CN103509553B - Rare earth and manganese co-activated manganese phosphate fluorescent powder and manufacturing method thereof - Google Patents
Rare earth and manganese co-activated manganese phosphate fluorescent powder and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses rare earth and manganese co-activated manganese phosphate fluorescent powder and a manufacturing method thereof. The rare earth and manganese co-activated manganese phosphate fluorescent powder has the chemical formula as follows: Ba1-a-bMg2-cAl16-xPxO27+x:Eua.Mb.Mnc, wherein M represents for Ce and/or Tb, 0.005<=x<=0.5, 0.1<=a<=0.3, 0.0001<=b<=0.001, and 0.2<=c<=0.75. According to the chemical composition and the manufacturing method thereof, green fluorescent powder with the emitting peak wavelength of 515nm, high brightness and low light attenuation can be obtained through carrying out 254nm ultraviolet excitation on a finished product obtained through the processes of proportioning, high temperature pre-sintering, crushing, hydrogen reduction, crushing after-treatment and the like.
Description
Technical field
The present invention relates to a kind of rare earth, the coactivated aluminophosphates fluorescent material of manganese and manufacture method thereof.
Background technology
The coactivated many aluminate blue-green fluorescent powders of well-known europium manganese, describe fully aware of in PHOSPHORHANDBOOK (CRC Press Boca Raton London New York Washington.D.C.May, a 1998) book.Its crystalline structure is hexagonal, beta-alumina structure:
Ba
1-aMg
2-bAl
16O
27:Eu
a 2+﹒Mn
b 2+
Mn
2+for d-d forbidden transition, Mn
2+luminescence be by Eu
2+transmission ofenergy with Mn
2+increase and produce the green glow of 515nm.Mn
2+surrounded by oxygen coordination in tetrahedron, when environment or use temperature raise, Mn
2+be easy to be oxidized to tetravalence, cause fluorescent material brightness not high, fast decay.Therefore, for a long time, can only be used in, Mn
2+few (the general Mn of content
2+be less than 0.02mol), emission peak wavelength is 450nm and secondary peak is 515nm, as in the bimodal blue-green fluorescent powder of three primary colors fluorescent powder.And emission peak wavelength is the green emitting phosphor of 515nm, because low lightness, light decay are large, seldom there is actual use value.In addition publication number is in the open file of CN101113329, aSrO ﹒ bAl
2o
3: dCe ﹒ fMn is under 254nm excites, and emission peak wavelength is 516nm, also because its luminosity is low, light decay large, does not also have actual use value.Instant invention overcomes above-mentioned difficulties, the manganese ion concentration of fluorescent material is improved more than 20 times, thus under the exciting of 254nm ultraviolet, emission peak wavelength is the fluorescent material of the strong green glow of 515nm.This light-emitting phosphor brightness is high, light decay is little, can be applicable to the complementary color fluorescent material in high colour developing or superelevation color developing fluorescent material.Also can as duplicating machine fluorescent-lamp-use fluorescent material.
Summary of the invention
One object of the present invention be to provide a kind of can by the high brightness of ultraviolet excitation, low light attenuation blue-green fluorescent powder.For realizing this purpose, the technical solution adopted in the present invention is: at Eu
2+and Mn
2+under coactivated condition, in many aluminate fluorescent powders, be mixed with Ce and/or Tb, thus the exciting and launch of sensitization Mn.And introduce micro anion phosphorus at aluminate, thus enhance the green emitting intensity of fluorescent material.
Chemical constitution formula of the present invention is:
Ba
1-a-bMg
2-cAl
16-xP
xO
27+x:Eu
a﹒M
b﹒Mn
c
In formula, M represents Ce and/or Tb; Wherein, 0.005≤x≤0.5; 0.1≤a≤0.3; 0.0001≤b≤0.001; 0.2≤c≤0.75.
Another object of the present invention is to provide the manufacture method of fluorescent material of the present invention, and step comprises:
1) batch mixing: according to the chemical constitution of fluorescent material of the present invention, take raw material, and it is fully mixed.
