CN103044892B - Fluorescent and transparent polycarbonate grating for LED (light-emitting diode) and preparation method for same - Google Patents
Fluorescent and transparent polycarbonate grating for LED (light-emitting diode) and preparation method for same Download PDFInfo
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Abstract
The invention provides a preparation method for a fluorescent and transparent polycarbonate grating for an LED (light-emitting diode). The materials of the fluorescent and transparent polycarbonate grating for an LED are composed of polycarbonate, fluorescent powder, an antioxidant, a coupling agent and a light dispersing agent. The fluorescent and transparent polycarbonate grating for an LED is formed by performing the preparation processes of sieving, preparing, mixing, drying, matching with auxiliaries, mixing, banburying, forming, annealing, cutting, etching and the like on the composition materials. The fluorescent and transparent polycarbonate grating can be used for an LED lamp bead/lamp, for adjusting the colour temperature of the LED, and solving the problems of the glare of the LED, the non-uniform distribution of the traditional silica gel fluorescent powder, and the like. The problem of non-uniform coating of the fluorescent powder is effectively solved, so that the light-emitting efficiency, the service life and the light spectrum stability of the white-light LED are improved; and moreover, the fluorescent and transparent polycarbonate grating is relatively simple in structure and preparation process, high in reliability, low in cost, good in plasticity and capable of being widely applied to LED manufacturing, as well as opens up unprecedented flexibility and creativity for the field of light sources.
Description
Technical field
The present invention relates to LED luminescent material preparation and semiconductor lighting, particularly relate to a kind of preparation method that can be used for the fluorescent transparent polycarbonate grating of great power LED illumination field.
Background technology
The remarkable advantages such as white light LEDs is high with its efficiency, power consumption is little, the life-span is long, solid-state energy-conservation, environmental protection, are considered to " green illumination light source ", estimate to become the third generation lighting source after continuous incandescent light, luminescent lamp, have huge development potentiality.Current domestic enterprise generally adopt large power white light LED mainly on blue-light LED chip the method for packing of drop fluorescent material realize white light, but the applied thickness of fluorescent material and shape are difficult to control in this encapsulation process, cause the homogeneity of LED component colour temperature still undesirable, the angle colour temperature difference of even single LEDs can arrive 800K greatly, and the colour temperature difference that human eye can be differentiated is 50-100K.On the other hand, existing LED lamp bead/light fixture generally adopts and allows LED light source directly emit in lighting space (being generally ground), because LED direct projection light is out uneven, larger to people's Eye irritation, have a strong impact on the illuminating effect of LED lamp, easily cause eye strain even visual deterioration, light pollution---glare problem that LED lamp bead/light fixture often exists that Here it is.
Chinese invention patent CN102337017A discloses a kind of polycarbonate compositions and the application thereof with LED light transition function, it is characterized in that polycarbonate resin, (additive comprises additive: fluorescent material, fire retardant, oxidation inhibitor, releasing agent, weather resisting agent) mix with certain proportion, employing screw extrusion press melt extrudes, coupling agent and dispersion agent is not had in these auxiliary agents, fluorescent material can be caused in the process of extrusion moulding to disperse uneven, thus cause polycarbonate compositions transmittance to decline, be difficult to the light-converting material obtaining excellent property, and disadvantageous effect can be caused to the optical property of material after life-time service.
Summary of the invention
The object of the invention is to for above-mentioned existing problems and deficiency, not only thickness is even, smooth surface, fluorescent material are evenly distributed to provide a kind of fluorescence sheet material, and fluorescence sheet surface has specific Grating Design, this fluorescence sheet material is encapsulated into the colour temperature that effectively can control LED lamp bead/light fixture in LED lamp bead/light fixture, effectively solves LED lamp bead/light fixture glare problem simultaneously.
Another object of the present invention is to provide a kind of method preparing LED fluorescent transparent polycarbonate condensing diaphragm newly, this method can make fluorescent material be evenly distributed in polycarbonate resin, and this method can be used for the fluorescent polycarbonate polymkeric substance making different shape lens, lamp outer casing.
Technical scheme of the present invention is achieved in that
Fluorescent transparent polycarbonate grating for LED of the present invention, is characterized in that described fluorescent transparent polycarbonate grating comprises following component in mass ratio:
Polycarbonate 48%-94.4%;
Fluorescent material 5%-49.5%;
Oxidation inhibitor 0.1%-1.5%;
Light diffusing agent 0.5%-1%.
