CN104130778B - superfine fluorescent powder preparation method - Google Patents
superfine fluorescent powder preparation method Download PDFInfo
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- CN104130778B CN104130778B CN201410374048.9A CN201410374048A CN104130778B CN 104130778 B CN104130778 B CN 104130778B CN 201410374048 A CN201410374048 A CN 201410374048A CN 104130778 B CN104130778 B CN 104130778B
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Abstract
The present invention relates to a kind of fluorescent material preparation method, be specially superfine fluorescent powder preparation method, raw material is Y
2o
3and Eu
2o
3, add BaCl
2and H
3bO
3as fusing assistant, by raw material high-temperature calcination, break process, pulverizing, cleaning, coating, sieve after powder slurry carry out centrifuge dehydration, dry can obtain superfine fluorescent powder.Superfine fluorescent powder preparation method provided by the invention, adopts high temperature solid-state method, and equipment is simple, and running cost is low, and synthesis cycle is short, without the need to the material using strong acid, alkoxide etc. harmful.At employing Al
2o
3or SiO
2after carrying out coating, avoid the secondary agglomeration of fluorescent material, and reach the effect of repairing plane of crystal defect, thus obtain that decay is little, brightness is high, the superfine fluorescent powder of good dispersity.
Description
Technical field
The present invention relates to a kind of fluorescent material preparation method, be specially superfine fluorescent powder preparation method.
Background technology
Superfine fluorescent powder refers to the fluorescent material near nanometer-submicron-scale, is that a class has the fluorescent material of important application prospect in display and lighting field.Because the physical influence such as quantum confined effect, small-size effect, surface state effect of nanometer-submicron particle itself affects, this kind of fluorescent material is had in physics, photochemistry etc. many peculiar and have the characteristic of using value.Conventional commercial fluorescent material is all micropowder, and on this basis, it is thinner that conventional commercial micropowder is done by the method be suitable for industry, and improve coating rate, and do not affect luminescent properties, the application for conventional fluorescent powder is significant.
The preparation method of the superfine fluorescent powder of current report mainly contains sol-gel method, combustion method, hydrothermal method, homogeneous precipitation method etc., all needs to use strong acid that material dissolution is become solution state, makes presoma, then calcine after adopting means such as regulating pH.These methods all need to use specific equipment, and operation is loaded down with trivial details, and technical difficulty is large, and cost is high, if matrix remains, then can reduce luminous intensity, strong acid, alkoxide etc. are also harmful to human body, and poor stability is unsuitable for scale operation.
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of technique simply, do not use the ultrafine powder production method of the objectionable impuritiess such as strong acid, concrete technical scheme is:
Superfine fluorescent powder preparation method, comprises the following steps:
(1) raw material is, medium particle diameter is the Y of 4-5 μm
2o
3and Eu
2o
3, mass ratio Y
2o
3: Eu
2o
3=100:5 ~ 8; First the half of raw material is dropped in mixing tank, add the BaCl of raw materials quality than 0.4-0.6%
2with the H of mass ratio 0.05%-0.1%
3bO
3as fusing assistant, then drop into remaining raw material, carry out batch mixing 20-40 hour;
(2) raw material mixed is loaded in crucible, be compacted into muffin, and get circular hole in the middle of the muffin compressed, muffin is heated evenly, adds a cover and carry out high-temperature calcination, at 1200-1350 DEG C, be incubated 5-7 hour;
(3) after calcining, fully cool, take out muffin and carry out break process;
(4) powder after sieving carries out airflow milling, and intake pressure is 0.5-1KPa, and pulverizing pressure is 0.2-0.6KPa;
(5) powder after airflow milling is added clear water to clean;
(6) the powder slurry after cleaning, adds the 0.02%-0.05% nanometer Al of raw materials quality ratio
2o
3or SiO
2, stir 10-15 minute, carry out coating;
(7) the powder slurry after coating is carried out wet sieving, sieve number is 300-400 order;
(8) the powder slurry after wet sieving is carried out centrifuge dehydration;
(9) powder after centrifuge dehydration puts into baking oven, toasts 12-18 hour at 110-150 DEG C;
(10) powder after drying sieves, and sieve number is 80-150 order, can obtain superfine fluorescent powder.
