CN102107178B - Fluorescent material coating method and substrate prepared by same - Google Patents
Fluorescent material coating method and substrate prepared by same Download PDFInfo
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- CN102107178B CN102107178B CN 200910265607 CN200910265607A CN102107178B CN 102107178 B CN102107178 B CN 102107178B CN 200910265607 CN200910265607 CN 200910265607 CN 200910265607 A CN200910265607 A CN 200910265607A CN 102107178 B CN102107178 B CN 102107178B
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Abstract
The invention relates to a fluorescent material coating method and a substrate prepared by the same. The fluorescent material coating method comprises the following steps of: (A) dispersing a fluorescent material in a first solvent to form fluorescent material solution; (B) filling the substrate in a container, injecting a second solvent in the container and covering the surface of the substrate by using the second solvent; (C) adding the fluorescent material solution into the second solvent to form a fluorescent material thin film on the surface of the second solvent; and (D) removing the second solvent from the container to form the fluorescent material thin film on the surface of the substrate.
Description
Technical field
The invention relates to a kind of fluorescent material coating method and prepared substrate thereof, especially refer to a kind ofly can evenly be coated with the method for fluorescent material on substrate, have character homogeneous and the good substrate that is coated with fluorescent material of refractive index to make.
Background technology
In recent years, because light emitting diode (LED) has that luminous efficiency is high, power consumption is few, long service life, and the advantage such as assembly volume is little, be widely used in various light-emitting devices, and replaced several lighting apparatus.
Yet LED but is difficult to be applied to people's livelihood illumination market, has except light emitting diode the problems such as heat radiation, luminance shortage and descending luminance, also has the problem that can't directly inspire white light.Therefore, existing many research attempts develop high efficiency white light LEDs, to replace existing lighting apparatus.
The present white light LEDs of main flow is to utilize blue LED chip to coordinate the YAG fluorescent powder of gold-tinted, with as white light source.Although with this complementary colours white light that principle is produced, the continuity that its spectral wavelength distributes is not as sunshine, and the situation of colored inequality, therefore color saturation is lower.Therefore, the white light source that produces in this way only can be used for the use of simply throwing light on, and can't be widely used in people's livelihood illumination market.
In addition, also can utilize the ultraviolet light-emitting diodes chip to coordinate ruddiness, green glow and blue light three-color phosphor, by red bluish-green trichromatic light mixing mechanism, can be mixed into white light.
At present, can to send the light emitting diode of white light be to adopt following method to encapsulate in formation.At first, weigh more than one fluorescent material of a proper proportion according to predetermined colour temperature.Then, fluorescent material is added to resin (as: silica resin or epoxy resin) and stirs, fluorescent material can be dispersed in resin.Then, the resin that is dispersed with fluorescent material is mixed with curing agent, the colloid 102 that will be dispersed with fluorescent material with point gum machine is covered on LED chip 101, and drying and packaging technology can make a LED assembly 10, as shown in Figure 1.
Yet, according to the prepared LED assembly of said method, because external form and the size of fluorescent material are irregular, therefore phosphor powder layer easily because of fluorescent material material character disunity, and cause colour temperature inaccurate with the unequal problem of mixed light.Therefore, need badly at present and develop a kind of fluorescent-powder coating method, it can produce even light mixing and the good substrate of refractive index, to be applied in LED luminous lighting equipment.
Summary of the invention
The object of the present invention is to provide a kind of fluorescent material coating method, it can easy method be formed at fluorescent material on substrate.
Another object of the present invention is to provide a kind of substrate that is coated with fluorescent material, its surface has the fluorescent material of character homogeneous, and can be as the luminescence component of light emitting diode.
For achieving the above object, fluorescent material coating method provided by the invention comprises the following steps:
(A) fluorescent material is scattered in one first solvent, to form a fluorescent material solution;
(B) substrate is placed in a container, and injects one second solvent, and the surface of the second solvent covered substrate;
(C) fluorescent material solution is added into the second solvent, to form a fluorescent material film in the second solvent surface; And
(D) remove the second solvent in container, make fluorescent material film be formed at substrate surface.
