CN107141805A - A kind of flexible red fluorescence film - Google Patents
A kind of flexible red fluorescence film Download PDFInfo
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- CN107141805A CN107141805A CN201710389636.3A CN201710389636A CN107141805A CN 107141805 A CN107141805 A CN 107141805A CN 201710389636 A CN201710389636 A CN 201710389636A CN 107141805 A CN107141805 A CN 107141805A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, 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
- C09K11/7784—Chalcogenides
- C09K11/7787—Oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2255—Oxides; Hydroxides of metals of molybdenum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2258—Oxides; Hydroxides of metals of tungsten
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Abstract
The invention discloses a kind of flexible red fluorescence film, it is made up of powder and organic matter, the mass ratio of powder and organic matter is (0.1~0.3): 1, organic matter is dimethyl silicone polymer.In powder, calculated with the mass percent of oxide, 0%<Na2O+Li2O+K2O total content<6.65%, 0<MgO<8.65%, 30%<WO3+MoO3Total content<49.75%, 5%<Gd2O3+La2O3+Y2O3Total content<34.95%, 0%<Eu2O3<22.28%.Present invention also offers the preparation method of above-mentioned flexible red fluorescence film, the present invention is simple to operate, and cost is low, can improve the uniformity and heat dissipation problem of fluorescent material coating, be suitable for long-distance fluorescent powder LED encapsulation and the extensive, industrialized production of mass.
Description
Technical field
The invention belongs to materialogy field, it is related to a kind of fluorescence membrane, specifically a kind of flexible red fluorescence film.
Background technology
Because white light LED part has luminous efficiency high, low-power consumption and advantages of environment protection, in recent years, white-light emitting two
Pole pipe（LED) receive much concern.Because fluorescent material is granular, easily reunite on substrate, and substrate is sticked
Power is also poor, and the performance such as heat endurance and uniformity is bad.And fluorescence membrane is due to its own preferable heat endurance, uniform
Property, and the adhesive force good to substrate, more and more paid attention to recently.Traditional dotting glue method is unfavorable for dissipating for LED chip
Heat, causes white light uneven, and scattering phenomenon is more serious.Because fluorescence membrane is conducive to array package and the radiating of LED chip
The features such as, as a study hotspot in recent years.
The flexible red fluorescence film being made of long-range red fluorescence powder, available in high-power LED lamp, it is to avoid
Phosphor material powder and blue-light LED chip energy source are directly contacted, and have broken away from traditional method for packing, it is only necessary on chip
The attached light conversion film in side, closely, traditional encapsulation mixes fluorescent material to the LED that illumination effect is made with packing forms
Close in glue, be then heating and curing on a chip, form fluorescent coating, because fluorescent material is than great, particle compares
Greatly, easily precipitate, thus hybrid resin point on chip to completion of cure this process, easily cause fluorescent material sinking, shape
Into hot spot, cause light extraction uneven, influence Luminescence Uniformity.And the phosphor material powder in light conversion film, often it is uniformly dispersed, by
This luminescent device being made has emission uniformity good, the advantages of light conversion effect is good.
Dimethyl silicone polymer (Polydimethylsiloxane, PDMS) is a kind of organosilicon polymer, with biology
Compatibility is good, cheap, make the advantages of simple, translucency is good, is generally made using the method for moulding by casting, it is easy into
Type, is the organic polymer material based on most widely used silicon.As far as we know, it there is no at present and use system described herein
Red fluorescence powder is combined with PDMS and the report of flexible fluorescence membrane is made.
The content of the invention
It is described the invention provides a kind of flexible red fluorescence film for above-mentioned technical problem of the prior art
This flexible red fluorescence film will solve fluorescent material of the prior art and easily form hot spot, cause light extraction uneven and shadow
Ring the technical problem of Luminescence Uniformity.
