CN105694875B - A kind of LED MAlSiO4:Er3+The preparation method of green light fluorescent powder - Google Patents
A kind of LED MAlSiO4:Er3+The preparation method of green light fluorescent powder Download PDFInfo
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Abstract
The invention belongs to wet chemistry method to prepare phosphor technologies field, and in particular to a kind of LED MAlSiO4：Er3+The preparation method of green light fluorescent powder.Using solvent hot preparation MxSr1‑xTiO3：Er3+(0 ＜ x≤0.5) high-purity green light fluorescent powder, can obtain MAlSiO under later stage low temperature calcination4：Er3+Green light fluorescent powder.Compared with traditional high temperature solid-state method, the later stage needed for solvent heat, calcining heat was low, and not high to equipment requirement, energy consumption is relatively low, was adapted to industrialized production；Er in gained fluorescent powder3+It is uniformly dispersed, easily into MxSr1‑xTiO3In realize energy transmission；The emission peak half-wave of gained green light fluorescent powder is wide relatively narrow, and green light excitation purity is high；Particle size distribution is uniform, is conducive to the uniform use for mixing, being adapted to high colour gamut white light LEDs with glue in the application of fluorescent powder later stage.
Description
Technical field
The invention belongs to wet chemistry method to prepare phosphor technologies field, and in particular to a kind of LED MAlS iO4:Er3+It is green
The preparation method of emitting phosphor.
Background technology
At present, rare earth luminescent material has become the core material in the fields such as presentation of information, lighting source, photoelectric device.
Wherein, what is be most widely used is that can be excited by ultraviolet light-blue light (200~500nm) and produce the fluorescence of different glow colors
Powder material.High luminous intensity, high color purity and the uniform particle size of fluorescent powder can significantly improve photoelectric device
Performance.Green light fluorescent powder is one of important composition of three primary colors fluorescent powder, and green light fluorescent powder basis material mainly wraps at present
Aluminate, silicate, tungstates and titanate etc. are included, but the green light fluorescent powder of different systems is in excitation purity and luminous intensity
Have differences.
2011, Huang Yanlin et al. was with alkaline earth carbonate, SiO2、Er2O3Deng for raw material, under reducing atmosphere condition in
1~15h is calcined at 1000~1500 DEG C, up to Ca7-7x-7yM7yEr7x(SiO4)4Green light fluorescent powder.It was found that the fluorescent powder is ultraviolet
Green light can be launched under near ultraviolet excitation, the characteristics of luminous efficiency is high, excitation wave length and width.2012, Chen Lei et al. with nanometer-
Micron SiO2、Er2O3And alkaline earth metal carbonate, alkaline earth oxide etc. are raw material, under hydrogen, nitrogen mixture atmosphere,
4~20h is calcined at 1400~1700 DEG C, up to (Ae1-xErx)3SiO5Green light fluorescent powder, it is glimmering under the excitation of 460nm blue lights
Light powder launches the green light that wavelength is 600nm, and the luminous intensity height of fluorescent powder, chemical stability are good.
At present, the Er reported3+The preparation method of silicate activated fluorescent powder is mostly high temperature solid-state method, after high-temperature calcination
Activator mixing is uneven in powder, causes phosphor emission peak wider, green light excitation purity is low.Meanwhile obtained by high temperature solid-state method
Fluorescent powder grain particle size is uneven, the strong influence actual use performance of fluorescent powder in the devices.
The content of the invention
For this reason, the technical problems to be solved by the invention are to overcome Er obtained by conventional solid-state method3+Silicate activated green light
Phosphor material powder, directly carries out high-temperature calcination, and activator mixing is uneven in gained fluorescent powder, and it is in broadband to cause green light fluorescent powder
Emission peak, green light excitation purity are low；Fluorescent powder grain particle size is uneven at the same time, influences during later stage use with encapsulating glue
Mixing uniformity technical bottleneck, so as to propose that a kind of fluorescent powder grain particle diameter distribution is uniform, emission peak half-wave is wide relatively narrow, green
Photochromic purity is high, is adapted to the MAlSiO used of high colour gamut white light LEDs4:Er3+The preparation method of green light fluorescent powder.
