CN103773372A - Emission peak-adjustable phosphate fluorescent powder for white-light LED (Light-Emitting Diode) and preparation method thereof - Google Patents
Emission peak-adjustable phosphate fluorescent powder for white-light LED (Light-Emitting Diode) and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of rare-earth light-emitting materials, relates to emission peak-adjustable phosphate fluorescent powder for a white-light LED (Light-Emitting Diode) and a preparation method thereof. Fluorescent powder for the white-light LED, which is stable in chemical property, high in light-emitting performance, high in physical phase purity and adjustable in the emission peak from green light to red light when being excited by near ultraviolet light, purple light and blue light and can be applied to the white-light LED excited by using a blue-light LED chip. The chemical components of the fluorescent powder can be shown as a chemical formula, namely, Ca9(1-x-y)-La(PO4)7:xEu<2+>,yMn<2+>, wherein x is more than or equal to 0.002 and less than or equal to 0.2, and y is more than or equal 0.002 and less than or equal to 0.2. The fluorescent powder can be used for exciting white light together with blue fluorescent powder BaMgAl10O17:xEu<2+>. An encapsulated device can reach a white-light area with low color temperature, warm tone (CCT is less than or equal 5,000K), high color rendering index (CRI, RA is more than or equal to 90) and a color coordinate being up to CIE1931. The preparation method is simple and easy to operate, contributes to saving energy and time, and has extremely good application prospect in the field of solid illumination.
Description
Technical field
The present invention relates to adjustable phosphate phosphor of a kind of white light LEDs emission peak and preparation method thereof, it can be applicable to, in ultraviolet one near ultraviolet type white light LEDs, belong to fluorescent material technical field.
Background technology
White light emitting diode (LED) be called as the 4th generation lighting source, as solid light source of new generation, 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 can not cause environmental pollution etc. to have advantage, be therefore widely used in fields such as demonstration, background light source, signal lamp, illuminations.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 of current replace fluorescent lamps and incandescent light.
At present, the form of acquisition white light LEDs mainly contains two kinds: one is by three kinds of LED chip combination results white lights of red, green, blue; Another kind is to use UV-light, near-ultraviolet light or blue-light LED chip to add yellow fluorescent powder, and the two light sending is mixed to form white light, the blue-light excited YAG:Ce that wherein GaN base chip is launched
3+fluorescent material is with the fastest developing speed, has realized marketization application.This method is that application is also the most ripe at most at present, but shortcoming is fairly obvious, and major cause is the white light that blue chip and gold-tinted two primary colours are compounded to form, lack red composition, cause colour rendering index (CRI, RA=75) on the low side, high color temperature (CCT=7756K).YAG:Ce
3+fluorescent material emmission spectrum between 550nm-560nm, can not with the LED device of the blue chip positive white light of compound preparation (x=0.333, y=0.333) and low color warm tone (CCT≤5000K).In addition YAG:Ce
3+the peak width at half height of fluorescent material is narrower, generally, in 110nm left and right, causes device colour rendering index to be difficult to reach more than 80.Above shortcomings has hindered the development of white light LED part.Therefore develop a kind of white light LEDs use transmitted wave spectrum width, color developing that can effectively be excited by near ultraviolet-UV-light good, the fluorescent material of chromaticity coordinates cooperation blue-light LED chip preferably becomes the focus of current research and urgent task.
The advantages such as in addition, phosphoric acid salt is a kind of traditional phosphor host, and it has high stable performance, and the cheap and preparation technology of raw materials cost is simple, phosphate phosphor is one of fluorescent material of excellent property.Therefore, use phosphate radical is base starting material, development of new phosphate radical base fluorescent powder become the focus of domestic and international research.
Summary of the invention
The problem of technology to be solved by this invention is, a kind of ultraviolet excitation adjustable phosphate phosphor Ca from green to red emission is provided
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+, this fluorescent material coordinates blue colour fluorescent powder BaMgAl
10o
17: xEu
2+inspire white light, packaging can reach low color warm tone (CCT≤5000K), high color rendering index (CRI) (CRI, RA>=90), chromaticity coordinates and reach the white light field of CIE1931.