The invention provides a kind of flexible red fluorescence film, it is made up of powder and organic matter, described powder and organic
The mass ratio of thing is (0.1~0.3): 1, described organic matter is dimethyl silicone polymer.In described powder, with oxide
Mass percent calculate, 0%<Na2O+Li2O+K2O total content<6.65%, 0<MgO<8.65%, 30%<WO3+MoO3Always contain
Amount<49.75%, 5%<Gd2O3+La2O3+Y2O3Total content<34.95%, 0%<Eu2O3<22.28%。
Present invention also offers a kind of preparation method of flexible red fluorescence film, comprise the following steps：
1) each raw material is weighed according to mass percent, the mass percent of each raw material is：0%<Na2O+Li2O+K2O total content<
6.65%, 0<MgO<8.65%, 30%<WO3+MoO3Total content<49.75%, 5%<Gd2O3+La2O3+Y2O3Total content<
34.95%, 0%<Eu2O3<22.28%；
2) phosphor raw material is placed in agate mortar and be fully ground uniformly, be subsequently placed in 1000 ~ 1200 DEG C of heating in Muffle furnace
10 ~ 25 hours, room temperature is cooled to, required red fluorescence powder is finally given；
3) dimethyl silicone polymer and curing agent are weighed, the mass ratio of dimethyl siloxane and curing agent is 10：1, it is sufficiently mixed,
4) fluorescent material and step 3 are weighed）Solution, described powder and the mass ratio of dimethyl silicone polymer are (0.1~0.3)
: 1, poured into after being sufficiently mixed ultrasonic in a container；
5) above-mentioned mixed liquor is poured into another container, and be transferred in baking oven, dried at a temperature of less than 100 DEG C
Afterwards, room temperature is cooled to, the film after solidification is removed, obtains flexible red fluorescence film.
It is of the invention compared with traditional dispensing coating processes, this method independently makes fluorescent powder film layer, the distribution of fluorescent material
Uniformly, and the thickness of fluorescent powder film layer can be controlled, greatly improves photochromic uniformity.Fluorescent powder film layer can cut into a variety of
Size and shape, it is adaptable to the integration packaging of single or multi-chip, while film surface can be a variety of micro- comprising microlens array etc.
Fine texture, can improve the uniformity and light extraction efficiency of light extraction.Fluorescent powder film layer is made using this method, technique is simple, can weigh
Renaturation is strong, is suitable for the extensive, industrialized production of mass.The flexible red fluorescence being made of this long-range red fluorescence powder
Film, available in high-power LED lamp, it is to avoid phosphor material powder and blue-light LED chip energy source are directly contacted, and are improved
The whole efficiency of LED lamp.
The present invention is compared with prior art, and its technological progress is significant.Fluorescent material is combined with PDMS to be film-made, grasped
Make simple, cost is low, the uniformity and heat dissipation problem of fluorescent material coating can be improved, be suitable for the extensive, industrialization of mass
Production.
Brief description of the drawings
Fig. 1 is that flexible red fluorescence film is excited（λem = 616nm）And transmitting（λex = 465nm）Spectrum.
Embodiment
Embodiment 1
1）According to Na2O ﹕ La2O3﹕ MgO ﹕ WO3﹕ Eu2O3The ﹕ 14.93 of 20.74 ﹕ of=6.58 ﹕, 8.55 ﹕ 49.2（In terms of oxide content）'s
Component ratio, accurately weighs the NaCO that gross mass is 10g3, La2O3, 4MgCO3·Mg(OH)2·5H2O, WO3, Eu2O3It is placed in agate
It is fully ground uniform in Nao mortars, is subsequently placed in Muffle furnace 1050 DEG C and heats 18 hours, be cooled to room temperature, finally give red
Fluorescent material.
2）It is 0.18 ﹕ 1 according to powder and organic matter mass ratio, precise 0.3148g red fluorescence powders and 2.99g are organic
Thing；Wherein organic matter is according to 10：1 quality is than the g dimethyl silicone polymers of accurate weighing 2.7182（A）With 0.2718 g solidifications
Agent（B）；
3）Said mixture is put into 10mL sample bottle, as ultrasound 40min in supersonic generator；
4）Sample after ultrasound is transferred to surface plate；
5）45min is dried at 100 DEG C, you can obtain flexible red fluorescence film.
5）Using model F-7000 XRF, the spectral quality of the system fluorescence membrane is tested, such as Fig. 1 institutes
Show, as a result show, the most strong excitation peak of the system fluorescent material is located at 465nm, and under the exciting of the excitation wavelength light, the system is glimmering
Optical thin film shows as the red emission that most strong launch wavelength is located at 616nm, shows the system fluorescence membrane to match blue light core
The red fluorescence film of piece.