Batch mixing described in step (1), adds rigid plastic balls at mixing tank, and every 500 kilograms of raw materials add 20 baton rounds, each baton round diameter 6cm, with the rotating speed batch mixing 20-40 hour of 10-20 rev/min.
Break process described in step (3), muffin is dropped into jaw crusher, carry out one time slightly to break, the powder input roller spacing after slightly breaking is that the roller crusher of 15-25 silk carries out twice thin broken, is finally sieved through 100 order sieving machines by the powder of fragmentation.
Cleaning described in step (5), method is, in powder weight: the ratio of the volume=1Kg:1 ~ 1.5L of water puts into cleaning barrels, first time cleaning water temperature >40 DEG C, stirred after 10-15 minute, powder is made to starch natural sedimentation, extract supernatant liquid to 3-8cm place, powder slurry top, second time cleaning water temperature >60 DEG C, stirred after 10-15 minute, make powder starch natural sedimentation, extract supernatant liquid to 3-8cm place, powder slurry top.
Three metafiltration cloth bags are put into whizzer bucket by the centrifuge dehydration described in step (8), start rotation and within one minute, make filter cloth bag be adjacent to a barrel wall, then it is centrifugal to dehydration to put into powder slurry.
Superfine fluorescent powder preparation method provided by the invention, adopts high temperature solid-state method, and equipment is simple, and running cost is low, and synthesis cycle is short, without the need to the material using strong acid, alkoxide etc. harmful, is suitable for industrial mass production.Crystal mass prepared by high temperature solid-state method is excellent, few surface defects, and luminous efficiency is high, at employing Al
2o
3or SiO
2after carrying out coating, avoid the secondary agglomeration of fluorescent material, and reach the effect of repairing plane of crystal defect, thus obtain that decay is little, brightness is high, the superfine fluorescent powder of good dispersity.The particle diameter of the superfine fluorescent powder of system is between 2-5 μm, and this superfine fluorescent powder has better upper lamp rate compared to common oarse-grained fluorescent material, and for T8 pipe, average saving powder about 30%, improves the utilization ratio of resource.
Figure of description
Fig. 1 is the SEM figure of embodiment 2 gained superfine fluorescent powder;
Fig. 2 commonly uses the SEM figure of red fluorescence powder;
The spectrum comparison diagram of Fig. 3 embodiment 2 and conventional red fluorescence powder.
Embodiment
The specific embodiment of the present invention is described in conjunction with the embodiments.
Embodiment 1
(1) raw material is, medium particle diameter is the Y of 4-5 μm
2o
3and Eu
2o
3, mass ratio Y
2o
3: Eu
2o
3=100:5; First the half of raw material is dropped in mixing tank, add the BaCl of raw materials quality than 0.6%
2with the H of mass ratio 0.08%
3bO
3as fusing assistant, then drop into remaining raw material, and add rigid plastic balls, with the rotating speed batch mixing 30 hours of 10 revs/min.
(2) raw material mixed is loaded in crucible, be compacted into muffin, and get circular hole in the middle of the muffin compressed, muffin is heated evenly, adds a cover and carry out high-temperature calcination, at 1300 DEG C, be incubated 5 hours.
(3) after calcining, fully cool, take out muffin and carry out break process; Muffin is dropped into jaw crusher, carries out one time and slightly break, the powder input roller spacing after slightly breaking is that the roller crusher of 15 carries out twice thin broken, is finally sieved through 100 order sieving machines by the powder of fragmentation.
(4) powder after sieving carries out airflow milling, and intake pressure is 0.5KPa, and pulverizing pressure is 0.2KPa.
(5) powder after airflow milling is added clear water to clean; In powder weight: the ratio of the volume=1Kg:1L of water puts into cleaning barrels, first time cleaning water temperature 50 DEG C, stir after 10 minutes, powder is made to starch natural sedimentation, extract supernatant liquid to 3cm place, powder slurry top, second time cleaning water temperature 70 DEG C, stirred after 15 minutes, make powder starch natural sedimentation, extract supernatant liquid to 3cm place, powder slurry top.
(6) the powder slurry after cleaning, adds 0.02% nanometer Al of raw materials quality ratio
2o
3, stir 10 minutes, carry out coating.