Further, another technical problem to be solved by this invention is that a kind of novel preparation method of above-mentioned phosphate phosphor is provided.The simple easy handling of the method, reaction times light-emitting phosphor intensity short and preparation is high, adjustable from green to red emission, stable chemical nature, and powder particle is evenly distributed, particle diameter is little etc.
The present invention gos deep into, at length research, by controlling the factors such as chemical constitution, proportioning raw materials, has solved above-mentioned technical problem.Concrete scheme is as follows:
Adjustable phosphate phosphor of emission peak and preparation method thereof for a kind of white light LEDs provided by the invention, its chemical composition can be by following chemical formulation: Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+, wherein 0.002≤x≤0.2,0.002≤y≤0.2, comprises the following steps:
1. according to chemical general formula Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+calculate respectively, take reaction reagent EuO, A.R.,, A.R. represents analytical pure, MnO, A.R., CaCO
3, purity is 99.9%, La
2o
3, purity is 99.99%, (NH
4)
2h (PO
4), purity is 99.99%; They are ground in mortar 2～3 hours, it is fully mixed.
2. said mixture is packed into crucible, compacting, and be placed in air High Temperature Furnaces Heating Apparatus, be warming up to 1200 ℃ and sintering 8 hours;
3. cooling rear taking-up its grinding is crushed to certain particle size, packs crucible into, then in reduction furnace, is warming up to 1000 ℃ of reduction 8 hours;
4. in reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, broken again, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain phosphate phosphor.
The preparation method of the adjustable phosphate phosphor of emission peak for described a kind of white light LEDs, is characterized in that: step takes (NH in 1.
4)
2h (PO
4) excessive 3～5% to make up the volatilization loss of calcination process.
The preparation method of the adjustable phosphate phosphor of emission peak for described a kind of white light LEDs, is characterized in that: the step speed that 2., 3. middle sintering temperature raises is 8～12 ℃/min.
The preparation method of the adjustable phosphate phosphor of emission peak for described a kind of white light LEDs, is characterized in that: step 3. middle reducing atmosphere is H
2/ N
2mixed gas (H
2volume content is 15%, N
2volume content is 85%).
The invention has the beneficial effects as follows:
Compared with prior art, technical scheme advantage of the present invention is:
1, the light-emitting phosphor performance that the present invention obtains is good, low color warm tone, and high color rendering index (CRI), thing phase purity is high.
2, the fluorescent powder excitation spectrum that the present invention obtains is wide, can effectively be excited by the blue chip of 370-470nm wave band.
3, the light-emitting phosphor peak wavelength that the present invention obtains is adjustable at 450-650nm, and spectrum covers green to yellow to red, can be adapted to the LED chip of different-waveband.
4, acquisition fluorescent material preparation method of the present invention, its step is simple, easy handling, production process contamination-free produces, and raw material is easy to get and is with low cost.
Accompanying drawing explanation
Fig. 1 Ca
9 (1-x)la (PO
4)
7: xEu
2+the fluorescent material sample different concns Eu that adulterates under supervisory wavelength 502nm
3+exciting light spectrogram.
Fig. 2 Ca
9 (1-x)la (PO
4)
7: xEu
2+fluorescent material sample excites lower doping different concns Eu at 365nm
3+exciting light spectrogram.
Fig. 3 Ca
9 (1-x)la (PO
4)
7: xEu
2+the luminescent spectrum of fluorescent material and Ca
9 (1-x)la (PO
4)
7: xMn
2+the overlapped spectra figure of the excitation spectrum of fluorescent material.
Fig. 4 Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+(x=0.005) fluorescent material excites lower doping different concns Mn at 365nm
2+luminescent spectrum figure.
Embodiment
Describe various preferred embodiment of the present invention below in detail.But the present invention is not limited to these concrete preferred embodiments.