A kind of in order to solve the above technical problems, LED MAlSiO of disclosure of the invention4:Er3+The preparation of green light fluorescent powder
Method, wherein, described method includes following steps：
1) Al (NO are weighed3)3·9H2O particles are placed in high-pressure bottle, then absolute ethyl alcohol and steaming are added into high-pressure bottle
Distilled water, treats Al (NO3)3·9H2O dissolves to form Al (NO3)3Solution；
2) M is weighed2O, MOH or MNO3In one kind, SiO2With Si (OC2H5)4In one kind；And Er (NO3)3·6H2O；
Then three is mixed, obtains mixture, the mixture added jointly in the high-pressure bottle of step 1)；
M element can be at least one of Li, Na, K, Ag；
3) high-pressure bottle of step 2) is placed in and carries out heated at high speed stirring, be sufficiently mixed each reactant；
4) by after the high-pressure bottle heating treatment in step 3), then slow cooling processing, obtain solvent hot；
5) the solvent hot obtained by step 4) is subjected to low temperature drying processing, obtains solvent heat presoma.
6) after the solvent heat presoma obtained by step 5) being carried out gradient increased temperature processing, then cooling grinding is carried out, obtained
To MAlSiO4:Er3+Green light fluorescent powder.
Preferably, the preparation method, wherein, the volume ratio of absolute ethyl alcohol and distilled water described in step 1) is
0.1~0.6: 1.
The preferable preparation method, wherein, the Al (NO described in step 1)3)3The concentration of solution for 0.20~
1.0mol/L。
Preferably, the preparation method, wherein, the Al (NO obtained by step 1)3)31 elements of A and step 2) in solution
The mixture in each metallic element molar ratio be Al: M: Si: Er=1: 1: 1: 0.002~0.05.
Preferably, the preparation method, wherein, step 1) and 2) in each material for weighing be required to be placed on high-pressure bottle
In, wherein the Al (NO3)3·9H2The ratio that O particles account for the high-pressure bottle volume is 10%~80%.
Preferably, any one of them preparation method, wherein, the blender used in stirring described in step 3) is magnetic force
Blender, magnetic rotor rotating speed are 240rpm, and temperature is 50 DEG C, and heating time is 3 0min.
Preferably, any one of them preparation method, wherein, solvent thermal reaction is specially in step 4)：First heat up
Speed is 5 DEG C/min, is warming up to 100~200 DEG C, the time is 1~6h；Then slow cooling processing is carried out again, and cooling rate is
0.1~0.3 DEG C/min, it is cooled to 80 DEG C.
It is any one of preferable, the preparation method, wherein, the temperature of the low temperature drying processing described in step 5) is 60
℃。
It is more highly preferred to, any one of them preparation method, wherein, in the step 6), the gradient increased temperature processing tool
Body is：Step 5 products therefrom is placed in resistance furnace, 320~380 DEG C are warming up to the programming rate of 5 DEG C/min, insulation 3~
10h；600~950 are warming up to the programming rate of 2 DEG C/min again, calcines 3~12h.
The above technical solution of the present invention has the following advantages over the prior art：
(1) present invention prepares MAlSiO using solvent-thermal method4:Er3+Green light fluorescent powder, under later stage low temperature calcination (700~
1000 DEG C) MAlSiO can be obtained4:Er3+Green light fluorescent powder.Compared with traditional high temperature solid-state method, the later stage needed for solvent-thermal method
Calcining heat is low, and technique is simple, and energy consumption is relatively low, is adapted to industrialized production.
(2) present invention prepares MAlSiO using solvent-thermal method4:Er3+Green light fluorescent powder, compared with conventional solid-state method, solvent
Er in fluorescent powder obtained by hot method3+It is uniformly dispersed, easily into MAlSiO4In realize energy transmission, the hair of gained green light fluorescent powder
It is wide relatively narrow to penetrate peak half-wave, green light excitation purity is higher.
(3) present invention prepares MAlSiO using solvent-thermal method4:Er3+Green light fluorescent powder, compared with conventional solid-state method, gained
The grain diameter size distribution of fluorescent powder is uniform, is conducive to mix with the uniform of glue in the application of fluorescent powder later stage.
Brief description of the drawings
In order to make the content of the present invention more clearly understood, the specific embodiment below according to the present invention and combination
Attached drawing, the present invention is described in further detail, wherein
Fig. 1 is KAlSiO prepared by embodiment 14:0.01Er3+The emission spectrum of green light fluorescent powder；
Fig. 2 is Li prepared by embodiment 50.25K0.75AlSiO4:0.002Er3+The XRD spectrum of green light fluorescent powder.