Wherein, described fluorescent material ratio is 5%-49.5%, and yellow fluorescent powder blending ratio is that in 10%-25%, effect is best in scope, reaches optimum regime when yellow fluorescent powder adding proportion is 20%.
If add red fluorescence powder in yellow fluorescent powder, then yellow fluorescent powder blending ratio effect in scope 10%-25% is best, when yellow fluorescent powder adding proportion is 20%, reaches optimum regime when red fluorescence powder adding proportion is 2%.
Fluorescent material is yellow fluorescent powder (YAG:Ce3+, yttrium aluminum garnet structure), or yellow fluorescent powder (YAG:Ce3+, yttrium aluminum garnet structure) and red fluorescence powder ((Ca, Sr, Ba) 2Si5N8:Eu2+, metastannic acid salt structure red fluorescence powder) mixture, or yellow fluorescent powder (YAG:Ce3+, yttrium aluminum garnet structure) and red fluorescence powder ((Ca, Sr) AlSiN3:Eu2+, red fluorescence powder based on nitride) mixture, or yellow fluorescent powder (YAG:Ce3+, yttrium aluminum garnet structure), red fluorescence powder ((Ca, Sr, Ba) 2Si5N8:Eu2+, metastannic acid salt structure red fluorescence powder) and red fluorescence powder ((Ca, Sr) AlSiN3:Eu2+, red fluorescence powder based on nitride) mixture of three.Wherein, the mixture of yellow fluorescent powder and yellowish red color fluorescent material accounts for the 5%-49.5% of total mass, and the particle diameter of fluorescent material is 9-15um.
Light diffusing agent is organosilicon light diffusing agent, organosilicon light diffusing agent is the regular ball-type micro mist of pure white, three-dimensional molecular chain can be formed in resin, effective dispersion and absorption fluorescent material, make it to be uniformly distributed, eliminate hot spot yellow circle, improve optical throughput, the rheological of resin can be improved simultaneously, improve yield rate and consistence, be different from traditional technology and utilize refraction of light to reach to deluster spot object.
Transmittance >=91.0% of the polycarbonate in fluorescent transparent polycarbonate, the particle diameter of polycarbonate powder is 30-90um.
The preparation method of the fluorescent transparent polycarbonate grating for LED of the present invention, is characterized in that comprising the following steps:
A) sieve material, selects with 150 object testing sieves the polycarbonate powder that particle diameter is 30-90um;
B) get the raw materials ready, taking particle diameter is in mass ratio 30-90um polycarbonate powder, fluorescent material, obtains raw material;
C) batch mixing, inserts the raw material taken in frequency conversion planetary ball mill and mixes, and frequency conversion planetary ball mill rotating speed is 160-250r/min, and mixing time is 1-5h, obtains compound;
D) dry, compound is put into vacuum constant temperature loft drier dry, drying temperature is 50-120 DEG C, and time of drying is 3-20h, obtains dry compound.The maximum moisture content <0.020% of polycarbonate powder;
E) join auxiliary agent, take four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and three (2,4-di-tert-butyl-phenyl) phosphorous acid ester or butylated hydroxytoluenes in mass ratio, light diffusing agent, mixes and obtains auxiliary agent;
F) mix, by the compound of drying and auxiliary agent mixing, obtain the raw material mixed;
G) banburying, joins in Banbury mixer by the raw material mixed in F, banburying 8-20 minute, and banburying temperature is 200-300 DEG C, and Banbury mixer rotating speed is 20-60r/min;
H) shaping, material after banburying is put into the vulcanizer compression moulding of being furnished with mould, vulcanizer temperature is 150-280 DEG C, pressure is 10-30MPa, deflation time is 30-500 second, and curing time is 30-500 second, and obtaining thickness is 0.5-50mm, diameter is 50-100mm, and the effigurate fluorescent transparent polycarbonate material of tool;
I) anneal, under in type fluorescent transparent polycarbonate material being positioned over certain temperature, Slow cooling is annealed, and obtains hard column fluorescent transparent polycarbonate material;
J) the hard column fluorescent transparent polycarbonate material prepared being cut into thickness is 0.5-2mm, and diameter is the fluorescent transparent polycarbonate sheet of 50-100mm, and by two surface finish of fluorescent transparent polycarbonate sheet;
K) delete after above-mentioned fluorescent transparent polycarbonate sheet wherein a surface finish with laser ablation Cheng Guang, raster shape can be cylindricality, trilateral, trapezoidal, obtains having under the exciting of short wavelength, short wavelength can be converted to long wavelength and to obtain the LED fluorescent transparent polycarbonate sheet that specific refractory power can be the special optical structure of 1.50 ~ 1.85 high refractive index.
