CN106206913B - A kind of preparation method of LED fluorescent powder coating - Google Patents
A kind of preparation method of LED fluorescent powder coating Download PDFInfo
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- CN106206913B CN106206913B CN201610830207.0A CN201610830207A CN106206913B CN 106206913 B CN106206913 B CN 106206913B CN 201610830207 A CN201610830207 A CN 201610830207A CN 106206913 B CN106206913 B CN 106206913B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
- H01L33/50—Wavelength conversion elements
- H01L33/505—Wavelength conversion elements characterised by the shape, e.g. plate or foil
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
Abstract
The invention discloses a kind of LED fluorescent powder coatings, its method is as follows: using strontium carbonate, ethyl orthosilicate, barium acetate, foaming agent and europium carbonate as raw material, fluorescent powder sol solutions are made in acetic acid and ethanol, and prepare LED fluorescent powder coating using the double-deck semar technique on substrate.The problem of preparation method of the present invention is simple, and the structure for solving fluoresent coating is uneven, poor controllability substantially increases the uniformity that LED goes out light.
Description
Technical field
The invention belongs to fluorescent technique fields, and in particular to a kind of LED fluorescent powder coating.
Background technique
LED is the abbreviation of light emitting diode (light emitting diode), can be with according to the difference of its luminescent material
It is divided into organic LED (i.e. OLED) and inorganic LED (commonly referred to as LED) two major classes.1996, in blue GaN base light-emitting diodes base
White LED is successfully realized on plinth, with low voltage drive, all solid state, low-power consumption, it is long-acting it is reliable, pollution-free, can change etc. it is excellent
Point.Therefore, in recent years, the semiconductor lighting based on white light LEDs (forth generation lighting engineering) has obtained quick development.
The current most common white light LEDs are achieved in that fluorescent powder conversion hysteria i.e. (pc-LED), such as in blue-light LED chip
Surface applies (yellow+blue) white light LEDs of one layer of yellow fluorescent powder.In addition the realization technology of phosphor powder layer, mainly using biography
The dosing technology of system, the i.e. gluing process of fluorescent powder mixing silica gel.But the fluorescent coating obtained in this way is since structure is uneven,
Poor controllability, so that the uniformity that LED goes out light is poor.
Overcome drawbacks described above, must just realize the thickness of phosphor powder layer, the uniform, controllable of shape.
Summary of the invention
The object of the present invention is to provide a kind of LED fluorescent powder coatings, and preparation method of the present invention is simple, solve fluoresent coating
Structure it is uneven, the problem of poor controllability, substantially increase the uniformity that LED goes out light.
A kind of LED fluorescent powder coating, preparation method are as follows:
Step 1, strontium carbonate is added in acetic acid, after being stirred to react, obtains strontium acetate acetic acid solution；
Step 2, ethyl orthosilicate and barium acetate are added in acetic acid solution, after mixing evenly, before obtaining uniform colloidal sol
Liquid；
Step 3, europium carbonate is added in solution, after mixing evenly natural subsidence while stirring, is obtained with white precipitate
Reaction solution；
Step 4, washes of absolute alcohol is used after white precipitate being filtered, and obtains cleaning solution；
Step 5, it is stirred evenly after filtered reaction solution being merged with cleaning solution, obtains colloidal sol dilution；
Step 6, foaming agent will be added in sol solutions, stirs evenly, form mixed liquor；
Step 7, mixed liquor is put into water-bath be evaporated under reduced pressure and carries out aeration concentration, be concentrated after water bath processing
Liquid；
Step 8, substrate is dipped to alcoholic solution, after ultrasonic cleaning, adopts and dry wash with distilled water；
Step 9, modified organic silicon dispersion liquid is coated in substrate surface, obtains organosilicone film；
Step 10, concentrate is added dropwise and carries out rotation smearing in organosilicone film, form fluorescent powder film；
Step 11, the substrate with organosilicone film and fluorescent powder film is put into constant temperature compressive reaction in reaction kettle, so
After be passed through pressurized with hydrogen heating reaction, obtain LED fluorescent powder coating after natural cooling.
Formula in the step are as follows: 11-12 parts of strontium carbonate, 20-35 parts of ethyl orthosilicate, 8-11 parts of barium acetate, foaming
1-2 parts of agent, the europium carbonate quality is the 1-5% of ethyl orthosilicate, and the foaming agent uses ammonium carbonate.
Mixing speed in the step is 300-1200r/min, mixing time 30-120min.