2) High Temperature Pre burns till: the raw material mixed is loaded crucible, and temperature controls more than 1600 DEG C, is incubated 2 ~ 5 hours.Because the present invention adopts fluxless solid reaction process, for guaranteeing that solid reaction process is carried through to the end, raw material in crucible compresses, pier is real, and in the feed between burrow.
3) hydrogen reduction: the material of pre-fired is broken, in small, broken bits, and 150 orders sieve, pine loads crucible, guarantee that temperature controls more than 1450 DEG C in reducing atmosphere, insulation reductase 12 ~ 4 hour.
4) material after reduction, fragmentation, 150 orders in small, broken bits are sieved, glassie wet ball mill, cleaning, wetly to sieve, dry, 200 orders sieve, and namely obtain product of the present invention.
High-lighting effect of the present invention is:
1) increase substantially the green emission intensity that emission peak wavelength is 515nm, the associated luminance of most preferred embodiment brings up to more than 150%;
2) fluorescent material also increases substantially in 600 DEG C of thermostabilitys heated and associated luminance sustainment rate.
As can be seen here, adopt chemical constitution of the present invention and manufacture method of the present invention just can obtain high brightness, fluorescent material that light decay is little, effect is fairly obvious.
Accompanying drawing explanation
Fig. 1 is the utilizing emitted light spectrogram of green emitting phosphor of the present invention under 254nm burst of ultraviolel;
Fig. 2 is under the burst of ultraviolel of 254nm, the dependent luminescence intensity comparison diagram of the emmission spectrum of the fluorescent material of comparative example 1 and embodiment 15;
Fig. 3 is comparative example 1 and embodiment 15 fluorescent material time dependent associated luminance (Br') variation diagram at 600 DEG C.
Embodiment
In conjunction with embodiment below, further illustrate the present invention.
In test, calculate each component content according to the chemical constitution formula of fluorescent material of the present invention, and take prepared using manufacture method synthesis of the present invention as required.In test, the introducing content b of Ce and/or Tb 0.0001 to 0.001 scope, the introducing content x of P (phosphorus) is 0.005-0.5, exceeds this scope, and successful declines.If the content a of rare-earth europium (Eu) is low lower than the energy of 0.1, Eu excitation-emission, the energy passing to manganese is little, causes fluorescent effect obviously to decline; If the content of europium is higher than 0.3, waste expensive rare-earth europium on the one hand, on the other hand, the europium of high density easily produces concentration quenching, causes fluorescent effect obviously to decline.When Fe content c is less than 0.2, launch 515nm green intensity by force, DeGrain; When Fe content c is more than 0.75, effect declines on the contrary.The content optimum value of preferred control manganese is 0.3.
embodiment 1
The chemical constitution formula of fluorescent material is: Ba
0.9mg
1.7al
16o
27: Eu
0.1mn
0.3
177.3g BaCO is accurately taken by above-mentioned chemical constitution
3, 68.51g MgO, 816g Al
2o
3, 17.6gEu
2o
3, 34.5g MnCO
3
embodiment 2
The chemical constitution formula of fluorescent material is: Ba
0.7mg
1.7al
16o
27: Eu
0.3mn
0.3
137.9g BaCO is accurately taken by above-mentioned chemical constitution
3, 68.51g MgO, 816g Al
2o
3, 52.8gEu
2o
3, 34.5g MnCO
3
embodiment 3
The chemical constitution formula of fluorescent material is: Ba
0.8mg
1.7al
15.995p
0.005o
27.
005: Eu
0.2mn
0.3
157.6g BaCO is accurately taken by above-mentioned chemical constitution
3, 68.51g MgO, 815.7g Al
2o
3, 66mg (NH
4)
2hPO
4, 35.2g Eu
2o
3, 34.5g MnCO
3
embodiment 4 ~ embodiment 13the chemical constitution formula of fluorescent material is as shown in table 1.