Embodiment
Present embodiment discloses a kind of LED MAlSiO for embodiment 14:Er3+The preparation method of green light fluorescent powder, specific step
It is rapid as follows：
(1) Al (NO of 3.001g are weighed3)3·9H2O particles are placed in high-pressure bottle, and (high-pressure bottle volume is 80mL, material
For polytetrafluoroethyllining lining, stainless steel casing, pressure limit is 0~10Mpa) in, (refer to solvent volume by packing ratio for 50%
Account for the ratio of high-pressure bottle volume), C2H5O (absolute ethyl alcohol): H2The volume ratio of O (distilled water)=0.29: 1, into high-pressure bottle
Add the C of 9mL2H5The H of O and 31mL2O, treats Al (NO3)3·9H2After O particles fully dissolve, concentration is formed in high-pressure bottle
For the Al (NO of 0.2mol/L3)3Solution (refers to Al3+Account for C2H5O and H2The concentration of O mixed liquor cumulative volumes)；
(2) according to K: Al: Si=1: 1: 1 molar ratio, weigh the KHCO of 0.801g3With the Si (OC of 1.667g2H5)4。
According to Er3+Molar concentration (refer to Er for 1.0mol%3+Account for basis material KAlSiO4Molar concentration), weigh the Er of 0.036g
(NO3)3·5H2O powders.By KHCO3、Si (OC2H5)4) and Er (NO3)3·5H2O powders add the high pressure of step 1) jointly
In container.
(3) high-pressure bottle of step 2) is placed on magnetic stirring apparatus, it is 2 40rpm to control magnetic rotor rotating speed, temperature
At 50 DEG C, to stir and heating 30min, it is sufficiently mixed each reactant.
(4) high-pressure bottle in step 3) is placed in baking oven, with the programming rate of 5 DEG C/min, is warming up to 200 DEG C, protects
Warm 2h.Again with the slow cooling speed of 0.3 DEG C/min, 80 DEG C are cooled to, is taken out after then cooling to room temperature with the furnace.
(5) solvent hot obtained by step 4) is dried in air atmosphere at 60 DEG C, is subsequently placed in mortar and grinds
Mill is uniform, that is, obtains solvent heat presoma.
(6) solvent heat presoma obtained by step 5) is placed in resistance furnace, 380 is warming up to the programming rate of 5 DEG C/min
DEG C insulation 5h, then with the programming rate of 2 DEG C/min be warming up to 900 DEG C calcining 3 h, take out, be ground after furnace cooling, to obtain the final product
KAlSiO4:0.01Er3+Green light fluorescent powder.Dependence test is carried out to gained fluorescent powder, as shown in Figure 1, finding KAlSiO4:
0.01Er3+The emission peak peak wavelength of green light fluorescent powder is 534nm, and chromaticity coordinates is (x=0.2052, y=0.6834).
Present embodiment discloses a kind of LED MAlSiO for embodiment 24:Er3+The preparation method of green light fluorescent powder, specific step
It is rapid as follows：
(1) Al (NO of 4.502g are weighed3)3·9H2O particles are placed in high-pressure bottle, and (high-pressure bottle volume is 80mL, material
For polytetrafluoroethyllining lining, stainless steel casing, pressure limit is 0~10Mpa) in, (refer to solvent volume by packing ratio for 30%
Account for the ratio of high-pressure bottle volume), C2H5O (absolute ethyl alcohol): H2The volume ratio of O (distilled water)=0.25: 1, into high-pressure bottle
Add the C of 4.8mL2H5The H of O and 19.2mL2O, treats Al (NO3)3·9H2After O particles fully dissolve, formed in high-pressure bottle
Concentration is the Al (NO of 0.5mol/L3)3Solution (refers to Al3+Account for C2H5O and H2The concentration of O mixed liquor cumulative volumes)；
(2) according to K: Al: Si=1: 1: 1 molar ratio, weigh the KHCO of 1.201g3With the SiO of 0.721g2.According to Er3 +Molar concentration (refer to Er for 2mol%3+Account for basis material KAlSi O4Molar concentration), weigh the Er (NO of 0.106g3)3·
5H2O powders.By KHCO3、SiO2And Er (NO3)3·5H2O powders add in the high-pressure bottle of step 1) jointly.