In fluorescent material coating method of the present invention, when fluorescent material solution is slowly splashed in the second solvent, and can form a fluorescent material film.Simultaneously, by slowly removing the second solvent, and can make fluorescent material film well be formed on substrate surface.
In fluorescent material coating method of the present invention, after step (D), can also comprise a step (E): drying is formed with the substrate of fluorescent material film, to remove the first solvent of suspension fluorescent material.Simultaneously, after step (E), can also comprise a step (F): repeat this step (A) to step (E), to form the plural layer fluorescent material film.
In fluorescent material coating method of the present invention, the first solvent and the second solvent there is no particular restriction, as long as the second solvent proportion and tension force are all greater than the first solvent.Preferably, the first solvent be select Free water, ethanol, propyl alcohol, and composition thereof the group that forms; This second solvent be select Free water, ethanol, propyl alcohol, and composition thereof the group that forms.
In addition, for making the substrate surface that is formed on that fluorescent material film can be more firm, can also utilize sol-gal process to be formed with a packed layer in the fluorescent material film surface, so that fluorescent material film has desirable refractive index.Therefore, in fluorescent material coating method of the present invention, after step (E), can also comprise the following steps: (G) provide an alkoxide solution and-acid solution; (H) mixed alcoholate solution and acid solution are to obtain a mixed solution; And (I) this mixed solution is coated on fluorescent material film, to form a packed layer.Simultaneously, after step (I), can also comprise a step (J): heat treatment is formed with the substrate of packed layer, then annealing in process is formed with the substrate of packed layer.
In fluorescent material coating method of the present invention, alkoxide can be a silicon alkoxide or a metal alkoxide, and the metal of the metal alkoxide group that selects free Al, Zn, Zr, Y, Ti, Co, Mn, Ni, Cu, Pb and form.In addition, acid solution can be nitric acid, hydrochloric acid, hydrofluoric acid, sulfuric acid, phosphoric acid or citric acid solution.Moreover acid solution can also comprise YAG, Y
2O
3, AlN or its mixture.Simultaneously, acid solution can comprise the metal ion of the group that the free Ce of at least one choosing, Nd, La, Eu, Tb, Gd, Dy, Er, Tm, Yb, Lu, Li, Mg, Ca, Sr, Ba and other lanthanide series (Pr, Pm, Sm, Ho, Er) form again.
On the other hand, the present invention also provides a kind of prepared substrate that is coated with fluorescent material of said method that utilizes, and it comprises: a substrate and is positioned at the fluorescent material film on substrate.Wherein, fluorescent material comprises a ball-type carrier and a fluorescent powder; Or fluorescent material is a fluorescent powder.In addition, in the substrate that is coated with fluorescent material of the present invention, can also comprise a packed layer, be positioned on fluorescent material film, and fluorescent material film be positioned between substrate and packed layer.
Therefore, utilize the substrate that is coated with fluorescent material of fluorescent material coating method made of the present invention, due to fluorescent material particle diameter and character homogeneous, and can form uniform fluorescent material film in substrate surface.Simultaneously, by the packed layer on fluorescent material film, how material film can not peeled off from substrate easily except protecting fluorescence, more can promote the refractive index of institute's formation substrate.
In fluorescent material coating method of the present invention and be coated with in the substrate of fluorescent material, fluorescent material comprises a ball-type carrier and a fluorescent powder.Wherein, fluorescent powder can cover the ball-type carrier surface; Fluorescent powder can be contained in the ball-type carrier inside; Or part fluorescent powder covering ball-type carrier surface, and the part fluorescent powder is contained in the ball-type carrier inside.Simultaneously, the material of ball-type carrier can be SiO
x, TiO
x, PS, PMMA or melmac.The material of fluorescent powder can be general known fluorescent material, as: select free ZnO, ZrO
2, PbO, Y
2O
3, Y
2O
2, Zn
2SiO
4, Y
3Al
5O
12, Y
3(AlGa)
5O
12Y
2SiO
5, LaOCl, InBO
3, ZnGa
2O
4, ZnS, PbS, CdS, CaS, SrS, Zn
xCd
1-xS, Y
2O
2S, AlN and Gd
2O
2The compound of the group that S forms, and as can also the adulterate element of the group that the free Cu of at least one choosing, Ag, Eu, Yb, La, Cl, Tb, Al, Ce, Er, Zn, Mn and other lanthanide series (Pr, Pm, Sm, Ho, Er) form of the compound of fluorescent powder.Moreover the particle diameter of ball-type carrier is preferably between 350nm to 10 μ m, is more preferably between 350nm to 5 μ m; And the particle diameter of fluorescent powder is preferably between between 10nm to 5000nm, is more preferably between between 10nm to 100nm, is between between 10nm to 30nm best.