(7) the powder slurry after coating is carried out wet sieving, sieve number is 300 orders.
(8) the powder slurry after wet sieving is carried out centrifuge dehydration; Three metafiltration cloth bags are put into whizzer bucket, starts rotation and within one minute, make filter cloth bag be adjacent to a barrel wall, then it is centrifugal to dehydration to put into powder slurry.
(9) powder after centrifuge dehydration puts into baking oven, toasts 12 hours at 110 DEG C.
(10) powder after drying sieves, and sieve number is 80 orders, can obtain superfine fluorescent powder.
Embodiment 2
(1) raw material is, medium particle diameter is the Y of 4-5 μm
2o
3and Eu
2o
3, mass ratio Y
2o
3: Eu
2o
3the half of=100:5.8 raw material drops in mixing tank, adds the BaCl of raw materials quality than 0.5%
2with the H of mass ratio 0.08%
3bO
3as fusing assistant, then drop into remaining raw material, and add rigid plastic balls, with the rotating speed batch mixing 24 hours of 15 revs/min.
(2) raw material mixed is loaded in crucible, be compacted into muffin, and get circular hole in the middle of the muffin compressed, muffin is heated evenly, adds a cover and carry out high-temperature calcination, at 1280 DEG C, be incubated 6 hours.
(3) after calcining, fully cool, take out muffin and carry out break process; Muffin is dropped into jaw crusher, carries out one time and slightly break, the powder input roller spacing after slightly breaking is that the roller crusher of 20 carries out twice thin broken, is finally sieved through 100 order sieving machines by the powder of fragmentation.
(4) powder after sieving carries out airflow milling, and intake pressure is 0.8KPa, and pulverizing pressure is 0.4KPa.
(5) powder after airflow milling is added clear water to clean; In powder weight: the ratio of the volume=1Kg:1.2L of water puts into cleaning barrels, first time cleaning water temperature 50 DEG C, stir after 15 minutes, powder is made to starch natural sedimentation, extract supernatant liquid to 5cm place, powder slurry top, second time cleaning water temperature 80 DEG C, stirred after 15 minutes, make powder starch natural sedimentation, extract supernatant liquid to 5cm place, powder slurry top.
(6) the powder slurry after cleaning, adds 0.03% nanometer Al of raw materials quality ratio
2o
3, stir 15 minutes, carry out coating.
(7) the powder slurry after coating is carried out wet sieving, sieve number is 380 orders.
(8) the powder slurry after wet sieving is carried out centrifuge dehydration; Three metafiltration cloth bags are put into whizzer bucket, starts rotation and within one minute, make filter cloth bag be adjacent to a barrel wall, then it is centrifugal to dehydration to put into powder slurry.
(9) powder after centrifuge dehydration puts into baking oven, toasts 17 hours at 130 DEG C.
(10) powder after drying sieves, and sieve number is 100 orders, can obtain superfine fluorescent powder.
The superfine fluorescent powder of the present embodiment gained carries out SEM detection with conventional red fluorescence powder performance, as Fig. 1 and Fig. 2, and the superfine fluorescent powder of embodiment 2 gained and the spectrum of conventional red fluorescence powder are compared, as Fig. 3, result shows, the superfine fluorescent powder particle diameter of embodiment 2 is less, but substantially the same with the luminescent spectrum of conventional red fluorescence powder.
Embodiment 3
(1) raw material is, medium particle diameter is the Y of 4-5 μm
2o
3and Eu
2o
3, mass ratio Y
2o
3: Eu
2o
3the half of=100:6.8 raw material drops in mixing tank, adds the BaCl of raw materials quality than 0.4%
2with the H of mass ratio 0.1%
3bO
3as fusing assistant, then drop into remaining raw material, and add rigid plastic balls, with the rotating speed batch mixing 20 hours of 20 revs/min.
(2) raw material mixed is loaded in crucible, be compacted into muffin, and get circular hole in the middle of the muffin compressed, muffin is heated evenly, adds a cover and carry out high-temperature calcination, at 1350 DEG C, be incubated 6 hours.
(3) after calcining, fully cool, take out muffin and carry out break process; Muffin is dropped into jaw crusher, carries out one time and slightly break, the powder input roller spacing after slightly breaking is that the roller crusher of 25 carries out twice thin broken, is finally sieved through 100 order sieving machines by the powder of fragmentation.