(3) high-pressure bottle of step 2) is placed on magnetic stirring apparatus, it is 2 40rpm to control magnetic rotor rotating speed, temperature
At 50 DEG C, to stir and heating 30min, it is sufficiently mixed each reactant.
(4) high-pressure bottle in step 3) is placed in baking oven, with the programming rate of 5 DEG C/min, is warming up to 190 DEG C, protects
Warm 3h.Again with the slow cooling speed of 0.25 DEG C/min, 80 DEG C are cooled to, is taken out after then cooling to room temperature with the furnace.
(5) solvent hot obtained by step 4) is dried in air atmosphere at 60 DEG C, is subsequently placed in mortar and grinds
Mill is uniform, that is, obtains solvent heat presoma.
(6) solvent heat presoma obtained by step 5) is placed in resistance furnace, 370 is warming up to the programming rate of 5 DEG C/min
DEG C insulation 9h, then with the programming rate of 2 DEG C/min be warming up to 800 DEG C calcining 6 h, take out, be ground after furnace cooling, to obtain the final product
KAlSiO4:0.02Er3+Green light fluorescent powder.Dependence test is carried out to gained fluorescent powder, finds KAlSiO4:0.02Er3+Green light is glimmering
The emission peak peak wavelength of light powder is 532nm, and chromaticity coordinates is (x=0.2045, y=0.6807).
Embodiment 3：Present embodiment discloses a kind of LED MAlSiO4:Er3+The preparation method of green light fluorescent powder, specific step
It is rapid as follows：
(1) Al (NO of 6.302g are weighed3)3·9H2O particles are placed in high-pressure bottle, and (high-pressure bottle volume is 80mL, material
For polytetrafluoroethyllining lining, stainless steel casing, pressure limit is 0~10Mpa) in, (refer to solvent volume by packing ratio for 60%
Account for the ratio of high-pressure bottle volume), C2H5O (absolute ethyl alcohol): H2The volume ratio of O (distilled water)=0.2: 1, into high-pressure bottle
Add the C of 8mL2 H5The H of O and 40mL2O, treats Al (NO3)3·9H2After O particles fully dissolve, concentration is formed in high-pressure bottle
For the Al (NO of 0.35mol/L3)3Solution (refers to Al3+Account for C2H5O and H2The concentration of O mixed liquor cumulative volumes)；
(2) according to Li: Na: Al: Si=0.5: 0.5: 1: 1 molar ratio, weigh the LiOHH of 0.352g2O、0.336g
NaOH and 3.450g Si (OC2H5)4.According to Er3+Molar concentration (refer to Er for 0.5mol%3+Account for basis material
Li0.5Na0.5AlSiO4Molar concentration), weigh the Er (NO of 0. 038g3)3·5H2O powders.By LiOHH2O、NaOH、Si
(OC2H5)4) and Er (N O3)3·5H2O powders add in the high-pressure bottle of step 1) jointly.
(3) high-pressure bottle of step 2) is placed on magnetic stirring apparatus, it is 2 40rpm to control magnetic rotor rotating speed, temperature
At 50 DEG C, to stir and heating 30min, it is sufficiently mixed each reactant.
(4) high-pressure bottle in step 3) is placed in baking oven, with the programming rate of 5 DEG C/min, is warming up to 180 DEG C, protects
Warm 1h.Again with the slow cooling speed of 0.15 DEG C/min, 80 DEG C are cooled to, is taken out after then cooling to room temperature with the furnace.
(5) solvent hot obtained by step 4) is dried in air atmosphere at 60 DEG C, is subsequently placed in mortar and grinds
Mill is uniform, that is, obtains solvent heat presoma.
(6) solvent heat presoma obtained by step 5) is placed in resistance furnace, 350 is warming up to the programming rate of 5 DEG C/min
DEG C insulation 6h, then with the programming rate of 2 DEG C/min be warming up to 950 DEG C calcining 9 h, take out, be ground after furnace cooling, to obtain the final product
Li0.5Na0.5AlSiO4:0.005Er3+Green light fluorescent powder.Dependence test is carried out to gained fluorescent powder, is found
Li0.5Na0.5AlSiO4:0.005Er3+The emission peak peak wavelength of green light fluorescent powder is 535nm, and chromaticity coordinates is (x=0.2103, y
=0.6747).