Moreover in fluorescent material coating method of the present invention and be coated with in the substrate of fluorescent material, substrate can be any LED chip or LED assembly semi-finished product, is preferably blue light epi-wafer or flip-chip LED chip that a sapphire substrate, is formed with epitaxial layer.
In addition, in the substrate that is coated with fluorescent material of the present invention, the material of packed layer can be SiO
2, Al
2O
3, ZnO, ZrO, Y
2O
3, TiO
2, CoO, MnO
2, NiO, CuO, PbO and compound thereof the group that forms.Simultaneously, packed layer can also comprise YAG, Y
2O
3, AlN or its mixture, and YAG or Y
2O
3Can also adulterate and select the element of the group that free Ce, Nd, La, Eu, Tb, Gd, Dy, Er, Tm, Yb, Lu, Li, Mg, Ca, Sr, Ba and other lanthanide series (Pr, Pm, Sm, Ho, Er) form.
Description of drawings
Fig. 1 is the schematic diagram of known light emitting diode.
Fig. 2 A to Fig. 2 F is the step schematic diagram that the fluorescent material of the embodiment of the present invention 1 is coated substrate surface.
Primary clustering symbol description in accompanying drawing
The 10-LED assembly; The 101-LED chip; The 102-colloid; The 20-substrate; 210-fluorescent material; 211-the first solvent; The 21-fluorescent powder film; The 22-packed layer; 23-the second solvent; The 24-container.
The specific embodiment
Embodiment 1
Fig. 2 A to Fig. 2 F is the step schematic diagram that the fluorescent material of the embodiment of the present invention 1 is coated substrate surface.
Preparation fluorescent material solution
At first, get fluorescent material as a fluorescent material, wherein the ball-type carrier of fluorescent material is that the employing particle diameter is that 500nm and material are SiO
2Nanosphere, fluorescent powder adopts the approximately Y of 30nm of particle diameter
2O
3: La
3+, YAG:La
3+And the mixture of CdSe:ZnS, and fluorescent powder is at the ball-type carrier surface by silane molecule (APTMS) bond.By the ratio of adjusting various fluorescent powders, after blue light-emitting diode excited, this fluorescent material can carry out mixed light and send white light in its surface.
Then, fluorescent material 210 is mixed in the first solvent 211 with polymolecularity, obtains a fluorescent material mixed solution, as shown in Fig. 2 A.At this, adopt ethanol as the first solvent.
Form fluorescent powder film
As shown in Fig. 2 B, get a substrate 20, and be placed on container 24 bottoms, wherein, this substrate is a flip-chip LED chip.Then, inject the second solvent 23 in container 24, at this, adopt pure water as the second solvent.Then, slowly drip the fluorescent material mixed solutions in the second solvent 23 surface, due to the proportion of pure water and tension force higher than ethanol, and reason SiO more
2Formed fluorescent material 210 has multiple hole, therefore fluorescent material 210 can be arranged in the pure water surface, and forms a fluorescent powder film 21, as shown in Fig. 2 C.
Then, slowly the second solvent 23 is released from the interior extraction of container 24 or from container 24 bottoms, until fluorescent powder film 21 is pressed close to substrate 20 surfaces, as shown in Fig. 2 D.Then, container 24 is placed in the equipment for drying (not shown), removes the ethanol (not shown) of tool polymolecularity with evaporation.To be dried fully after, can obtain a fluorescent powder film 21 that is formed at substrate 20 surfaces, as shown in Fig. 2 E.
