CN110467913A - A kind of method for coating of big granularity LED fluorescent powder - Google Patents

A kind of method for coating of big granularity LED fluorescent powder Download PDF

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CN110467913A
CN110467913A CN201910668197.9A CN201910668197A CN110467913A CN 110467913 A CN110467913 A CN 110467913A CN 201910668197 A CN201910668197 A CN 201910668197A CN 110467913 A CN110467913 A CN 110467913A
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fluorescent powder
silica gel
coating
big granularity
solution
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CN110467913B (en
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贾国秀
周卫新
顾竟涛
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Intel American Photoelectric (suzhou) Co Ltd
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Intel American Photoelectric (suzhou) Co Ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02Use of particular materials as binders, particle coatings or suspension media therefor
    • C09K11/025Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7774Aluminates
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/7792Aluminates
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50Wavelength conversion elements
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008Processes
    • H01L2933/0033Processes relating to semiconductor body packages
    • H01L2933/0041Processes relating to semiconductor body packages relating to wavelength conversion elements

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

The present invention relates to a kind of method for coating of big granularity LED fluorescent powder, it goes after acid solution clean fluorescent powder with hot water multiple the following steps are included: (a) uses acid soak fluorescent powder, until cleaning solution conductivity < 5mS/cm, dries to obtain and handles fluorescent powder;(b) the first silica gel, the second silica gel are dissolved in respectively in organic solvent and form the first silica gel solution, the second silica gel solution;By the first silica gel, the second silica gel, 1:2.8 ~ 3.2 carry out mixing to obtain covering liquid by volume;First silica gel and second silica gel can cooperate solidification, and its refractive index is independently of each other >=1.54;(c) under conditions of being stirred continuously, the processing fluorescent powder is added in Xiang Suoshu covering liquid, filter residue is dried after suction filtration, is solidified.So that generating the active force that identical charges repel each other between fluorescent powder and encapsulation silica gel, reducing fluorescent powder reduces speed;So that clad and fluorescent powder form an entirety, to reduce the density of whole fluorescent powder.