Embodiment 4：Present embodiment discloses a kind of LED MAlSiO4:Er3+The preparation method of green light fluorescent powder, specific step
It is rapid as follows：
(1) Al (NO of 2.251g are weighed3)3·9H2O particles are placed in high-pressure bottle, and (high-pressure bottle volume is 80mL, material
For polytetrafluoroethyllining lining, stainless steel casing, pressure limit is 0~10Mpa) in, (refer to solvent volume by packing ratio for 10%
Account for the ratio of high-pressure bottle volume), C2H5O (absolute ethyl alcohol): H2The volume ratio of O (distilled water)=0.45: 1, into high-pressure bottle
Add the C of 2.5mL2H5The H of O and 5.5mL2O, treats Al (NO3)3·9H2After O particles fully dissolve, formed in high-pressure bottle dense
Spend the Al (NO for 0.75mol/L3)3Solution (refers to Al3+Account for C2H5O and H2The concentration of O mixed liquor cumulative volumes)；
(2) according to Ag: Li: Al: Si=0.2: 0.8: 1: 1 molar ratio, weigh the AgNO of 0.204g3, 0.201g
LiOH·H2The SiO of O and 0.361g2.According to Er3+Molar concentration (refer to Er for 3.5mol%3+Account for basis material
Ag0.2Li0.8AlSiO4Molar concentration), weigh the Er (NO of 0.093g3)3·5H2O powders.By AgNO3、LiOH·H2O、
SiO2And Er (NO3)3·5H2O powders add in the high-pressure bottle of step 1) jointly.
(3) high-pressure bottle of step 2) is placed on magnetic stirring apparatus, it is 2 40rpm to control magnetic rotor rotating speed, temperature
At 50 DEG C, to stir and heating 30min, it is sufficiently mixed each reactant.
(4) high-pressure bottle in step 3) is placed in baking oven, with the programming rate of 5 DEG C/min, is warming up to 160 DEG C, protects
Warm 6h.Again with the slow cooling speed of 0.10 DEG C/min, 80 DEG C are cooled to, is taken out after then cooling to room temperature with the furnace.
(5) solvent hot obtained by step 4) is dried in air atmosphere at 60 DEG C, is subsequently placed in mortar and grinds
Mill is uniform, that is, obtains solvent heat presoma.
(6) solvent heat presoma obtained by step 5) is placed in resistance furnace, 330 is warming up to the programming rate of 5 DEG C/min
DEG C insulation 10h, then with the programming rate of 2 DEG C/min be warming up to 600 DEG C calcining 4h, take out, be ground after furnace cooling, i.e.,
Obtain Ag0.2Li0.8AlSiO4:0.035Er3+Green light fluorescent powder.Dependence test is carried out to gained fluorescent powder, as shown in Figure 1, finding
Ag0.2Li0.8AlSiO4:0.035 Er3+The emission peak peak wavelength of green light fluorescent powder is 530nm, chromaticity coordinates for (x=0.2027,
Y=0.6819).
Embodiment 5：Present embodiment discloses a kind of LED MAlSiO4:Er3+The preparation method of green light fluorescent powder, specific step
It is rapid as follows：
(1) Al (NO of 6.002g are weighed3)3·9H2O particles are placed in high-pressure bottle, and (high-pressure bottle volume is 80mL, material
For polytetrafluoroethyllining lining, stainless steel casing, pressure limit is 0~10Mpa) in, (refer to solvent volume by packing ratio for 80%
Account for the ratio of high-pressure bottle volume), C2H5O (absolute ethyl alcohol): H2The volume ratio of O (distilled water)=0.1: 1, into high-pressure bottle
Add the C of 5.8mL2H5The H of O and 58.2mL2O, treats Al (NO3)3·9H2After O particles fully dissolve, formed in high-pressure bottle
Concentration is the Al (NO of 0.25mol/L3)3Solution (refers to Al3+Account for C2H5O and H2The concentration of O mixed liquor cumulative volumes)；
(2) according to Li: K: Al: Si=0.25: 0.75: 1: 1 molar ratio, weigh the LiOHH of 0.168g2O、
1.022g KHCO3With the SiO of 0.961g2.According to Er3+Molar concentration (refer to Er for 0.2mol%3+Account for basis material
Li0.25K0.75AlSiO4Molar concentration), weigh the Er (NO of 0.014g3)3·5H2O powders.By LiOHH2O、KHCO3、
SiO2And Er (NO3)3·5H2O powders add in the high-pressure bottle of step 1) jointly.