In addition, also can repeat the above-mentioned steps as shown in Fig. 2 B to Fig. 2 E etc., form the fluorescent powder film with sandwich construction, so that formed fluorescent powder film light mixing effect reaches colour temperature and the color rendering of expection.
With the above-mentioned flip-chip LED chip that is coated with fluorescent powder film that makes, after pilot was bright, the color temperature of mixed light that sends was 5400K.
Form packed layer
At first, provide an alkoxide solution, wherein, this alkoxide solution can be silanol saline solution or single or composition metal alkoxide solution.In the present embodiment, be to adopt the aqueous solution of silicon alkoxide (as: TEOS) as collosol and gel precursor solution.
Simultaneously, also provide a kind of acid solution, wherein, this acid solution is by with YAG and La
3+It is formulated that salt is dissolved in a nitric acid institute.
Then, after the above-mentioned alkoxide solution of preparing and acid solution are mixed, with method of spin coating, mixed solution is coated on fluorescent powder film 21, and formed a packed layer 22, as shown in Fig. 2 F.By sol-gal process, the obtained packed layer of the present embodiment is for containing YAG:La
3+SiO
2Material layer.
After standing, the substrate 20 that will have fluorescent powder film 21 and packed layer 22 is heat-treated, then carries out annealing in process, completes the substrate that is coated with fluorescent material of the present embodiment.
By heat treatment and annealing in process, can make the YAG recrystallization in packed layer 22, can promote the material homogeneity of fluorescent powder film, and more can make fluorescent powder film reach the homogeneous refractive index of being scheduled to.Simultaneously, be formed in the gap that reaches on fluorescent powder film between fluorescent material, therefore more can protect fluorescent material can not peel off from substrate due to packed layer 22.
Embodiment 2
The preparation method of the present embodiment as described in Example 1.Wherein, the fluorescent material that the present embodiment uses is that the employing particle diameter is that 500nm and material are SiO
2Nanosphere as the ball-type carrier, fluorescent powder adopts the approximately Y of 50nm of particle diameter
2O
3: Eu
3+, Y
2O
3: yb
3+, Y
2O
3: Ce
3+, YAG:Ce
3+And the mixture of CdSe:ZnS, and the mixture of fluorescent powder is to be contained in the ball-type carrier inside.In addition, the present embodiment substrate to be coated is to use sapphire substrate.Moreover, use Al and Ti composition metal alkoxide solution as the collosol and gel precursor aqueous solution, and use is added with La
3+Y
2O
3Salpeter solution carries out solgel reaction to form packed layer.Therefore, the packed layer of the present embodiment is for containing Y
2O
3: La
3+Al
2O
3-TiO
2Material layer.
Embodiment 3
The preparation method of the present embodiment as described in Example 1.Wherein, the fluorescent material that the present embodiment uses is that the employing particle diameter is that 1000nm and material are SiO
2Nanosphere as the ball-type carrier, and the ball-type carrier inside comprises the CdSe:ZnS quantum dot; Fluorescent powder adopts the approximately Y of 50nm of particle diameter
2O
3: La
3+And YAG:La
3+Mixture, and fluorescent powder is at the ball-type carrier surface by the silane molecule bond.
Above-described embodiment is only to give an example for convenience of description, and the interest field that the present invention advocates is from should with described being as the criterion of claim scope of application, but not only limiting to above-described embodiment.
Claims (18)
1. a fluorescent material coating method, comprise the following steps:
A) fluorescent material is scattered in one first solvent, to form a fluorescent material solution;
B) substrate is placed in a container, and injects one second solvent, and this second solvent covers the surface of this substrate;
C) this fluorescent material solution is added into this second solvent, to form a fluorescent material film in this second solvent surface; And
D) remove this second solvent in this container, make this fluorescent material film be formed at this substrate surface.
2. fluorescent material coating method as claimed in claim 1, wherein, after step D, comprise a step e: drying is formed with this substrate of this fluorescent material film.
3. fluorescent material coating method as claimed in claim 2, wherein, after step e, comprise a step F: repeat this steps A to step e, to form the plural layer fluorescent material film.