embodiment 14
The chemical constitution formula of fluorescent material is: Ba
0.7994mg
1.7(Al
15.5p
0.5o
27.5): Eu
0.2mn
0.3ce
0.0003tb
0.0003
157.48g BaCO is accurately taken by above-mentioned chemical constitution
3, 68.51g MgO, 790.5g Al
2o
3, 66g (NH
4)
2hPO
4, 35.2g Eu
2o
3, 34.5g MnCO
3, 51.6mg CeO, 56mg Tb
4o
7
embodiment 15
The chemical constitution formula of fluorescent material is: Ba
0.799mg
1.7(Al
15.5p
0.5o
27.5) Eu
0.2: Mn
0.3ce
0.0005tb
0.0005
157.4g BaCO is accurately taken by above-mentioned chemical constitution
3, 68.51g MgO, 790.5g Al
2o
3, 66g (NH
4)
2hPO
4, 35.2g Eu
2o
3, 34.5g MnCO
3, 86mg CeO, 93.5mg Tb
4o
7
manufacture method:
In the manufacture method of fluorescent material of the present invention, add high temperature burn in step.The object introducing high temperature burn in step is the formation preventing two aluminates, and two aluminates cause light-emitting phosphor brightness not high, the major reason that light-induced degradation is fast.In usual method, adopt a reduction method just can generate many aluminate fluorescent powders, but reduction temperature is generally all less than 1450 DEG C, this is because reduction furnace temperature is higher, particularly exists in the high temperature of reducing atmosphere, very easily damage equipment.Also have and adopt secondary reduction method not high to make up fluorescent material brightness.Even if reduction temperature is at 1500 DEG C, still has two a small amount of aluminates in fluorescent material, show through X diffraction, when temperature is more than 1600 DEG C, do not have two aluminates in fluorescent material, the present invention that Here it is introduces the object of high temperature pre-burning, be also the key character of manufacture method of the present invention.
The manufacture method of embodiment 1 ~ embodiment 13 is as follows:
1) batch mixing: accurately take raw material by the composition of fluorescent material, drops in blender and mixes 24 hours;
2) High Temperature Pre burns till: by the material of mixing, loads crucible, and compression, pier are real, at 1600 DEG C, in atmospheric air, is incubated 3 hours;
3) hydrogen reduction: by the material coarse crushing of burning till, crosses 100 mesh sieves, more in small, broken bits, crosses 150 mesh sieves, uses H
2: N
2the reducing atmosphere of=7:3,1450 DEG C are incubated reduction 3 hours;
4) material of high temperature reduction is broken, cross 150 mesh sieves, by the powder after sieving, diameter be the glassie of 2 ~ 5mm and pure water by powder: ball: the mass ratio mixing of pure water=1:2:3, ball milling 1 hour, removes glassie, takes advantage of 500 mesh sieves that wet;
5) use the hot water cleaning twice of 60 ~ 80 DEG C, then clean 3 times with normal temperature pure water, the consumption of each water is 5 times of powder;
6) material after cleaning dries 24 hours in 200 DEG C after dewatering, crosses 200 mesh sieves, obtain finished product after drying.
Wherein, High Temperature Pre burns till the object of step is generation in order to prevent dephasign two aluminate.The temperature of pre-fired must be greater than 1600 DEG C, and temperature is more high better, but too high temperature easily causes the damage of body of heater.Meet 1600 DEG C of insulations 3 hours as long as general, just enough can prevent the generation of dephasign two aluminate.High Temperature Pre burns till step and adopts fluxless solid reaction process, and for guaranteeing that solid reaction process is carried through to the end, the raw material in crucible compresses, pier is real, and in the feed between burrow.
Wherein, the object that last step (6) crosses 200 mesh sieves allows fluorescent material rub on screen cloth, and make powder produce the electrostatic of two like magnetic poles repel each other, such fluorescent tube factory is when using fluorescent material to size mixing, and fluorescent material can not be reunited, and film is even, and film quality is excellent.
In embodiment 1 ~ embodiment 13, the manufacture of fluorescent material adds P, Eu, Ce, Tb (see table 1) of different amount respectively, and it finally affects fluorescent material chromaticity coordinates y value, relative luminous brightness (Br) and associated luminance (Br ').Embodiment 14,15 is best composition embodiments, wherein comprehensively adds Eu, Mn, P, Ce, Tb (see table 1), below the manufacture method of DETAILS SECTIONExample 14,15.