Description

A kind of method for coating of big granularity LED fluorescent powder
Technical field
The invention belongs to LED fluorescent powder technical fields, and in particular to a kind of method for coating of big granularity LED fluorescent powder.
Background technique
With the development of LED illumination industry, the maximum contention point of the light efficiency of LED light source and service life as each manufacturer, Since 20 world end white light LEDs inventions, the light efficiency of white light LEDs was realized the breakthrough of 100 lm/w in 2006 by day Asia chemical industry; By 2008 (after short 2 years), Cree company, the U.S. just realized the white light of 157lm/w in laboratory;Then, each LED light Source manufacturer competes with one another, the important characterization of the light efficiency of light source and service life as source mass.It up to the present, in the market can be real The manufacturer of existing 200lm/w is also not within minority.
The light efficiency of LED light source depends primarily on two factors: first is that blue chip, second is that fluorescent powder.And fluorescent powder conduct The granularity of a kind of powder crystal, crystallinity and crystal determines the light emission luminance of powder, and crystallinity is better, and the particle of crystal is got over Greatly, the light emission luminance of fluorescent powder is bigger, and in the led, the light efficiency of LRED light source also can be higher for encapsulation, but the fluorescent powder of big granularity exists It is too fast that sedimentation is often had in LED package application, the problem of so as to cause aperture.Especially some density of material it is big shine it is glimmering Light powder, such as Luetcium aluminum garnet, and Luetcium aluminum garnet is to apply in high-power LED light source, green portions are essential high-quality Luminescent material.The settlement issues for how solving such material, at the luminous one important technological difficulties of industry of LED fluorescent powder.
Summary of the invention
A kind of cladding side of big granularity LED fluorescent powder is provided the invention aims to overcome the deficiencies in the prior art Method.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of method for coating of big granularity LED fluorescent powder, It the following steps are included:
(a) use acid soak fluorescent powder, go after acid solution clean fluorescent powder with hot water it is multiple, up to cleaning solution conductivity < 5mS/ Cm dries to obtain processing fluorescent powder;
(b) the first silica gel, the second silica gel are dissolved in respectively in organic solvent and form the first silica gel solution, the second silica gel solution;It will 1:2.8 ~ 3.2 carry out mixing to obtain covering liquid by volume for first silica gel, the second silica gel;First silica gel and second silica gel Solidification can be cooperated, and its refractive index is independently of each other >=1.54;
(c) under conditions of being stirred continuously, the processing fluorescent powder is added in Xiang Suoshu covering liquid, dries filter residue after suction filtration Dry, solidification.
Optimally, in step (a), the acid solution is the hydrochloric acid solution that mass concentration is 5 ~ 15%.
Further, in step (a), fluorescent powder first is cleaned repeatedly to cleaning solution conductivity≤10mS/cm, enriching with hot water Degree is neutralized to neutrality for 5% ammonia spirit, and reusable heat water cleaning fluorescent powder repeatedly arrives electrical conductivity of solution < 5mS/cm.
Optimally, in step (b), first silica gel, second silica gel be respectively DOW CORNING OE-6650A, DOW CORNING OE-6650B。
Further, in step (b), first silica gel, second silica gel volume ratio be 1:3.
Optimally, in step (c), concentration≤0.5 g/ml of the processing fluorescent powder in the covering liquid.
Further, in step (c), the temperature of the drying is 120 ~ 160 DEG C.
Due to the above technical solutions, the present invention has the following advantages over the prior art: the big granularity LED of the present invention The method for coating of fluorescent powder coats the first silica gel and the second silica gel of high refractive index by the phosphor surface crossed in surface clean To be solidified, the surface property (such as surface polarity and surface tension) of phosphor powder crystal can be changed in this way, so that glimmering The active force that identical charges repel each other is generated between light powder and encapsulation silica gel, reducing fluorescent powder reduces speed;And in phosphor surface packet One layer of organic layer is covered, so that clad and fluorescent powder form an entirety, to reduce the density of whole fluorescent powder.
Detailed description of the invention
Fig. 1 is the using effect schematic diagram of existing big granularity LED fluorescent powder.
Fig. 2 is the using effect schematic diagram of the method for coating of the big granularity LED fluorescent powder of the present invention.
Specific embodiment
The method for coating of the big granularity LED fluorescent powder of the present invention, it is the following steps are included: (a) uses acid soak fluorescent powder, Go after acid solution to clean fluorescent powder with hot water it is multiple, until cleaning solution conductivity < 5mS/cm, dries to obtain processing fluorescent powder;(b) by One silica gel, the second silica gel, which are dissolved in respectively in organic solvent, forms the first silica gel solution, the second silica gel solution;By the first silica gel, 1:2.8 ~ 3.2 carry out mixing to obtain covering liquid second silica gel by volume;First silica gel and second silica gel can cooperate solidification, And its refractive index is independently of each other >=1.54;(c) under conditions of being stirred continuously, it is glimmering that the processing is added in Xiang Suoshu covering liquid Filter residue is dried after suction filtration, is solidified by light powder.High refractive index is coated by the phosphor surface crossed in surface clean First silica gel and the second silica gel can change surface property (such as surface polarity of phosphor powder crystal to be solidified in this way And surface tension), so that generating the active force that identical charges repel each other between fluorescent powder and encapsulation silica gel, reducing fluorescent powder reduces speed; And coat one layer of organic layer in phosphor surface so that clad and fluorescent powder form an entirety, thus reduce whole it is glimmering The density of light powder.Above-mentioned fluorescent powder is usually Y3Al5O12: Ce, Lu3Al5O12: Ce or CaAlSiN3: Eu
Above-mentioned method for coating can not only solve the settlement issues of big granularity, high density luminescent material, while can also reduce LED Big granularity, the dosage of high density phosphor material powder (i.e. so that fluorescent powder has good dispersion performance, while increasing again in encapsulation Granularity, the anti-settling of high density fluorescent powder are increased, (LED principle of luminosity is exactly thus under the premise of not influencing LED light source light efficiency The blue light that blue light crystal issues is divided into two parts, and a part meeting excitated red fluorescent powder and green emitting phosphor issue feux rouges and green light, The feux rouges and green light that another part blue light will be issued with fluorescent powder are compound with the principle of three primary colours, issue white light), reduce big granularity The usage amount of high density fluorescent powder).This is because: being with green Luetcium aluminum garnet fluorescent powder (industry abbreviation Gal or LuAG) Example, as depicted in figs. 1 and 2, when fluorescent powder does not have anti-settling layer (i.e. uncoated), the fluorescent powder grain rate of settling is very Fastly, before silica gel is fully cured, fluorescent powder is more deposited in bottom, and the blue light that on the one hand can be issued to chip blocks work With the green light on the other hand issued can be more by red light absorption, that is to say, that, it should the luminous blue light of excitated red fluorescent powder It is at least partially obscured loss, red fluorescence powder transfers to absorb the light of green emitting phosphor, and (absorption spectra of red fluorescence powder is comprising green light Wide range), to increase the dosage of green emitting phosphor.