(4) powder after sieving carries out airflow milling, and intake pressure is 0.8KPa, and pulverizing pressure is 0.4KPa.
(5) powder after airflow milling is added clear water to clean; In powder weight: the ratio of the volume=1Kg:1.4L of water puts into cleaning barrels, first time cleaning water temperature 60 DEG C, stir after 15 minutes, powder is made to starch natural sedimentation, extract supernatant liquid to 5cm place, powder slurry top, second time cleaning water temperature 80 DEG C, stirred after 10 minutes, make powder starch natural sedimentation, extract supernatant liquid to 8cm place, powder slurry top.
(6) the powder slurry after cleaning, adds 0.03% Nano-meter SiO_2 of raw materials quality ratio
2, stir 12 minutes, carry out coating.
(7) the powder slurry after coating is carried out wet sieving, sieve number is 300 orders.
(8) the powder slurry after wet sieving is carried out centrifuge dehydration; Three metafiltration cloth bags are put into whizzer bucket, starts rotation and within one minute, make filter cloth bag be adjacent to a barrel wall, then it is centrifugal to dehydration to put into powder slurry.
(9) powder after centrifuge dehydration puts into baking oven, toasts 18 hours at 140 DEG C.
(10) powder after drying sieves, and sieve number is 100 orders, can obtain superfine fluorescent powder.
(9) powder after step (8) being dried finally goes over sieve, and sieve number is 100 orders, can obtain target superfine fluorescent powder.
Embodiment 4
(1) raw material is, medium particle diameter is the Y of 4-5 μm
2o
3and Eu
2o
3, mass ratio Y
2o
3: Eu
2o
3the half of=100:8 raw material drops in mixing tank, adds the BaCl of raw materials quality than 0.6%
2with the H of mass ratio 0.05%
3bO
3as fusing assistant, then drop into remaining raw material, and add rigid plastic balls, with the rotating speed batch mixing 40 hours of 15 revs/min.
(2) raw material mixed is loaded in crucible, be compacted into muffin, and get circular hole in the middle of the muffin compressed, muffin is heated evenly, adds a cover and carry out high-temperature calcination, at 1200 DEG C, be incubated 7 hours.
(3) after calcining, fully cool, take out muffin and carry out break process; Muffin is dropped into jaw crusher, carries out one time and slightly break, the powder input roller spacing after slightly breaking is that the roller crusher of 20 carries out twice thin broken, is finally sieved through 100 order sieving machines by the powder of fragmentation.
(4) powder after sieving carries out airflow milling, and intake pressure is 1KPa, and pulverizing pressure is 0.6KPa.
(5) powder after airflow milling is added clear water to clean; In powder weight: the ratio of the volume=1Kg:1.5L of water puts into cleaning barrels, first time cleaning water temperature 60 DEG C, stir after 10 minutes, powder is made to starch natural sedimentation, extract supernatant liquid to 8cm place, powder slurry top, second time cleaning water temperature 80 DEG C, stirred after 10 minutes, make powder starch natural sedimentation, extract supernatant liquid to 5cm place, powder slurry top.
(6) the powder slurry after cleaning, adds 0.05% nanometer Al of raw materials quality ratio
2o
3, stir 15 minutes, carry out coating.
(7) the powder slurry after coating is carried out wet sieving, sieve number is 350 orders.
(8) the powder slurry after wet sieving is carried out centrifuge dehydration; Three metafiltration cloth bags are put into whizzer bucket, starts rotation and within one minute, make filter cloth bag be adjacent to a barrel wall, then it is centrifugal to dehydration to put into powder slurry.
(9) powder after centrifuge dehydration puts into baking oven, toasts 15 hours at 150 DEG C.
(10) powder after drying sieves, and sieve number is 150 orders, can obtain superfine fluorescent powder.
By embodiment product detect with conventional red fluorescence powder performance, the results are shown in Table 1:
Table 1: the Performance comparision of embodiment and conventional rouge and powder
According to upper table, visible, the superfine fluorescent powder particle diameter of embodiment gained is less, but relative brightness is suitable with conventional red fluorescence powder.