The present invention is owing to have employed rear-earth-doped fluorescent transparent polycarbonate as LED novel encapsulated material, and encapsulation uses on the led device.LED can be solved in the problem encapsulated and use from the following aspects:
1) due to domestic enterprise generally adopt large power white light LED mainly on blue-light LED chip the method for packing of drop fluorescent material realize white light, but in this encapsulation process, the applied thickness of fluorescent material and shape are difficult to control, and cause the homogeneity of LED component colour temperature undesirable.But the present invention effectively controls shape and the thickness of fluorescent transparent polycarbonate sheet, well solve fluorescent powder coated uneven, thus improve white light LEDs luminous efficiency, work-ing life and spectrum stability.
2) LED lights for a long time and epoxy resin (or silica gel) temperature can be made to rise and occur aging, and accelerate the aging of epoxy resin (or silica gel), transparency degradation, greatly shortens the life-span of white light LEDs, and affects the luminous efficiency of LED.Compared with resin (or silica gel), fluorescent transparent polycarbonate material is more high temperature resistant, anticorrosive, plasticity-strong, in structure and chemical stability, have special performance.In addition, be directly coated on chip by the resin containing fluorescent material, under making it be in hot environment for a long time, the quantum yield of fluorescent material can reduce due to temperature quenching effect, and higher temperature also can accelerate the aging of fluorescent material.In order to obtain the more stable white light LED part of performance, fluorescent transparent polycarbonate sheet separates with chip when encapsulating by the present invention, reduces phosphor surface temperature, effective raising fluorescent material light conversion efficiency.
3) the present invention is uneven by the dazzle and Light distribation improving LED at fluorescent transparent polycarbonate sheet surface etch grating.
4) the present invention mixes by what change the mass ratio of fluorescent material and different red fluorescence powder the colour temperature and development index changing white light LEDs.
5) simultaneously, fluorescent transparent polycarbonate material has good plasticity-, by making difform mould, fluorescent transparent polycarbonate material can be processed into the light-converting material of different structure, as different shapeies such as plane, sphere, curved surfaces, for light source field has opened up unprecedented handiness and creativeness.
Compared with prior art, tool of the present invention has the following advantages and technique effect:
1) adopt fluorescent transparent polycarbonate sheet as the packaged material of white light LEDs, effectively can control shape and the thickness of fluorescent transparent polycarbonate sheet, good solution is fluorescent powder coated uneven, thus improves white light LEDs luminous efficiency, work-ing life and spectrum stability.
2) more high temperature resistant, anticorrosive, the plasticity-of fluorescent transparent polycarbonate sheet is strong, in structure and chemical stability, have special performance, improves fluorescent material at high temperature aging.Fluorescent transparent polycarbonate sheet separates with chip when encapsulating by the present invention simultaneously, reduces phosphor surface temperature, effective raising fluorescent material light conversion efficiency.
3) light diffusing agent is added in fluorescent transparent polycarbonate, its composition is organosilicon light diffusing agent, organosilicon light diffusing agent is the regular ball-type micro mist of pure white, can form three-dimensional molecular chain in resin, effective dispersion and absorption fluorescent material, make it to be uniformly distributed, eliminate hot spot yellow circle, improve optical throughput, the rheological of resin can be improved simultaneously, improve yield rate and consistence, be different from traditional technology and utilize refraction of light to reach to deluster spot object.
4) the present invention is uneven by the dazzle and Light distribation improving LED at fluorescent transparent polycarbonate sheet surface etch grating.
5) the present invention mixes by what change the mass ratio of fluorescent material and different red fluorescence powder the colour temperature and development index changing white light LEDs.
6) fluorescent transparent polycarbonate material has good plasticity-, for light source field has opened up unprecedented handiness and creativeness.