In step (a), the acid solution is usually the hydrochloric acid solution that mass concentration is 5 ~ 15%.In step (a), hot water is first used Fluorescent powder is cleaned repeatedly to cleaning solution conductivity≤10mS/cm, and adding concentration is that 5% ammonia spirit is neutralized to neutrality, reusable heat water Cleaning fluorescent powder repeatedly arrives electrical conductivity of solution < 5mS/cm.In step (b), first silica gel, second silica gel difference are preferred For DOW CORNING OE-6650A, DOW CORNING OE-6650B;The volume ratio of first silica gel, second silica gel Optimal is 1:3.In step (c), concentration≤0.5 g/ml of the processing fluorescent powder in the covering liquid.In step (c), institute The temperature for stating drying is 120 ~ 160 DEG C.
It is described in detail below in conjunction with to the preferred embodiment of the invention:
Embodiment 1
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it the following steps are included:
(a) surface cleaning of fluorescent powder: fluorescent powder (Y is impregnated with the hydrochloric acid solution that mass concentration is 10%3Al5O12: Ce fluorescent powder, Granularity D50 is respectively 18 μm) half an hour, it is stirred for half an hour, stands after fluorescent powder precipitates completely, removes hydrochloric acid solution;With 80 ~ 100 DEG C of hot water cleaning is multiple, until conductivity < 10mS/cm of solution;The ammonia spirit that a small amount of concentration is 5% is added to neutralize To neutrality, pH=7 are tested;Continue to be cleaned with 80 ~ 100 DEG C of hot water repeatedly, until electrical conductivity of solution < 5mS/cm;After precipitating 3h is dried in 120 DEG C of baking oven must handle fluorescent powder;
(b) mixing of covering liquid (i.e. coating liquid): the coated fertilizer of selection is high refractive index AB silica gel, is DOW CORNING The first silica gel of OE-6650A() and the second silica gel of DOW CORNING OE-6650B();500ml second is added in the first silica gel of 1ml Alcohol forms the first silica gel solution, and 500ml ethyl alcohol is added in the second silica gel of 1ml and forms the second silica gel solution, is taken with the volume ratio of 1:3 Above two silica gel solution, which is placed in beaker, to be mixed, and stirring half an hour obtains covering liquid;
(c) 50g processing fluorescent powder (noticing that fluorescent powder is slowly spilt into covering liquid) is added into 100ml covering liquid, stirring half is small When;Filter residue (i.e. fluorescent powder) is dried to 3 hours (solidification for promoting AB silica gel) at 150 DEG C after suction filtration.
Fluorescent powder after above-mentioned cladding is packaged with uncoated fluorescent powder, in the condition of same LED light source light efficiency Under, the percentage that the fluorescent powder usage amount (usage amount relative to uncoated fluorescent powder) after cladding reduces is 4%.
Embodiment 2
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, it is different Be: in step (a), the MODEL OF THE PHOSPHOR PARTICLE SIZE D50 used is 23 μm, and the percentage that the fluorescent powder usage amount after final cladding reduces is 5%。
Embodiment 3
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, it is different Be: in step (a), the MODEL OF THE PHOSPHOR PARTICLE SIZE D50 used is 30 μm, and the percentage that the fluorescent powder usage amount after final cladding reduces is 6%。
Embodiment 4
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, it is different Be: in step (a), the fluorescent powder used is Lu3Al5O12: Ce, the percentage that finally the fluorescent powder usage amount after cladding reduces are 3%。
Embodiment 5
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 4, it is different Be: in step (a), the MODEL OF THE PHOSPHOR PARTICLE SIZE D50 used is 20 μm, and the percentage that the fluorescent powder usage amount after final cladding reduces is 5%。
Embodiment 6
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 4, it is different Be: in step (a), the MODEL OF THE PHOSPHOR PARTICLE SIZE D50 used is 25 μm, and the percentage that the fluorescent powder usage amount after final cladding reduces is 6%。
Embodiment 7
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, it is different Be: in step (a), the fluorescent powder used is CaAlSiN3: Eu, the percentage that finally the fluorescent powder usage amount after cladding reduces are 2.5%。
Embodiment 8
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 7, it is different Be: in step (a), the MODEL OF THE PHOSPHOR PARTICLE SIZE D50 used is 22 μm, and the percentage that the fluorescent powder usage amount after final cladding reduces is 4%。
Embodiment 9
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 7, it is different Be: in step (a), the MODEL OF THE PHOSPHOR PARTICLE SIZE D50 used is 26 μm, and the percentage that the fluorescent powder usage amount after final cladding reduces is 5%。
Embodiment 10
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, it is different It is: in step (c), 10g processing fluorescent powder is only added into 100ml covering liquid;Fluorescent powder usage amount after final cladding reduces Percentage be 3.5%.
Embodiment 11
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, it is different It is: in step (b), two kinds of silica gel solutions is taken with the volume ratio of 1:2.8;The percentage that fluorescent powder usage amount after final cladding reduces Than being 3.9%.
Embodiment 12
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, it is different It is: in step (b), two kinds of silica gel solutions is taken with the volume ratio of 1:3.2;The percentage that fluorescent powder usage amount after final cladding reduces Than being 4.1%.
Embodiment 13
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, it is different It is: in step (b), the first silica gel of 2ml, the second silica gel is separately added into 500ml ethyl alcohol and form corresponding silica gel solution, it is final to wrap The percentage that fluorescent powder usage amount after covering reduces is 4.2%.
Embodiment 14
The present embodiment provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, it is different It is: in step (b), the first silica gel of 3ml, the second silica gel is separately added into 500ml ethyl alcohol and form corresponding silica gel solution, it is final to wrap The percentage that fluorescent powder usage amount after covering reduces is 4.5%.
Comparative example 1
This example provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, unlike: not It carries out step (a), the percentage that the fluorescent powder usage amount after final cladding reduces is 1%.
Comparative example 2
This example provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, unlike: not It carries out step (a), does not ammoniate aqueous solution to neutrality, also do not make electrical conductivity of solution < 5mS/cm, the fluorescent powder after final cladding makes The percentage that dosage reduces is 1.5%.
Comparative example 3
This example provides a kind of method for coating of big granularity LED fluorescent powder, it with it is almost the same in embodiment 1, unlike: step Suddenly in (c), processing fluorescent powder is excessive, reaches 60g, and the percentage that the fluorescent powder usage amount after final cladding reduces is 2.0%.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention, it is all according to the present invention Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.