Acetic acid concentration in the step 1 is 0.1-0.6mol/L, and acetic acid is added in the strontium carbonate until pH reaches 3-
4。
It is 0.1-0.3mg/min that speed, which is added, in europium carbonate in the step 3.
Washes of absolute alcohol number in the step 4 is 2-5 times, and the dehydrated alcohol total amount is the 0.8-1.1 of acetic acid
Times, the dehydrated alcohol washing principle is a small amount of multiple.
Water bath temperature is 80-90 DEG C in the step 7, and the concentrate is the 25-40% of mixed liquor, and the aeration is anti-
It should be using slightly boiled mode be heated, with foaming agent dispersion aeration reaction combination.
Alcoholic solution in the step 8 uses one of ethyl alcohol, propyl alcohol, isopropanol, and the supersonic frequency is 30-
60kHz, ultrasonic time 5-15min.
Modified organic silicon dispersion liquid in the step 9 uses modified organic silicon concentration for the ethanol solution of 3-11%, described
The coated weight of substrate surface is 0.1-0.7mg/cm2。
The coated weight of concentrate in the step 10 is 0.5-1.2mg/cm2, the revolving speed that the rotation is smeared is 900-
1500r/min。
The temperature of constant temperature compressive reaction in the step 11 is 80-120 DEG C, pressure 2-4MPa, reaction time 2-
4h, the pressure of the pressurized, heated reaction are 9-11MPa, and temperature is 150-180 DEG C, reaction time 3-8h, the cooling side
Formula is using air-cooled.
Compared with prior art, the invention has the following advantages:
1, the problem of preparation method of the present invention is simple, and the structure for solving fluoresent coating is uneven, poor controllability, mentions significantly
High LED goes out the uniformity of light.
2, the present invention is using the double-deck semar technique, the film smeared by modified organic silicon and colloidal sol, and with the pressurization of this constant temperature
It is reacted with reproducibility pressurized, heated, improves the cohesive force between substrate and fluorescent coating, while bringing by modified organic silicon
Silica reduce silicic acid base fluorescent powder coating defect.
3, the present invention substantially increases the dispersibility of phosphor material powder by the sol solutions that Ethanol-Acetic Acid mixed liquor configures,
It not only ensure that crystallinity significantly, while the increase of dispersibility improves the chemical stability and thermal stability of fluorescent material, mentions
Its high service life.
Specific embodiment
The present invention is described further below with reference to embodiment:
Embodiment 1
A kind of LED fluorescent powder coating, preparation method are as follows:
Step 1, strontium carbonate is added in acetic acid, after being stirred to react, obtains strontium acetate acetic acid solution；
Step 2, ethyl orthosilicate and barium acetate are added in acetic acid solution, after mixing evenly, before obtaining uniform colloidal sol
Liquid；
Step 3, europium carbonate is added in solution, after mixing evenly natural subsidence while stirring, is obtained with white precipitate
Reaction solution；
Step 4, washes of absolute alcohol is used after white precipitate being filtered, and obtains cleaning solution；
Step 5, it is stirred evenly after filtered reaction solution being merged with cleaning solution, obtains colloidal sol dilution；
Step 6, foaming agent will be added in sol solutions, stirs evenly, form mixed liquor；
Step 7, mixed liquor is put into water-bath be evaporated under reduced pressure and carries out aeration concentration, be concentrated after water bath processing
Liquid；
Step 8, substrate is dipped to alcoholic solution, after ultrasonic cleaning, adopts and dry wash with distilled water；
Step 9, modified organic silicon dispersion liquid is coated in substrate surface, obtains organosilicone film；
Step 10, concentrate is added dropwise and carries out rotation smearing in organosilicone film, form fluorescent powder film；
Step 11, the substrate with organosilicone film and fluorescent powder film is put into constant temperature compressive reaction in reaction kettle, so
After be passed through pressurized with hydrogen heating reaction, obtain LED fluorescent powder coating after natural cooling.
Formula in the step are as follows: 11 parts of strontium carbonate, 20 parts of ethyl orthosilicate, 8 parts of barium acetate, 1 part of foaming agent, it is described
Europium carbonate quality is the 1% of ethyl orthosilicate, and the foaming agent uses ammonium carbonate.
Mixing speed in the step is 300r/min, mixing time 30min.
Acetic acid concentration in the step 1 is 0.1mol/L, and acetic acid is added in the strontium carbonate until pH reaches 3.
It is 0.1mg/min that speed, which is added, in europium carbonate in the step 3.
Washes of absolute alcohol number in the step 4 is 2 times, and the dehydrated alcohol total amount is 0.8 times of acetic acid, described
It is a small amount of multiple that dehydrated alcohol, which washs principle,.