Meanwhile, prove when fluorescent material thickness is at 0.5-1mm by theory deduction and related experiment, phosphor concentration is between 10%-30%, and the LED lamp bead luminous efficiency encapsulated, colour developing coefficient reach optimum.In this patent, the per-cent of fluorescent material is that 5%-49.5% coincidence theory and requirement of experiment can meet production requirement, and the excessive requirement being constantly difficult to meet experiment and production of fluorescent material per-cent simultaneously also can cause unnecessary waste simultaneously.The per-cent of polycarbonate is 48%-94.4%, calculates the ratio of fluorescent material, oxidation inhibitor, light diffusing agent with crossing.And in Chinese invention patent CN102337017A the mass ratio of fluorescent material to be that 1-50% scope is too large be difficult to sufficient LED blue light is converted into gold-tinted to the fluorescent material with 1%-5% mass ratio, the phosphor concentration of 45%-50% mass ratio is too high simultaneously makes the LED yellow component after encapsulating higher.
In Chinese invention patent CN102337017A, auxiliary agent employs the transmitance that releasing agent can affect resin, proves that transmitance that the use of releasing agent can have influence on resin is difficult to use in the preparation of optical material in lot of documents and experiment.
And this patent uses Banbury mixer to prepare fluorescence resin material, consider that fluorescent material and polycarbonate are difficult to fully mix, and Banbury mixer can allow fluorescent material and polycarbonate fully contact, and makes fluorescent material be evenly distributed in polycarbonate.Secondly in the encapsulation of fluorescent material price height, consumption is few, if use twin screw extruder once to feed intake can cause unnecessary waste too much.The consumption using banburying function effectively to control fluorescent material makes fluorescent material be evenly distributed in polycarbonate simultaneously.
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Accompanying drawing explanation
Fig. 1 is the structural representation of the white light LEDs that the present invention encapsulates.
Wherein, 1 be fluorescent transparent polycarbonate sheet, 2 be LED chip, 3 be electrode, 4 be epoxy resin light penetrating object, 5 be heat-radiating substrate, 6 to be reflection cup, 7 be that to fill connector, 11 be the end face, 12 of fluorescent transparent polycarbonate sheet is the bottom surface of fluorescent transparent polycarbonate sheet.
Embodiment
As shown in Figure 1, the fluorescent transparent polycarbonate grating for LED of the present invention, comprises following component in mass ratio:
Polycarbonate 48%-94.4%;
Fluorescent material 5%-49.5%;
Oxidation inhibitor 0.1%-1.5%;
Light diffusing agent 0.5%-1%.
Wherein, above-mentioned light diffusing agent is organosilicon light diffusing agent, and organosilicon light diffusing agent is the regular ball-type micro mist of pure white, and consumption is 0.5%-1%.Above-mentioned fluorescent material is the mixture of yellow fluorescent powder or red fluorescence powder or yellow fluorescent powder and red fluorescence powder.Transmittance >=91.0% of above-mentioned polycarbonate, the particle diameter of polycarbonate powder is 30-90um.Above-mentioned oxidation inhibitor is butylated hydroxytoluene (antioxidant 264) or four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] mixture of pentaerythritol ester (primary antioxidant 1010) and three (2,4-di-tert-butyl-phenyl) phosphorous acid ester (auxiliary antioxidant 168).