Claims (7)

1. a kind of method for coating of big granularity LED fluorescent powder, which is characterized in that it the following steps are included:
(a) use acid soak fluorescent powder, go after acid solution clean fluorescent powder with hot water it is multiple, up to cleaning solution conductivity < 5mS/ Cm dries to obtain processing fluorescent powder;
(b) the first silica gel, the second silica gel are dissolved in respectively in organic solvent and form the first silica gel solution, the second silica gel solution;It will 1:2.8 ~ 3.2 carry out mixing to obtain covering liquid by volume for first silica gel, the second silica gel;First silica gel and second silica gel Solidification can be cooperated, and its refractive index is independently of each other >=1.54;
(c) under conditions of being stirred continuously, the processing fluorescent powder is added in Xiang Suoshu covering liquid, dries filter residue after suction filtration Dry, solidification.
2. the method for coating of big granularity LED fluorescent powder according to claim 1, it is characterised in that: in step (a), the acid Liquid is the hydrochloric acid solution that mass concentration is 5 ~ 15%.
3. the method for coating of big granularity LED fluorescent powder according to claim 1 or claim 2, it is characterised in that: in step (a), first use Hot water cleans fluorescent powder repeatedly to cleaning solution conductivity≤10mS/cm, and adding concentration is that 5% ammonia spirit is neutralized to neutrality, then uses Hot water cleaning fluorescent powder repeatedly arrives electrical conductivity of solution < 5mS/cm.
4. the method for coating of big granularity LED fluorescent powder according to claim 1, it is characterised in that: in step (b), described One silica gel, second silica gel are respectively DOW CORNING OE-6650A, DOW CORNING OE-6650B.
5. the method for coating of big granularity LED fluorescent powder according to claim 4, it is characterised in that: in step (b), described One silica gel, second silica gel volume ratio be 1:3.
6. the method for coating of big granularity LED fluorescent powder according to claim 1, it is characterised in that: in step (c), the place Manage concentration≤0.5 g/ml of the fluorescent powder in the covering liquid.
7. the method for coating of big granularity LED fluorescent powder according to claim 1 or 6, it is characterised in that: described in step (c) The temperature of drying is 120 ~ 160 DEG C.
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