The manufacture method of embodiment 14,15 is as follows:
1) batch mixing: accurately take raw material by the composition of fluorescent material, drops in blender and mixes 24 hours;
2) High Temperature Pre burns till: by the material of mixing, loads crucible, and compression, pier are real, at 1650 DEG C, in atmospheric air, is incubated 2 hours;
3) hydrogen reduction: by the material coarse crushing of burning till, crosses 100 mesh sieves, more in small, broken bits, crosses 150 mesh sieves, uses H
2: N
2the reducing atmosphere of=7:3,1550 DEG C of insulation reductase 12s hour;
4) material of high temperature reduction is broken, cross 150 mesh sieves, by the powder after sieving, diameter be the glassie of 2 ~ 5mm and pure water by powder: ball: the mass ratio mixing of pure water=1:2:3, ball milling 1 hour, removes glassie, takes advantage of 500 mesh sieves that wet;
5) use the hot water cleaning twice of 60 ~ 80 DEG C, then clean 3 times with normal temperature pure water, the consumption of each water is 5 times of powder;
6) material after cleaning dries 24 hours in 200 DEG C after dewatering, crosses 200 mesh sieves, obtain finished product after drying.
Wherein, High Temperature Pre burns till the object of step is generation in order to prevent dephasign two aluminate.The temperature of pre-fired must be greater than 1600 DEG C, and temperature is more high better, but too high temperature easily causes the damage of body of heater.High Temperature Pre burns till step and adopts fluxless solid reaction process, and for guaranteeing that solid reaction process is carried through to the end, the raw material in crucible compresses, pier is real, and in the feed between burrow.
Wherein, the object that last step (6) crosses 200 mesh sieves allows fluorescent material rub on screen cloth, and make powder produce the electrostatic of two like magnetic poles repel each other, such fluorescent tube factory is when using fluorescent material to size mixing, and fluorescent material can not be reunited, and film is even, and film quality is excellent.
For absolutely proving the superiority of fluorescent material of the present invention and manufacture method thereof, two comparative examples are devised in test, they all adopt same chemical constitution formula, and difference is that comparative example 1 adopts the manufacture of industry usual method, and comparative example 2 adopts manufacture method manufacture of the present invention.Object is contrast two kinds of manufacture method.
comparative example 1
The chemical constitution formula of fluorescent material is: Ba
0.8mg
1.7al
16eu
0.2: Mn
0.3
Comparative example 1 is common blue colour fluorescent powder chemical constitution, and its common manufacture method is as follows:
1) batch mixing: accurately take 157.6g BaCO
3, 68.51g MgO, 816g Al
2o
3, 35.2g Eu
2o
3, 34.5g MnCO
3, 2.5g fusing assistant H
3bO
3, drop in blender and mix 24 hours;
2) reductive firing: by the material of mixing, loads crucible, and send in reduction furnace and reduce, reducing atmosphere is H
2: N
2=7:3, reduction temperature is 1450 DEG C, and soaking time is 3 hours;
3) carry out fragmentation by operation in the same manner as in Example 1, sieve, ball milling, wet to sieve, clean, drying and processing;
4) after drying, 200 mesh sieves crossed by material, obtain finished product.
comparative example 2
The chemical constitution formula of fluorescent material is: Ba
0.8mg
1.7al
16eu
0.2: Mn
0.3
The chemical constitution of comparative example 2 is identical with the chemical constitution of comparative example 1, but manufacturing process is different, and its manufacture method is as follows;
1) batch mixing: accurately take 157.6g BaCO
3, 68.51g MgO, 816g Al
2o
3, 35.2g Eu
2o
3, 34.5g MnCO
3, drop in blender and mix 24 hours;
2) High Temperature Pre burns till: by the material of mixing, loads crucible, and compression, pier are real, at 1650 DEG C, in atmospheric air, is incubated 5 hours;
3) hydrogen reduction: by the material coarse crushing of burning till, crosses 100 mesh sieves, more in small, broken bits, crosses 150 mesh sieves, uses H
2: N
2the reducing atmosphere of=7:3,1550 DEG C are incubated reduction 4 hours;
4) material of high temperature reduction is broken, cross 150 mesh sieves, by the powder after sieving, diameter be the glassie of 2 ~ 5mm and pure water by powder: ball: the mass ratio mixing of pure water=1:2:3, ball milling 1 hour, removes glassie, takes advantage of 500 mesh sieves that wet;
5) use the hot water cleaning twice of 60 ~ 80 DEG C, then clean 3 times with normal temperature pure water, the consumption of each water is 5 times of powder.