(3) high-pressure bottle of step 2) is placed on magnetic stirring apparatus, it is 2 40rpm to control magnetic rotor rotating speed, temperature
At 50 DEG C, to stir and heating 30min, it is sufficiently mixed each reactant.
(4) high-pressure bottle in step 3) is placed in baking oven, with the programming rate of 5 DEG C/min, is warming up to 130 DEG C, protects
Warm 5h.Again with the slow cooling speed of 0.12 DEG C/min, 80 DEG C are cooled to, is taken out after then cooling to room temperature with the furnace.
(5) solvent hot obtained by step 4) is dried in air atmosphere at 60 DEG C, is subsequently placed in mortar and grinds
Mill is uniform, that is, obtains solvent heat presoma.
(6) solvent heat presoma obtained by step 5) is placed in resistance furnace, 360 is warming up to the programming rate of 5 DEG C/min
DEG C insulation 3h, then with the programming rate of 2 DEG C/min be warming up to 700 DEG C calcining 1 0h, take out, be ground after furnace cooling, i.e.,
Obtain Li0.25K0.75AlSiO4:0.002Er3+Green light fluorescent powder.Dependence test is carried out to gained fluorescent powder, as shown in Fig. 2, finding
Li0.25K0.75AlSiO4:0.002 Er3+The emission peak peak wavelength of green light fluorescent powder is 532nm, chromaticity coordinates for (x=0.2035,
Y=0.6833).
Embodiment 6：Present embodiment discloses a kind of LED MAlSiO4:Er3+The preparation method of green light fluorescent powder, specific step
It is rapid as follows：
(1) Al (NO of 12.004g are weighed3)3·9H2O particles are placed in high-pressure bottle, and (high-pressure bottle volume is 80mL, material
For polytetrafluoroethyllining lining, stainless steel casing, pressure limit is 0~10Mpa) in, (refer to solvent volume by packing ratio for 40%
Account for the ratio of high-pressure bottle volume), C2H5O (absolute ethyl alcohol): H2The volume ratio of O (distilled water)=0.6: 1, into high-pressure bottle
Add the C of 12mL2H5The H of O and 20mL2O, treats Al (NO3)3·9H2After O particles fully dissolve, concentration is formed in high-pressure bottle
For the Al (NO of 1.0mol/L3)3Solution (refers to Al3+Account for C2H5O and H2The concentration of O mixed liquor cumulative volumes)；
(2) according to Na: Al: Si=1: 1: 1 molar ratio, weigh the SiO of the NaOH and 1.923g of 1.281g2.According to Er3 +Molar concentration (refer to Er for 5mol%3+Account for basis material NaAlSi O4Molar concentration), weigh the Er (NO of 0.709g3)3·
5H2O powders.By NaOH, SiO2And Er (NO3)3·5H2O powders add in the high-pressure bottle of step 1) jointly.
(3) high-pressure bottle of step 2) is placed on magnetic stirring apparatus, it is 2 40rpm to control magnetic rotor rotating speed, temperature
At 50 DEG C, to stir and heating 30min, it is sufficiently mixed each reactant.
(4) high-pressure bottle in step 3) is placed in baking oven, with the programming rate of 5 DEG C/min, is warming up to 100 DEG C, protects
Warm 4h.Again with the slow cooling speed of 0.2 DEG C/min, 80 DEG C are cooled to, is taken out after then cooling to room temperature with the furnace.
(5) solvent hot obtained by step 4) is dried in air atmosphere at 60 DEG C, is subsequently placed in mortar and grinds
Mill is uniform, that is, obtains solvent heat presoma.
(6) solvent heat presoma obtained by step 5) is placed in resistance furnace, 320 is warming up to the programming rate of 5 DEG C/min
DEG C insulation 8h, then with the programming rate of 2 DEG C/min be warming up to 850 DEG C calcining 1 2h, take out, be ground after furnace cooling, i.e.,
Obtain NaAlSiO4:0.05Er3+Green light fluorescent powder.Dependence test is carried out to gained fluorescent powder, finds NaAlSiO4:0.05Er3+It is green
The emission peak peak wavelength of emitting phosphor is 532nm, and chromaticity coordinates is (x=0.2031, y=0.6850).