The preparation method of the fluorescent transparent polycarbonate grating for LED of the present invention, comprises the following steps:
A) sieve material, selects with 150 object testing sieves the polycarbonate powder that particle diameter is 30-90um;
B) get the raw materials ready, taking particle diameter is in mass ratio 30-90um polycarbonate powder, fluorescent material, obtains raw material;
C) batch mixing, inserts the raw material taken in frequency conversion planetary ball mill and mixes, and frequency conversion planetary ball mill rotating speed is 160-250r/min, and mixing time is 1-5h, obtains compound;
D) dry, compound is put into vacuum constant temperature loft drier dry, drying temperature is 50-120 DEG C, and time of drying is 3-20h, obtains dry compound.The maximum moisture content <0.020% of polycarbonate powder;
E) auxiliary agent is joined, take four [β-(3 in mass ratio, 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (primary antioxidant 1010) and three (2,4-di-tert-butyl-phenyl) phosphorous acid ester (auxiliary antioxidant 168) or butylated hydroxytoluene (antioxidant 264), light diffusing agent, mixes and obtains auxiliary agent;
F) mix, by the compound of drying and auxiliary agent mixing, obtain the raw material mixed;
G) banburying, joins in Banbury mixer by the raw material mixed in F, banburying 8-20 minute, and banburying temperature is 200-300 DEG C, and Banbury mixer rotating speed is 20-60r/min;
H) shaping, material after banburying is put into the vulcanizer compression moulding of being furnished with mould, vulcanizer temperature is 150-280 DEG C, pressure is 10-30MPa, deflation time is 30-500 second, and curing time is 30-500 second, and obtaining thickness is 0.5-50mm, diameter is 50-100mm, and the effigurate fluorescent transparent polycarbonate material of tool;
I) anneal, under in type fluorescent transparent polycarbonate material being positioned over certain temperature, Slow cooling is annealed, and obtains hard column fluorescent transparent polycarbonate material;
J) the hard column fluorescent transparent polycarbonate material prepared being cut into thickness is 0.5-2mm, and diameter is the fluorescent transparent polycarbonate sheet of 50-100mm, and by two surface finish of fluorescent transparent polycarbonate sheet;
K) delete after above-mentioned fluorescent transparent polycarbonate sheet wherein a surface finish with laser ablation Cheng Guang, raster shape can be cylindricality, trilateral, trapezoidal, obtains having under the exciting of short wavelength, short wavelength can be converted to long wavelength and to obtain the LED fluorescent transparent polycarbonate sheet that specific refractory power can be the special optical structure of 1.50 ~ 1.85 high refractive index.
Embodiment one:
The raw material of configuration preparation needed for product of the present invention: polycarbonate powder, yellow fluorescent powder, antioxidant 1010, irgasfos 168, organosilicon light diffusing agent, the concrete ratio of each component is as described in Table 1.Implementation step is as follows:
A) sieve material, selects with 150 object testing sieves the polycarbonate powder that particle diameter is 30-90um;
B) get the raw materials ready, taking particle diameter by example in table 11 constituent mass ratio is 30-90um polycarbonate, yellow fluorescent powder;
C) batch mixing, will take polycarbonate powder and fluorescent material and insert in frequency conversion planetary ball mill and mix, frequency conversion planetary ball mill rotating speed is 160-250r/min, and mixing time is 1-5h, obtains compound;
D) dry, compound is put into vacuum constant temperature loft drier dry, drying temperature is 50-120 DEG C, and time of drying is 3-20h, obtains dry compound.The maximum moisture content <0.020% of polycarbonate powder;
E) auxiliary agent is joined, antioxidant 1010, irgasfos 168, light diffusing agent is taken by example in table 11 constituent mass ratio, wherein antioxidant 1010 can change mass ratio according to actual demand within the scope of 0.1%-0.5%, irgasfos 168 can change mass ratio according to actual demand within the scope of 0.05%-1%, and light diffusing agent can change mass ratio according to actual demand within the scope of 0.5%-1%;
F) mix, by the compound of drying and auxiliary agent mixing, obtain the raw material mixed;
G) banburying, joins in Banbury mixer by the raw material mixed in F, banburying 8-20 minute, and banburying temperature is 200-300 DEG C, and Banbury mixer rotating speed is 20-60r/min;
H) shaping, material after banburying is put into the vulcanizer compression moulding of being furnished with mould, vulcanizer temperature is 150-280 DEG C, pressure is 10-30MPa, deflation time is 30-500 second, and curing time is 30-500 second, and obtaining thickness is 0.5-50mm, diameter is 50-100mm, and the effigurate fluorescent transparent polycarbonate of tool;
I) anneal, in type fluorescent transparent polycarbonate is positioned over Slow cooling under certain temperature, obtains hard column fluorescent transparent polycarbonate;
J) be 0.5-2mm by obtained fluorescent transparent polycarbonate with being laser-cut into thickness, diameter is the fluorescent transparent polycarbonate sheet of 50-100mm, and by the end face 11 of fluorescent transparent polycarbonate sheet 1 and bottom surface 12 polishing;
K) with laser, the end face 11 of fluorescent transparent polycarbonate sheet is etched into the grating with special construction, wherein special construction can be cylindricality, trilateral, trapezoidal, obtains the LED fluorescent transparent polycarbonate sheet 1 with special optical structure.
The LED fluorescent transparent polycarbonate sheet 1 with special optical structure is encapsulated in LED the LED lamp bead/fitting structure obtaining adjustable color.
Embodiment 2:
Only by step B in embodiment 1) and E) in batching become by example in table 12 constituent mass than batching, all the other are all same as the description of embodiment 1.