6) material after cleaning dries 24 hours in 200 DEG C after dewatering, crosses 200 mesh sieves, obtain product after drying.
For comparative example 2, wherein, the object that High Temperature Pre burns till is the generation in order to prevent dephasign two aluminate, and the temperature of pre-fired must be greater than 1600 DEG C.Temperature is more high better, but too high temperature easily causes body of heater to damage.High Temperature Pre burns till step and adopts fluxless solid reaction process, and for guaranteeing that solid reaction process is carried through to the end, the raw material in crucible compresses, pier is real, and in the feed between burrow.
Wherein, the object that last step (6) crosses 200 mesh sieves allows fluorescent material rub on screen cloth, and make powder produce the electrostatic of two like magnetic poles repel each other, such fluorescent tube factory is when using fluorescent material to size mixing, and fluorescent material can not be reunited, and film is even, and film quality is excellent.
In manufacture method of the present invention, during initial feed loading crucible, compression, pier are in fact, and get rid of the air in raw material as far as possible, be conducive to growing of crystal, make crystal more hard solid in pre-fired; The temperature of pre-fired is high, is conducive to the carrying out of solid state reaction, but too high temperature can damage body of heater.
After broken, material loads the material of crucible is pine dress, is conducive to the carrying out of reduction reaction.
Rubbed on screen cloth by fluorescent material when finally sieving, make powder produce the electrostatic of two like magnetic poles repel each other, such fluorescent material, when coating sized mixing by lamp processed, is easy to dispersion, not easily produces agglomeration, makes fluorescent tube be coated with uniformity.
For further illustrating the superiority of fluorescent material of the present invention and manufacture method thereof, comparative example and embodiment are analyzed.The data of this test, all have the ultraviolet-visible-near-infrared spectrum instrument (distant place PMS-50) generally used to obtain.
In order to contrast add different amount P, Eu, Ce, Tb on the impact of product brightness, the parameter that invention introduces fluorescent material relative luminous brightness (Br) and associated luminance (Br ') compares product.
The relative luminous brightness of usual fluorescent material is relevant to the chromaticity coordinates y value of this fluorescent material, and general y value is larger, and relative luminous brightness is higher, and different chemical constitutions and different manufacturing process obtain fluorescent material y value produce skew.Due to different y values, different relative brightnesses cannot be compared, and for obtaining normalized y value, is defined as follows for this reason: by the y value of the luminosity of fluorescent material divided by this fluorescent material, obtains a brightness relevant to y value and is referred to as associated luminance:
I.e. associated luminance Br '=relative brightness Br/y value.
Be the utilizing emitted light spectrogram of embodiment 15 shown in Fig. 1, its emission peak wavelength is the green glow of 515nm.On the basis of comparative example, P, Eu, Ce, Tb of adding different amount form each embodiment standard, and carry out luminescent properties detection, the results detailed in Table 1 to all samples.
Demonstrate the dependent luminescence intensity comparison diagram of embodiment 15 and comparative example 1 in Fig. 2, can find out, the emissive porwer of embodiment 15 is obviously greater than comparative example 1, and its luminous intensity performance significantly improves.
Fig. 3 is that the thermostability of fluorescent material at 600 DEG C and associated luminance maintain state graph.Can find out in figure, embodiment 15 shows good thermostability, and 600 DEG C of lasting insulations 60 minutes, test under normal temperature, its associated luminance almost seldom changed; Review comparative example 1,600 DEG C of lasting insulations 60 minutes, test under normal temperature, its associated luminance obviously dropped to less than 50%.