Water bath temperature is 80 DEG C in the step 7, and the concentrate is the 25% of mixed liquor, and the aeration reaction uses
Slightly boiled mode is heated, with foaming agent dispersion aeration reaction combination.
Alcoholic solution in the step 8 uses ethyl alcohol, and the supersonic frequency is 30kHz, ultrasonic time 5min.
Modified organic silicon dispersion liquid in the step 9 use modified organic silicon concentration for 3% ethanol solution, the base
The coated weight on material surface is 0.1mg/cm2。
The coated weight of concentrate in the step 10 is 0.5mg/cm2, the revolving speed that the rotation is smeared is 900r/min.
The temperature of constant temperature compressive reaction in the step 11 is 80 DEG C, pressure 2MPa, reaction time 2h, described to add
The pressure of pressure heating reaction is 9MPa, and temperature is 150 DEG C, reaction time 3h, and the type of cooling is using air-cooled.
Coating layer thickness of the present invention is 5.4 μm, in 254nm ultraviolet excitation, issues high efficiency blue, transmitting main peak in 454nm,
Stability is good, and luminous intensity is high.
Embodiment 2
A kind of LED fluorescent powder coating, preparation method are as follows:
Step 1, strontium carbonate is added in acetic acid, after being stirred to react, obtains strontium acetate acetic acid solution；
Step 2, ethyl orthosilicate and barium acetate are added in acetic acid solution, after mixing evenly, before obtaining uniform colloidal sol
Liquid；
Step 3, europium carbonate is added in solution, after mixing evenly natural subsidence while stirring, is obtained with white precipitate
Reaction solution；
Step 4, washes of absolute alcohol is used after white precipitate being filtered, and obtains cleaning solution；
Step 5, it is stirred evenly after filtered reaction solution being merged with cleaning solution, obtains colloidal sol dilution；
Step 6, foaming agent will be added in sol solutions, stirs evenly, form mixed liquor；
Step 7, mixed liquor is put into water-bath be evaporated under reduced pressure and carries out aeration concentration, be concentrated after water bath processing
Liquid；
Step 8, substrate is dipped to alcoholic solution, after ultrasonic cleaning, adopts and dry wash with distilled water；
Step 9, modified organic silicon dispersion liquid is coated in substrate surface, obtains organosilicone film；
Step 10, concentrate is added dropwise and carries out rotation smearing in organosilicone film, form fluorescent powder film；
Step 11, the substrate with organosilicone film and fluorescent powder film is put into constant temperature compressive reaction in reaction kettle, so
After be passed through pressurized with hydrogen heating reaction, obtain LED fluorescent powder coating after natural cooling.
Formula in the step are as follows: 12 parts of strontium carbonate, 35 parts of ethyl orthosilicate, 11 parts of barium acetate, 2 parts of foaming agent, institute
5% that europium carbonate quality is ethyl orthosilicate is stated, the foaming agent uses ammonium carbonate.
Mixing speed in the step is 1200r/min, mixing time 120min.
Acetic acid concentration in the step 1 is 0.6mol/L, and acetic acid is added in the strontium carbonate until pH reaches 4.
It is 0.3mg/min that speed, which is added, in europium carbonate in the step 3.
Washes of absolute alcohol number in the step 4 is 5 times, and the dehydrated alcohol total amount is 1.1 times of acetic acid, described
It is a small amount of multiple that dehydrated alcohol, which washs principle,.
Water bath temperature is 90 DEG C in the step 7, and the concentrate is the 40% of mixed liquor, and the aeration reaction uses
Slightly boiled mode is heated, with foaming agent dispersion aeration reaction combination.
Alcoholic solution in the step 8 uses propyl alcohol, and the supersonic frequency is 60kHz, ultrasonic time 15min.
Modified organic silicon dispersion liquid in the step 9 use modified organic silicon concentration for 11% ethanol solution, the base
The coated weight on material surface is 0.7mg/cm2。
The coated weight of concentrate in the step 10 is 1.2mg/cm2, the revolving speed that the rotation is smeared is 1500r/
min。
The temperature of constant temperature compressive reaction in the step 11 is 120 DEG C, pressure 4MPa, reaction time 4h, described
The pressure of pressurized, heated reaction is 11MPa, and temperature is 180 DEG C, reaction time 8h, and the type of cooling is using air-cooled.
Coating layer thickness of the present invention is 11.3 μm, in 254nm ultraviolet excitation, issues high efficiency blue, transmitting main peak exists
465nm, stability is good, and luminous intensity is high.