According to the preferred embodiments of the invention, the present invention is the adjustable phosphate phosphor of emission peak for a kind of white light LEDs, and its chemical composition can be by following chemical formulation: Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+, wherein 0.002≤x≤0.02,0.002≤y≤0.02.Further, Ca
9 (1-x)la (PO
4)
7: xEu
2+, rare-earth metal doped Eu
3+amount x can be 0.001,0.003,0.005,0.01,0.05, be finally preferably x=0.005.Again further, Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+(x=0.005), alkali doped Mn
2+amount y can be 0.000,0.01,0.015,0.03,0.05,0.07,0.10, described transmitting is adjustable, and phosphate phosphor consists of Ca
8.955la (PO
4)
7: 0.005Eu
2+, Ca
8.865la (PO
4)
7: 0.005Eu
2+, 0.01Mn
2+, Ca
8.82la (PO
4)
7: 0.005Eu
2+, 0.015Mn
2+, Ca
8.685la (PO
4)
7: 0.005Eu
2+, 0.03Mn
2+, Ca
8.505la (PO
4)
7: 0.005Eu
2+, 0.05Mn
2+, Ca
8.325la (PO
4)
7: 0.005Eu
2+, 0.07Mn
2+, Ca
8.055la (PO
4)
7: 0.005Eu
2+, 0.1Mn
2+.
Specific embodiment of the invention scheme is described below with reference to accompanying drawings.It is evident that for the person of ordinary skill of the art: in the situation that not deviating from the spirit and scope of the invention, can therefrom carry out various modifications and variations.Thereby improvement of the present invention and the variation within the scope in claims and equivalent thereof contained in the present invention.
Embodiment 1:Ca
8.991la (PO
4)
7: 0.001Eu
2+preparation
First, by chemical formula Ca
9 (1-x)la (PO
4)
7: xEu
2+stoichiometric ratio take reaction raw materials EuO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.001: 8.991: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Embodiment 2:Ca
8.973la (PO
4)
7: 0.003Eu
2+preparation
First, by chemical formula Ca
9 (1-x)la (PO
4)
7: xEu
2+stoichiometric ratio take reaction raw materials EuO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.003: 8.973: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Embodiment 3:Ca
8.955la (PO
4)
7: 0.005Eu
2+preparation
First, by chemical formula Ca
9 (1-x)la (PO
4)
7: xEu
2+stoichiometric ratio take reaction raw materials EuO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.005: 8.955: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Embodiment 4:Ca
8.91la (PO
4)
7: 0.01Eu
2+preparation
First, by chemical formula Ca
9 (1-x)la (PO
4)
7: xEu
2+stoichiometric ratio take reaction raw materials EuO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.01: 8.91: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Embodiment 5:Ca
8.55la (PO
4)
7: 0.05Eu
2+preparation
First, by chemical formula Ca
9 (1-x)la (PO
4)
7: xEu
2+stoichiometric ratio take reaction raw materials EuO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.05: 8.55: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Referring to accompanying drawing 1, it is Ca
9 (1-x)la (PO
4)
7: xEu
2+fluorescent material sample is the ultraviolet that obtains of 502nm and the exciting light spectrogram of near ultraviolet region at monitoring wavelength.