Following table 1 tests chemical constitution and the luminescent properties table thereof of each fluorescent material for this:
Comparative examples 1 and comparative example 2, final relative luminous brightness and associated luminance promote all to some extent, and visible manufacture method of the present invention is obviously better than common preparation method;
Comparative examples and embodiment, the luminescent properties of the fluorescent material of visible manufacture of the present invention is better than the common fluorescent material of comparative example;
Compare embodiment 3,4,5, P element atom content drops to 0.5 from 0.005, and relative luminous brightness and associated luminance significantly promote, wherein, associated luminance with 5% incremental lift, successful;
Comparative example 3,4,5 and embodiment 6,7,8, its difference is that rear three adds the Ce element of different amount, thus makes relative luminous brightness improve more than 5%, and associated luminance even promotes more than 9%, and within the scope of finite concentration, the concentration with Ce element increases and increases;
In like manner, comparative example 3,4,5 and embodiment 9,10,11, its difference is that rear three adds the Tb element of different amount, thus make relative luminous brightness improve more than 6%, associated luminance even promotes more than 10%, and within the scope of finite concentration, the concentration with Tb element increases and increases;
Contrast each embodiment, visible embodiment 15 is most preferred embodiments, adds Ce and Tb element simultaneously, and its associated luminance (Br ') bring up to 152%.
Test-results shows:
1) fluorescent material of manufacture of the present invention increases substantially the green emission intensity that emission peak wavelength is 515nm, and the associated luminance of most preferred embodiment brings up to more than 150%;
2) fluorescent material of manufacture of the present invention also increases substantially in 600 DEG C of thermostabilitys heated and associated luminance sustainment rate.
Claims (6)
1. rare earth, the coactivated aluminophosphates fluorescent material of manganese, it is characterized in that, the chemical constitution formula of described fluorescent material is:
Ba
1-a-bMg
2-cAl
16-xP
xO
27+x:Eu
a﹒M
b﹒Mn
c
In formula, M represents Ce and/or Tb;
Wherein, 0.1≤a≤0.3; 0.0001≤b≤0.001; 0.3 < c≤0.75; 0.005≤x≤0.5.
2. fluorescent material according to claim 1, is characterized in that, the chemical constitution formula of described fluorescent material is:
Ba
0.799Mg
1.7Al
15.5P
0.5O
27.5:Eu
0.2﹒Mn
0.3﹒Ce
0.0005﹒Tb
0.0005。
3. a method for the fluorescent material described in manufacturing claims 1, comprises the following steps:
1) batch mixing: according to the chemical constitution of fluorescent material of the present invention, take raw material, and it is fully mixed;
2) High Temperature Pre burns till: the raw material mixed is loaded crucible, and temperature controls at 1600 DEG C ~ 1650 DEG C, is incubated 2 ~ 5 hours;
3) hydrogen reduction: the material of pre-fired is broken, in small, broken bits, sieve, load crucible, guarantees that in reducing atmosphere temperature controls at 1450 DEG C ~ 1550 DEG C, insulation reductase 12 ~ 4 hour;
4) broken aftertreatment: by broken for the material after reduction, sieve, ball milling, cleaning, wetly to sieve, dry, namely sieve obtains product of the present invention;
Wherein, described raw material is selected from BaCO
3, MgO, Al
2o
3, (NH
4)
2hPO
4, Eu
2o
3, MnCO
3, CeO and Tb
4o
7.
4. method according to claim 3, is characterized in that, High Temperature Pre burns till step and adopts fluxless solid reaction process, and the raw material in crucible compresses, pier is real, and in the feed between burrow.
5. method according to claim 3, is characterized in that, in hydrogen reduction step, material loads the mode of crucible is pine dress.
6. according to any one method described in claim 3-5, it is characterized in that, the ball milling in broken post-processing step, adopt glassie to carry out wet ball mill.
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JP2010192254A (en) * | 2009-02-18 | 2010-09-02 | Nec Lighting Ltd | Cold-cathode fluorescent lamp, and aluminate-based phosphor |
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