Embodiment 3
A kind of LED fluorescent powder coating, preparation method are as follows:
Step 1, strontium carbonate is added in acetic acid, after being stirred to react, obtains strontium acetate acetic acid solution；
Step 2, ethyl orthosilicate and barium acetate are added in acetic acid solution, after mixing evenly, before obtaining uniform colloidal sol
Liquid；
Step 3, europium carbonate is added in solution, after mixing evenly natural subsidence while stirring, is obtained with white precipitate
Reaction solution；
Step 4, washes of absolute alcohol is used after white precipitate being filtered, and obtains cleaning solution；
Step 5, it is stirred evenly after filtered reaction solution being merged with cleaning solution, obtains colloidal sol dilution；
Step 6, foaming agent will be added in sol solutions, stirs evenly, form mixed liquor；
Step 7, mixed liquor is put into water-bath be evaporated under reduced pressure and carries out aeration concentration, be concentrated after water bath processing
Liquid；
Step 8, substrate is dipped to alcoholic solution, after ultrasonic cleaning, adopts and dry wash with distilled water；
Step 9, modified organic silicon dispersion liquid is coated in substrate surface, obtains organosilicone film；
Step 10, concentrate is added dropwise and carries out rotation smearing in organosilicone film, form fluorescent powder film；
Step 11, the substrate with organosilicone film and fluorescent powder film is put into constant temperature compressive reaction in reaction kettle, so
After be passed through pressurized with hydrogen heating reaction, obtain LED fluorescent powder coating after natural cooling.
Formula in the step are as follows: 11 parts of strontium carbonate, 28 parts of ethyl orthosilicate, 9 parts of barium acetate, 1 part of foaming agent, it is described
Europium carbonate quality is the 4% of ethyl orthosilicate, and the foaming agent uses ammonium carbonate.
Mixing speed in the step is 900r/min, mixing time 90min.
Acetic acid concentration in the step 1 is 0.5mol/L, and acetic acid is added in the strontium carbonate until pH reaches 4.
It is 0.2mg/min that speed, which is added, in europium carbonate in the step 3.
Washes of absolute alcohol number in the step 4 is 4 times, and the dehydrated alcohol total amount is 1.0 times of acetic acid, described
It is a small amount of multiple that dehydrated alcohol, which washs principle,.
Water bath temperature is 85 DEG C in the step 7, and the concentrate is the 35% of mixed liquor, and the aeration reaction uses
Slightly boiled mode is heated, with foaming agent dispersion aeration reaction combination.
Alcoholic solution in the step 8 uses isopropanol, and the supersonic frequency is 50kHz, ultrasonic time 10min.
Modified organic silicon dispersion liquid in the step 9 use modified organic silicon concentration for 9% ethanol solution, the base
The coated weight on material surface is 0.5mg/cm2。
The coated weight of concentrate in the step 10 is 1.1mg/cm2, the revolving speed that the rotation is smeared is 1200r/
min。
The temperature of constant temperature compressive reaction in the step 11 is 100 DEG C, pressure 3MPa, reaction time 4h, described
The pressure of pressurized, heated reaction is 10MPa, and temperature is 170 DEG C, reaction time 6h, and the type of cooling is using air-cooled.
Coating layer thickness of the present invention is 1.2 μm, in 254nm ultraviolet excitation, issues high efficiency blue, transmitting main peak in 450nm,
Stability is good, and luminous intensity is high.
The foregoing is merely one embodiment of the invention, are not intended to limit the present invention, all to use equivalent substitution or equivalent transformation
Mode technical solution obtained, fall within the scope of protection of the present invention.
Claims (10)
1. a kind of preparation method of LED fluorescent powder coating, which is characterized in that preparation method is as follows:
Step 1, strontium carbonate is added in acetic acid, after being stirred to react, obtains strontium acetate acetic acid solution；
Step 2, ethyl orthosilicate and barium acetate are added in strontium acetate acetic acid solution, after mixing evenly, obtain uniform colloidal sol
Preceding liquid；
Step 3, europium carbonate is added while stirring before colloidal sol in liquid, natural subsidence, obtains with white precipitate after mixing evenly
Reaction solution；
Step 4, washes of absolute alcohol is used after white precipitate being filtered, and obtains cleaning solution；
Step 5, it is stirred evenly after filtered reaction solution being merged with cleaning solution, obtains colloidal sol dilution；
Step 6, foaming agent will be added in colloidal sol dilution, stirs evenly, form mixed liquor；
Step 7, mixed liquor is put into water-bath be evaporated under reduced pressure and carries out aeration concentration, obtain concentrate after water bath processing；
Step 8, substrate is dipped to alcoholic solution, after ultrasonic cleaning, adopts and dry wash with distilled water；
Step 9, modified organic silicon dispersion liquid is coated in substrate surface, obtains organosilicone film；
Step 10, concentrate is added dropwise and carries out rotation smearing in organosilicone film, form fluorescent powder film；
Step 11, the substrate with organosilicone film and fluorescent powder film is put into constant temperature compressive reaction in reaction kettle, then led to
Enter pressurized with hydrogen heating reaction, obtains LED fluorescent powder coating after natural cooling.
