stir, until precipitation capacity no longer increases, then filter and obtain white precipitate, white precipitate is dried and namely obtains precursors, for subsequent use;
5) precursors step 4) obtained in air atmosphere, is heated to 1300 DEG C with the temperature rise rate of 9 DEG C/min, and sinters 4h at this temperature, pulverize after naturally cooling, and uses deionized water ultrasonic cleaning, namely obtains product after drying.
Claims (7)
1. the yttrium phosphate barium fluorescent material that samarium is europium-doped, is characterized in that: the chemical formula of this fluorescent material is: Ba
3y
(1-x-y)sm
xeu
y(PO
4)
3, in formula, x gets 0.001 ~ 0.2, y and gets 0.001 ~ 0.2.
2. the preparation method of the yttrium phosphate barium fluorescent material that a kind of samarium according to claim 1 is europium-doped, is characterized in that, comprise the following steps:
1) barium source, yttrium source, samarium source, europium source and phosphorus source is taken according to stoichiometric ratio according to claim 1, and with deionized water, phosphorus source is dissolved completely, be prepared into phosphorus source solution, and in the solution of phosphorus source, phosphate radical or equivalent phosphate concentration be 0.05mol/l to saturation concentration, for subsequent use;
2) get nitrosonitric acid, add deionized water wherein and regulate its concentration to be 15 ~ 20mol/l, obtained reaction system, for subsequent use;
Wherein, the amount of nitric acid will ensure that it can dissolving step 1 completely) in weigh barium source, yttrium source, samarium source and europium source;
3) to step 2) in add the load weighted barium source of step 1) in obtained reaction system, add the load weighted yttrium source of step 1) until completely dissolved, the load weighted samarium source of step 1) is added again after yttrium source is dissolved completely, the load weighted europium source of step 1) is added again after samarium source is dissolved completely, finally dripping ammoniacal liquor adjust ph is 1 ~ 2, in the process, keeps the temperature of reaction system to remain on 85 ~ 90 DEG C while stirring by heating, finally obtain transparent settled solution, for subsequent use;
4) the phosphorus source solution that step 1) prepares is added in the transparent settled solution obtained in step 3), drip ammoniacal liquor after abundant stirring, to make it, precipitin reaction occurs, temperature of reaction system is kept to be 85 ~ 90 DEG C, pH >=8.0, and constantly stir, until precipitation capacity no longer increases, then filter and obtain white precipitate, white precipitate is dried and namely obtains precursors, for subsequent use;
5) precursors step 4) obtained in air atmosphere, be heated to 1000 ~ 1350 DEG C with the temperature rise rate of 4 ~ 15 DEG C/min, and sinter 2 ~ 8h at this temperature, pulverize after naturally cooling, and use deionized water ultrasonic cleaning, namely obtain product after drying.
3. the preparation method of the yttrium phosphate barium fluorescent material that a kind of samarium according to claim 2 is europium-doped, is characterized in that: described barium source is one or more mixing in barium carbonate, nitrate of baryta, barium sulfate, bariumchloride.
4. the preparation method of the yttrium phosphate barium fluorescent material that a kind of samarium according to claim 2 is europium-doped, is characterized in that: described yttrium source is one or more mixing in yttrium oxide, yttrium carbonate, Yttrium trinitrate.
5. the preparation method of the yttrium phosphate barium fluorescent material that a kind of samarium according to claim 2 is europium-doped, is characterized in that: described samarium source is one or more mixing of Samarium trioxide, samaric nitrate, samarium trichloride.
6. the preparation method of the yttrium phosphate barium fluorescent material that a kind of samarium according to claim 2 is europium-doped, is characterized in that: described europium source is one or more mixing in europium sesquioxide, europium nitrate, Europium trichloride.
7. the preparation method of the yttrium phosphate barium fluorescent material that a kind of samarium according to claim 2 is europium-doped, is characterized in that: described phosphorus source is one or more mixing in Secondary ammonium phosphate, primary ammonium phosphate, ammonium phosphate.
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| CN104629762A (en) * | 2015-02-05 | 2015-05-20 | 洛阳理工学院 | Europium-ion/manganese-ion-codoped barium yttrium phosphate red fluorescent powder and preparation method thereof |
-
2015
- 2015-09-06 CN CN201510556401.XA patent/CN105087006A/en active Pending
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| CN101824322A (en) * | 2009-03-05 | 2010-09-08 | 建兴电子科技股份有限公司 | Fluorescent material and fluorescent lamp applying the same |
| CN102115671A (en) * | 2010-01-04 | 2011-07-06 | 海洋王照明科技股份有限公司 | Phosphate-base red luminescent material and preparation method thereof |
| CN102604638A (en) * | 2012-01-19 | 2012-07-25 | 苏州大学 | Eu<3+>-activated phosphate red phosphor powder as well as preparation method and application thereof |
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Application publication date: 20151125 |