Embodiment 3:
Only by step B in embodiment 1) and E) in batching become by example in table 13 constituent mass than batching, all the other are all same as the description of embodiment 1.
Embodiment 4:
Only by step B in embodiment 1) and E) in batching become by example in table 14 constituent mass than batching, all the other are all same as the description of embodiment 1.
Embodiment 5:
Only by step B in embodiment 1) and E) in batching become by example in table 15 constituent mass than batching, all the other are all same as the description of embodiment 1.
Embodiment 6:
Only by step B in embodiment 1) and E) in batching become by example in table 16 constituent mass than batching, all the other are all same as the description of embodiment 1.
Embodiment 7:
Only by step B in embodiment 1) and E) in batching become by example in table 17 constituent mass than batching, all the other are all same as the description of embodiment 1.
Embodiment 8:
The raw material of configuration preparation needed for product of the present invention: polycarbonate powder, yellow fluorescent powder, antioxidant 264, organosilicon light diffusing agent, the concrete ratio of each component is as described in Table 1.Implementation step is as follows:
A) sieve material, selects with 150 object testing sieves the polycarbonate powder that particle diameter is 30-90um;
B) get the raw materials ready, taking particle diameter by example in table 18 constituent mass ratio is 30-90um polycarbonate, yellow fluorescent powder;
C) batch mixing, will take polycarbonate powder and fluorescent material and insert in frequency conversion planetary ball mill and mix, frequency conversion planetary ball mill rotating speed is 160-250r/min, and mixing time is 1-5h, obtains compound;
D) dry, compound is put into vacuum constant temperature loft drier dry, drying temperature is 50-120 DEG C, and time of drying is 3-20h, obtains dry compound.The maximum moisture content <0.020% of polycarbonate powder;
E) auxiliary agent is joined, antioxidant 264, light diffusing agent is taken by example in table 18 constituent mass ratio, wherein antioxidant 264 can change mass ratio according to actual demand within the scope of 0.1%-1%, and light diffusing agent can change mass ratio according to actual demand within the scope of 0.5%-1%;
F) mix, by the compound of drying and auxiliary agent mixing, obtain the raw material mixed;
G) banburying, joins in Banbury mixer by the raw material mixed in F, banburying 8-20 minute, and banburying temperature is 200-300 DEG C, and Banbury mixer rotating speed is 20-60r/min;
H) shaping, material after banburying is put into the vulcanizer compression moulding of being furnished with mould, vulcanizer temperature is 150-280 DEG C, pressure is 10-30MPa, deflation time is 30-500 second, and curing time is 30-500 second, and obtaining thickness is 0.5-50mm, diameter is 50-100mm, and the effigurate fluorescent transparent polycarbonate of tool;
I) anneal, in type fluorescent transparent polycarbonate is positioned over Slow cooling under certain temperature, obtains hard column fluorescent transparent polycarbonate;
J) be 0.5-2mm by obtained fluorescent transparent polycarbonate with being laser-cut into thickness, diameter is the fluorescent transparent polycarbonate sheet of 50-100mm, and by the end face 11 of fluorescent transparent polycarbonate sheet and bottom surface 12 polishing;
K) with laser, the end face 11 of fluorescent transparent polycarbonate sheet 1 is etched into the grating with special construction, wherein special construction can be cylindricality, trilateral, trapezoidal, obtains the LED fluorescent transparent polycarbonate sheet with special optical structure.
The LED fluorescent transparent polycarbonate sheet with special optical structure is encapsulated in LED the LED lamp bead/fitting structure obtaining adjustable color.
Embodiment 9:
Only by step B in embodiment 8) and E) in batching become by example in table 19 constituent mass than batching, all the other are all same as the description of embodiment 8.
Embodiment 10:
Only by step B in embodiment 8) and E) in batching become by example in table 1 10 constituent mass than batching, all the other are all same as the description of embodiment 8.
Embodiment 11:
Only by step B in embodiment 8) and E) in batching become by example in table 1 11 constituent mass than batching, all the other are all same as the description of embodiment 8.
Embodiment 12:
Only by step B in embodiment 8) and E) in batching become by example in table 1 12 constituent mass than batching, all the other are all same as the description of embodiment 8.
Embodiment 13:
Only by step B in embodiment 8) and E) in batching become by example in table 1 13 constituent mass than batching, all the other are all same as the description of embodiment 8.