Obviously, the above embodiments are merely examples for clarifying the description, and the restriction not to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (8)
- A kind of 1. LED MAlSiO4：Er3+The preparation method of green light fluorescent powder, it is characterised in that the described method includes following step Suddenly：1) Al (NO are weighed3)3·9H2O, adds absolute ethyl alcohol and distilled water, treats Al (NO3)3·9H2O dissolves to form Al (NO3)3 Solution；2) M is weighed2O, MOH or MNO3In one kind, SiO2With Si (OC2H5)4In one kind；And Er (NO3)3·6H2O；Then Three is mixed, obtains at least one of mixture, M element Li, Na, K, Ag；3) Al (NO for obtaining step 1)3)3The mixture that solution and step 2) obtain is mixed, and stirring, fills each reactant Divide mixing；4) material obtained by step 3) is subjected to solvent thermal reaction, obtains solvent hot；5) processing is dried in the solvent hot obtained by step 4)；6) product obtained by step 5) is carried out gradient increased temperature to handle to 600~950 DEG C, is subsequently cooled to room temperature, then grind place Reason, obtains MAlSiO4：Er3+Green light fluorescent powder.
- 2. preparation method as claimed in claim 1, it is characterised in that the body of absolute ethyl alcohol and distilled water described in step 1) Product is than being 0.1~0.6: 1.
- 3. preparation method as claimed in claim 2, it is characterised in that the Al (NO described in step 1)3)3The concentration of solution is 0.20~1.0mol/L.
- 4. preparation method as claimed in claim 3, it is characterised in that the Al (NO obtained by step 1)3)3Al elements in solution Molar ratio with each metallic element in the mixture of step 2) is Al: M: Si: Er=1: 1: 1: 0.002~0.05.
- 5. the preparation method as described in any one of claim 1-4, it is characterised in that stirring used in the stirring described in step 3) It is magnetic stirring apparatus to mix device, and magnetic rotor rotating speed is 240rpm, and temperature is 50 DEG C, heating time 30min.
- 6. the preparation method as described in any one of claim 1-4, it is characterised in that solvent thermal reaction is specially in step 4)： It is 5 DEG C/min first to carry out programming rate, is warming up to 100~200 DEG C, the time is 1~6h；Then slow cooling processing is carried out again, Cooling rate is 0.1~0.3 DEG C/min, is cooled to 80 DEG C.
- 7. the preparation method as described in any one of claim 1-4, it is characterised in that the temperature of the drying process described in step 5) For 60 DEG C.
- 8. the preparation method as described in any one of claim 1-4, it is characterised in that in the step 6), the gradient increased temperature Processing is specially：Step 5) products therefrom is placed in resistance furnace, 320~380 DEG C are warming up to the programming rate of 5 DEG C/min, Keep the temperature 3~10h；600~950 DEG C are warming up to the programming rate of 2 DEG C/min again, calcines 3~12h.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20130035757A (en) * | 2011-09-30 | 2013-04-09 | 엘지이노텍 주식회사 | Phosphor and method of fabricating phosphor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20130035757A (en) * | 2011-09-30 | 2013-04-09 | 엘지이노텍 주식회사 | Phosphor and method of fabricating phosphor |
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| Eu3+掺杂新颖铝硅酸盐的合成、表征及发光特性;常加忠 等;《无机材料学报》;20060531;第21卷;565-570 * |
| Eu3+掺杂铝硅酸钾发光材料的合成及性能研究;石文杰 等;《中国稀土学报》;20140415;第32卷;164-169 * |
| Luminescent properties of (Na,M)AlSiO4:Eu2+ phosphors (M = Li, K, Mg, Ca);Deok Su Jo 等;《Journal of Ceramic Processing Research》;20131231;第14卷;s9-s11 * |
| Porous materials for alkali contaminated environments;Nora Brachold等;《Journal of the European Ceramic Society》;20130221;第33卷;2013-2021 * |
| Structural and Photoluminescence properties of nepheline-structure NaAlSiO4:Dy3+ nanophosphor;Ashwini Kumar等;《Journal of Alloys and Compounds》;20140430;第609卷;100-106 * |
| Synthesis and photoluminescence properties of new NaAlSiO4:Eu2+ phosphors for near-UV white LED applications;Deok Su Jo 等;《Optical Materials》;20111104;第34卷;696-699 * |
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