Referring to accompanying drawing 2, it is the divalent europium Eu of the different concns of embodiment 1,2,3,4 and 5 preparations
2+at Ca
9 (1-x)la (PO
4)
7: xEu
2+in fluorescent material, excite with UV-light 365nm the luminescent spectrum figure obtaining.In Fig. 2, curve (1), (2), (3), (4), (5) are respectively the spectral radiation curves of the fluorescent material sample prepared by embodiment 1,2,3,4 and 5 technical schemes, as seen from Figure 2, along with the energy of europium ion concentration is large, the luminous intensity of fluorescent material strengthens gradually, works as x=0.005, it is the strongest that luminous intensity reaches substantially, the concentration that continues to increase europium ion, luminous intensity reduces, and this is the result of concentration quenching
Embodiment 6:Ca
8.865la (PO
4)
7: 0.005Eu
2+, 0.01Mn
2+preparation
First, by chemical formula Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+stoichiometric ratio take reaction raw materials EuO, MnO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.005: 0.01: 8.865: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Embodiment 7:Ca
8.82la (PO
4)
7: 0.005Eu
2+, 0.015Mn
2+preparation
First, by chemical formula Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+stoichiometric ratio take reaction raw materials EuO, MnO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.005: 0.015: 8.82: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Embodiment 8:Ca
8.685la (PO
4)
7: 0.005Eu
2+, 0.03Mn
2+preparation
First, by chemical formula C Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+stoichiometric ratio take reaction raw materials EuO, MnO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.005: 0.03: 8.685: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Embodiment 9:Ca
8.505la (PO
4)
7: 0.005Eu
2+, 0.05Mn
2+preparation
First, by chemical formula Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+stoichiometric ratio take reaction raw materials EuO, MnO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.005: 0.05: 8.505: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Embodiment 10:Ca
8.325la (PO
4)
7: 0.005Eu
2+, 0.07Mn
2+preparation
First, by chemical formula Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+stoichiometric ratio take reaction raw materials EuO, MnO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.005: 0.07: 8.325: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Embodiment 11:Ca
8.055la (PO
4)
7: 0.005Eu
2+, 0.1Mn
2+preparation
First, by chemical formula Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+stoichiometric ratio take reaction raw materials EuO, MnO, CaCO
3, La
2o
3, (NH
4)
2h (PO
4) mol ratio be 0.005: 0.1: 8.055: 0.5: 7; They are ground 2～3 hours in mortar, it is fully mixed.Then pack crucible, compacting into, and be placed in air High Temperature Furnaces Heating Apparatus, 1200 ℃ of sintering 8 hours; Cooling rear taking-up is also crushed to certain particle size by its grinding, packs crucible into, then under reduction furnace 1000 ℃ reduction 8 hours; In reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, in fragmentation, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain described phosphate phosphor.
Referring to accompanying drawing 3, Ca
9 (1-x)la (PO
4)
7: xEu
2+the luminescent spectrum of fluorescent material and Ca
9 (1-x)la (PO
4)
7: xMn
2+the overlapped spectra figure of the excitation spectrum of fluorescent material, Ca
9 (1-x)la (PO
4)
7: xMn
2+the excitation peak of the excitation spectrum of fluorescent material is mainly positioned at 267nm, 343nm, 370nm, 405nm, 417nm and 454nm, near wavelength is 454nm, produces spectra overlapping, and the present invention mainly utilizes the energy transfer of spectra overlapping to prepare the adjustable fluorescent material of emission peak.
Referring to accompanying drawing 4, it is that the divalent manganesetion of different concns of the invention process example 3,6,7,8,9,10 and 11 preparation is at Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+(x=0.005) in fluorescent material, excite with UV-light 365nm the luminescent spectrum figure obtaining.Can be seen by Fig. 4, the different fluorescent powder that the each enforcement of the present invention provides, their peak luminous wavelength is adjustable at 450-650nm, and spectrum covering is green to the yellow redness that arrives, and can be adapted to the LED chip of different-waveband.In Fig. 4, curve (1), (2), (3), (4), (5), (6), (7) be respectively by embodiment 3,, the spectral radiation curves of the fluorescent material sample prepared of 6,7,8,9,10 and 11 technical schemes, as seen from Figure 4, along with the energy of divalent manganesetion concentration is large, the luminous intensity of fluorescent material weakens gradually.The cie color coordinate of the different fluorescent powder that the each enforcement of the present invention provides is as shown in table 1 below:
Table 1: fluorescent material Ca of the present invention
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+(x=0.005) with white light use Y
3al
5o
12: xCe
2+the contrast of cie color coordinate
Claims (5)
1. the adjustable phosphate phosphor of emission peak for white light LEDs, is characterized in that: its moiety is by following chemical formulation: Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+, x span is that 0.002～0.2, y span is 0.002～0.2.