4. fluorescent material coating method as claimed in claim 2, wherein, after step e, comprise the following steps:
G) provide an alkoxide solution and an acid solution;
H) mix this alkoxide solution and this acid solution, to obtain a mixed solution; And
I) be coated with this mixed solution on this fluorescent material film, to form a packed layer.
5. fluorescent material coating method as claimed in claim 4, wherein, after step I, comprise a step J: heat treatment is formed with this substrate of this packed layer, then annealing in process is formed with this substrate of this packed layer.
6. fluorescent material coating method as claimed in claim 1, wherein, the proportion of this second solvent is greater than this first solvent.
7. fluorescent material coating method as claimed in claim 1, wherein, this fluorescent material comprises a ball-type carrier and a fluorescent powder.
8. fluorescent material coating method as claimed in claim 7, wherein, this fluorescent powder covers this ball-type carrier surface.
9. fluorescent material coating method as claimed in claim 7, wherein, this fluorescent powder is contained in this ball-type carrier inside.
10. fluorescent material coating method as claimed in claim 7, wherein, the material of this ball-type carrier is SiO
x, TiO
x, PS, PMMA or melmac, and the X scope is between 0.5～2.
11. fluorescent material coating method as claimed in claim 7, wherein, the particle diameter of this ball-type carrier is between 350nm to 10 μ m.
12. fluorescent material coating method as claimed in claim 7, wherein, the particle diameter of this fluorescent powder is between between 10nm to 5000nm.
13. fluorescent material coating method as claimed in claim 1, wherein, this first solvent is the group that selects Free water, ethanol, propyl alcohol and composition thereof to form.
14. fluorescent material coating method as claimed in claim 1, wherein, this second solvent is the group that selects Free water, ethanol, propyl alcohol and composition thereof to form.
15. fluorescent material coating method as claimed in claim 1, wherein, this substrate is a sapphire substrate, a blue light epi-wafer or flip-chip LED chip.
16. fluorescent material coating method as claimed in claim 4, wherein, this alkoxide is a silicon alkoxide or a metal alkoxide, and the metal of this metal alkoxide group that selects free Al, Zn, Zr, Y, Ti, Co, Mn, Ni, Cu, Pb and combination thereof to form.
17. fluorescent material coating method as claimed in claim 4, wherein, this acid solution comprises YAG, Y
2O
3, AlN or its mixture.
18. fluorescent material coating method as claimed in claim 4, wherein, this acid solution comprises the metal ion of the group that the free Ce of at least one choosing, Nd, La, Eu, Tb, Gd, Dy, Er, Tm, Yb, Lu, Li, Mg, Ca, Sr, Ba, Pr, Pm, Sm, Ho and Er form.
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|---|---|---|---|
| CN 200910265607 CN102107178B (en) | 2009-12-28 | 2009-12-28 | Fluorescent material coating method and substrate prepared by same |
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|---|---|---|---|
| CN 200910265607 CN102107178B (en) | 2009-12-28 | 2009-12-28 | Fluorescent material coating method and substrate prepared by same |
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| CN102107178B true CN102107178B (en) | 2013-06-05 |
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| CN104279514B (en) * | 2013-07-03 | 2015-12-02 | 深圳市绎立锐光科技开发有限公司 | Wavelength converter and preparation method thereof, related lighting fixtures and optical projection system |
| TWI649900B (en) * | 2015-02-04 | 2019-02-01 | 億光電子工業股份有限公司 | LED package structure and manufacturing method thereof |
| TWI591864B (en) * | 2015-08-26 | 2017-07-11 | 廣科精密股份有限公司 | Light emitting device and method for preparing the same |
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| CN108281535A (en) * | 2018-02-02 | 2018-07-13 | 温州大学 | Composite fluorescence laminated glass and preparation method thereof and the application on white light LEDs |
| TWI710129B (en) * | 2020-02-10 | 2020-11-11 | 台灣愛司帝科技股份有限公司 | Led chip package structure and method of manufacturing the same |
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| CN1597840A (en) * | 2004-08-06 | 2005-03-23 | 孙祥民 | Light storage luminous energy saving material made by mini-glass bead and its use |
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