2. a kind of preparation method of LED fluorescent powder coating according to claim 1, which is characterized in that in the step
Formula are as follows: 11-12 parts of strontium carbonate, 20-35 parts of ethyl orthosilicate, 8-11 parts of barium acetate, 1-2 parts of foaming agent, the europium carbonate matter
Amount is the 1-5% of ethyl orthosilicate, and the foaming agent uses ammonium carbonate；Mixing speed in the step is 300-1200r/
Min, mixing time 30-120min.
3. a kind of preparation method of LED fluorescent powder coating according to claim 1, which is characterized in that in the step 1
Acetic acid concentration is 0.1-0.6mol/L, and acetic acid is added in the strontium carbonate until pH reaches 3-4.
4. a kind of preparation method of LED fluorescent powder coating according to claim 1, which is characterized in that in the step 3
It is 0.1-0.3mg/min that speed, which is added, in europium carbonate.
5. a kind of preparation method of LED fluorescent powder coating according to claim 1, which is characterized in that in the step 4
Washes of absolute alcohol number be 2-5 time, the dehydrated alcohol total amount is 0.8-1.1 times of acetic acid, and the dehydrated alcohol washs
Principle is a small amount of multiple.
6. a kind of preparation method of LED fluorescent powder coating according to claim 1, which is characterized in that water in the step 7
Bath temperature is 80-90 DEG C, and the concentrate is the 25-40% of mixed liquor, and the aeration concentration, which uses, heats slightly boiled mode, with
Foaming agent disperses aeration reaction combination.
7. a kind of preparation method of LED fluorescent powder coating according to claim 1, which is characterized in that in the step 8
Alcoholic solution uses one of ethyl alcohol, propyl alcohol, isopropanol, and the supersonic frequency is 30-60kHz, ultrasonic time 5-15min.
8. a kind of preparation method of LED fluorescent powder coating according to claim 1, which is characterized in that in the step 9
Modified organic silicon dispersion liquid uses modified organic silicon concentration for the ethanol solution of 3-11%, and the coated weight of the substrate surface is
0.1-0.7mg/cm2。
9. a kind of preparation method of LED fluorescent powder coating according to claim 1, which is characterized in that in the step 10
Concentrate coated weight be 0.5-1.2mg/cm2, the revolving speed that the rotation is smeared is 900-1500r/min.
10. a kind of preparation method of LED fluorescent powder coating according to claim 1, which is characterized in that in the step 11
The temperature of constant temperature compressive reaction be 80-120 DEG C, pressure 2-4MPa, reaction time 2-4h, pressurized, heated reaction
Pressure is 9-11MPa, and temperature is 150-180 DEG C, reaction time 3-8h, and the type of cooling is using air-cooled.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202153536U (en) * | 2011-07-20 | 2012-02-29 | 福建泰德视讯数码科技有限公司 | High power LED packaging structure |
| CN103788947A (en) * | 2012-10-29 | 2014-05-14 | 海洋王照明科技股份有限公司 | Silicate luminescence material and preparation method thereof |
| CN105199728A (en) * | 2015-06-01 | 2015-12-30 | 井冈山大学 | Novel Eu<3+> and Mn<2+> co-doped tungstate red fluorescent material and preparation method thereof |
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2016
- 2016-09-19 CN CN201610830207.0A patent/CN106206913B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202153536U (en) * | 2011-07-20 | 2012-02-29 | 福建泰德视讯数码科技有限公司 | High power LED packaging structure |
| CN103788947A (en) * | 2012-10-29 | 2014-05-14 | 海洋王照明科技股份有限公司 | Silicate luminescence material and preparation method thereof |
| CN105199728A (en) * | 2015-06-01 | 2015-12-30 | 井冈山大学 | Novel Eu<3+> and Mn<2+> co-doped tungstate red fluorescent material and preparation method thereof |
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