Claims (2)
1. a kind of flexible red fluorescence film, it is characterised in that：It is made up of powder and organic matter, described powder and organic matter
Mass ratio is (0.1~0.3): 1, described organic matter is dimethyl silicone polymer, in described powder, with the matter of oxide
Measure percentage to calculate, 0%<Na2O+Li2O+K2O total content<6.65%, 0<MgO<8.65%, 30%<WO3+MoO3Total content<
49.75%, 5%<Gd2O3+La2O3+Y2O3Total content<34.95%, 0%<Eu2O3<22.28%。
2. the preparation method of a kind of flexible red fluorescence film described in claim 1, it is characterised in that comprise the following steps：
1）Each raw material is weighed according to mass percent, the mass percent of each raw material is：0%<Na2O+Li2O+K2O total content<
6.65%, 0<MgO<8.65%, 30%<WO3+MoO3Total content<49.75%, 5%<Gd2O3+La2O3+Y2O3Total content<
34.95%, 0%<Eu2O3<22.28%；
2）Phosphor raw material is placed in agate mortar and is fully ground uniformly, 1000 ~ 1200 DEG C of heating in Muffle furnace are subsequently placed in
10 ~ 25 hours, room temperature is cooled to, required red fluorescence powder is finally given；
3）Weigh dimethyl silicone polymer and curing agent, the mass ratio of dimethyl siloxane and curing agent is 10：1, it is sufficiently mixed,
4）Weigh fluorescent material and step 3）Solution, described powder and the mass ratio of dimethyl silicone polymer are (0.1~0.3)
: 1, poured into after being sufficiently mixed ultrasonic in a container；
5）Above-mentioned mixed liquor is poured into another container, and is transferred in baking oven, is dried at a temperature of less than 100 DEG C
Afterwards, room temperature is cooled to, the film after solidification is removed, obtains flexible red fluorescence film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710389636.3A CN107141805A (en) | 2017-05-27 | 2017-05-27 | A kind of flexible red fluorescence film |
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| CN201710389636.3A CN107141805A (en) | 2017-05-27 | 2017-05-27 | A kind of flexible red fluorescence film |
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| CN107141805A true CN107141805A (en) | 2017-09-08 |
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| CN201710389636.3A Pending CN107141805A (en) | 2017-05-27 | 2017-05-27 | A kind of flexible red fluorescence film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110016333A (en) * | 2019-04-22 | 2019-07-16 | 甘肃兰辰科技有限公司 | Mechanoluminescence material and preparation method thereof based on yttrium-aluminium-garnet structure fluorescent powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120931A (en) * | 2010-12-03 | 2011-07-13 | 深圳职业技术学院 | Red fluorophor and preparation method thereof |
| WO2015099115A1 (en) * | 2013-12-27 | 2015-07-02 | 三菱化学株式会社 | Light-emitting device and method for designing light emitting device |
| CN104830333A (en) * | 2015-03-06 | 2015-08-12 | 江苏师范大学 | Li/Mg-codoped bi-perovskite red fluorescent powder and preparation method of same |
| CN105968812A (en) * | 2016-05-24 | 2016-09-28 | 中国科学院长春光学精密机械与物理研究所 | Application of polydimethylsiloxane, fluorescent film and preparation method thereof |
-
2017
- 2017-05-27 CN CN201710389636.3A patent/CN107141805A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120931A (en) * | 2010-12-03 | 2011-07-13 | 深圳职业技术学院 | Red fluorophor and preparation method thereof |
| WO2015099115A1 (en) * | 2013-12-27 | 2015-07-02 | 三菱化学株式会社 | Light-emitting device and method for designing light emitting device |
| CN104830333A (en) * | 2015-03-06 | 2015-08-12 | 江苏师范大学 | Li/Mg-codoped bi-perovskite red fluorescent powder and preparation method of same |
| CN105968812A (en) * | 2016-05-24 | 2016-09-28 | 中国科学院长春光学精密机械与物理研究所 | Application of polydimethylsiloxane, fluorescent film and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110016333A (en) * | 2019-04-22 | 2019-07-16 | 甘肃兰辰科技有限公司 | Mechanoluminescence material and preparation method thereof based on yttrium-aluminium-garnet structure fluorescent powder |
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Application publication date: 20170908 |