Claims (5)
1. superfine fluorescent powder preparation method, is characterized in that: comprise the following steps,
(1) raw material is, medium particle diameter is the Y of 4-5 μm
2o
3and Eu
2o
3, mass ratio Y
2o
3: Eu
2o
3=100:5 ~ 8; First the half of raw material is dropped in mixing tank, add the BaCl of raw materials quality than 0.4-0.6%
2with the H of mass ratio 0.05%-0.1%
3bO
3as fusing assistant, then drop into remaining raw material, carry out batch mixing 20-40 hour;
(2) raw material mixed is loaded in crucible, be compacted into muffin, and get circular hole in the middle of the muffin compressed, muffin is heated evenly, adds a cover and carry out high-temperature calcination, at 1200-1350 DEG C, be incubated 5-7 hour;
(3) after calcining, fully cool, take out muffin and carry out break process;
(4) powder after sieving carries out airflow milling, and intake pressure is 0.5-1KPa, and pulverizing pressure is 0.2-0.6KPa;
(5) powder after airflow milling is added clear water to clean;
(6) the powder slurry after cleaning, adds the 0.02%-0.05% nanometer Al of raw materials quality ratio
2o
3or SiO
2, stir 10-15 minute, carry out coating;
(7) the powder slurry after coating is carried out wet sieving, sieve number is 300-400 order;
(8) the powder slurry after wet sieving is carried out centrifuge dehydration;
(9) powder after centrifuge dehydration puts into baking oven, toasts 12-18 hour at 110-150 DEG C;
(10) powder after drying sieves, and sieve number is 80-150 order, can obtain superfine fluorescent powder.
2. superfine fluorescent powder preparation method according to claim 1, it is characterized in that: the batch mixing described in step (1), adds rigid plastic balls at mixing tank, every 500 kilograms of raw materials add 20 baton rounds, each baton round diameter 6cm, with the rotating speed batch mixing 20-40 hour of 10-20 rev/min.
3. superfine fluorescent powder preparation method according to claim 1, it is characterized in that: the break process described in step (3), muffin is dropped into jaw crusher, carry out one time slightly to break, powder input roller spacing after slightly breaking is that the roller crusher of 15-25 silk carries out twice thin broken, is finally sieved through 100 order sieving machines by the powder of fragmentation.
4. superfine fluorescent powder preparation method according to claim 1, it is characterized in that: the cleaning described in step (5), method is, in powder weight: the ratio of the volume=1Kg:1 ~ 1.5L of water puts into cleaning barrels, first time cleaning water temperature >40 DEG C, stir after 10-15 minute, powder is made to starch natural sedimentation, extract supernatant liquid to 3-8cm place, powder slurry top, second time cleaning water temperature >60 DEG C, stir after 10-15 minute, make powder starch natural sedimentation, extract supernatant liquid to 3-8cm place, powder slurry top.
5. superfine fluorescent powder preparation method according to claim 1, it is characterized in that: the centrifuge dehydration described in step (8), three metafiltration cloth bags are put into whizzer bucket, starts rotation and within one minute, make filter cloth bag be adjacent to a barrel wall, then it is centrifugal to dehydration to put into powder slurry.
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| CN107118759B (en) * | 2017-05-23 | 2020-04-10 | 苏州中科纳福材料科技有限公司 | Anti-hardening special-shaped composite luminescent powder and preparation method thereof |
| CN108755161A (en) * | 2018-07-05 | 2018-11-06 | 佛山市衣香蒂丝服装设计有限公司 | A kind of manufacturing method of fluorescent fabric |
| CN108914604A (en) * | 2018-07-05 | 2018-11-30 | 佛山市衣香蒂丝服装设计有限公司 | A kind of fluorescent fabric |
| WO2020100574A1 (en) * | 2018-11-12 | 2020-05-22 | デンカ株式会社 | Package for accommodating fluorescent substance, and container box |
| CN110644897A (en) * | 2019-08-16 | 2020-01-03 | 浙江金凯门业有限责任公司 | Self-luminous indoor door |
| CN111334281B (en) * | 2020-03-06 | 2023-07-04 | 英特美光电（苏州）有限公司 | Preparation method of composite coated yellow fluorescent powder special for COB |
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