2. the preparation method of the adjustable phosphate phosphor of emission peak for a kind of white light LEDs according to claim 1, is characterized in that comprising the following steps:
1. according to chemical general formula Ca
9 (1-x-y)la (PO
4)
7: xEu
2+, yMn
2+calculate respectively, take reaction reagent EuO, A.R.,, A.R. represents analytical pure, MnO, A.R., CaCO
3, purity is 99.9%, La
2o
3, purity is 99.99%, (NH
4)
2h (PO
4), purity is 99.99%; They are ground in mortar 2～3 hours, it is fully mixed.
2. said mixture is packed into crucible, compacting, and be placed in air High Temperature Furnaces Heating Apparatus, be warming up to 1200 ℃ and sintering 8 hours;
3. cooling rear taking-up its grinding is crushed to certain particle size, packs crucible into, then in reduction furnace, is warming up to 1000 ℃ of reduction 8 hours;
4. in reducing atmosphere, be cooled to room temperature, by above-mentioned calcination thing from reduction furnace, take out, broken again, with deionized water wash, then in 120～150 ℃ of baking ovens, toast 6～8 hours, obtain phosphate phosphor.
3. the preparation method of the adjustable phosphate phosphor of emission peak for a kind of white light LEDs according to claim 2, is characterized in that: step takes (NH in 1.
4)
2h (PO
4) excessive 3～5% to make up the volatilization loss of calcination process.
4. the preparation method of the adjustable phosphate phosphor of emission peak for a kind of white light LEDs according to claim 2, is characterized in that: the step speed that 2., 3. middle sintering temperature raises is 8～12 ℃/min.
5. the preparation method of the adjustable phosphate phosphor of emission peak for a kind of white light LEDs according to claim 2, is characterized in that: step 3. middle reducing atmosphere is H
2/ N
2mixed gas (H
2volume content is 15%, N
2volume content is 85%).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105087003A (en) * | 2015-09-02 | 2015-11-25 | 中国科学院长春应用化学研究所 | Orange LED fluorescent powder as well as preparation method and application thereof |
| CN106833603A (en) * | 2016-10-26 | 2017-06-13 | 广东工业大学 | A kind of inorganic particle ability of reverse photochromism material and its preparation method and application |
| CN108300466A (en) * | 2018-01-16 | 2018-07-20 | 北京科技大学 | A kind of red fluorescence powder and preparation method thereof |
| CN111978961A (en) * | 2020-09-10 | 2020-11-24 | 山东大学 | Preparation method of phosphate luminescent material with adjustable luminescent color and luminescent material prepared by method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105087003A (en) * | 2015-09-02 | 2015-11-25 | 中国科学院长春应用化学研究所 | Orange LED fluorescent powder as well as preparation method and application thereof |
| CN105087003B (en) * | 2015-09-02 | 2017-05-17 | 中国科学院长春应用化学研究所 | Orange LED fluorescent powder as well as preparation method and application thereof |
| US10414975B2 (en) | 2015-09-02 | 2019-09-17 | Changchun Institute Of Applied Chemistry Chinese Academy Of Sciences | Orange-yellow-emitting phosphor for LEDs, preparation method and use thereof |
| CN106833603A (en) * | 2016-10-26 | 2017-06-13 | 广东工业大学 | A kind of inorganic particle ability of reverse photochromism material and its preparation method and application |
| CN106833603B (en) * | 2016-10-26 | 2019-08-27 | 广东工业大学 | A kind of inorganic particle ability of reverse photochromism material and its preparation method and application |
| CN108300466A (en) * | 2018-01-16 | 2018-07-20 | 北京科技大学 | A kind of red fluorescence powder and preparation method thereof |
| CN111978961A (en) * | 2020-09-10 | 2020-11-24 | 山东大学 | Preparation method of phosphate luminescent material with adjustable luminescent color and luminescent material prepared by method |
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