Embodiment 14:
Only by step B in embodiment 8) and E) in batching become by example in table 1 14 constituent mass than batching, all the other are all same as the description of embodiment 8.
Embodiment 15:
The raw material of configuration preparation needed for product of the present invention: polycarbonate powder, yellow fluorescent powder, red fluorescence powder, antioxidant 1010, irgasfos 168, organosilicon light diffusing agent, the concrete ratio of each component is as described in Table 1.Implementation step is as follows:
A) sieve material, selects with 150 object testing sieves the polycarbonate powder that particle diameter is 30-90um;
B) get the raw materials ready, taking particle diameter by example in table 1 15 constituent mass ratio is 30-90um polycarbonate, yellow fluorescent powder, red fluorescence powder;
C) batch mixing, will take polycarbonate powder and fluorescent material and insert in frequency conversion planetary ball mill and mix, frequency conversion planetary ball mill rotating speed is 160-250r/min, and mixing time is 1-5h, obtains compound;
D) dry, compound is put into vacuum constant temperature loft drier dry, drying temperature is 50-120 DEG C, and time of drying is 3-20h, obtains dry compound.The maximum moisture content <0.020% of polycarbonate powder;
E) auxiliary agent is joined, antioxidant 1010, irgasfos 168, light diffusing agent is taken by example in table 1 15 constituent mass ratio, wherein antioxidant 1010 can change mass ratio according to actual demand within the scope of 0.1%-0.5%, irgasfos 168 can change mass ratio according to actual demand within the scope of 0.05%-1%, and light diffusing agent can change mass ratio according to actual demand within the scope of 0.5%-1%;
F) mix, by the compound of drying and auxiliary agent mixing, obtain the raw material mixed;
G) banburying, joins in Banbury mixer by the raw material mixed in F, banburying 8-20 minute, and banburying temperature is 200-300 DEG C, and Banbury mixer rotating speed is 20-60r/min;
H) shaping, material after banburying is put into the vulcanizer compression moulding of being furnished with mould, vulcanizer temperature is 150-280 DEG C, pressure is 10-30MPa, deflation time is 30-500 second, and curing time is 30-500 second, and obtaining thickness is 0.5-50mm, diameter is 50-100mm, and the effigurate fluorescent transparent polycarbonate of tool;
I) anneal, in type fluorescent transparent polycarbonate is positioned over Slow cooling under certain temperature, obtains hard column fluorescent transparent polycarbonate;
J) be 0.5-2mm by obtained fluorescent transparent polycarbonate with being laser-cut into thickness, diameter is the fluorescent transparent polycarbonate sheet 1 of 50-100mm, and by the end face 11 of fluorescent transparent polycarbonate sheet 1 and bottom surface 12 polishing;
K) with laser, the end face 11 of fluorescent transparent polycarbonate sheet is etched into the grating with special construction, wherein special construction can be cylindricality, trilateral, trapezoidal, obtains the LED fluorescent transparent polycarbonate sheet with special optical structure.
The LED fluorescent transparent polycarbonate sheet with special optical structure is encapsulated in LED the LED lamp bead/fitting structure obtaining adjustable color.
Embodiment 16:
Only by step B in embodiment 15) and E) in batching become by example in table 1 16 constituent mass than batching, all the other are all same as the description of embodiment 15.
Embodiment 17:
Only by step B in embodiment 15) and E) in batching become by example in table 1 17 constituent mass than batching, all the other are all same as the description of embodiment 15.
Embodiment 18:
Only by step B in embodiment 15) and E) in batching become by example in table 1 18 constituent mass than batching, all the other are all same as the description of embodiment 15.
Embodiment 19:
Only by step B in embodiment 15) and E) in batching become by example in table 1 19 constituent mass than batching, all the other are all same as the description of embodiment 15.
Embodiment 20:
Only by step B in embodiment 15) and E) in batching become by example in table 1 20 constituent mass than batching, all the other are all same as the description of embodiment 15.
Embodiment 21:
Only by step B in embodiment 15) and E) in batching become by example in table 1 21 constituent mass than batching, all the other are all same as the description of embodiment 15.
Embodiment 22:
The raw material of configuration preparation needed for product of the present invention: polycarbonate powder, yellow fluorescent powder, red fluorescence powder, antioxidant 264, organosilicon light diffusing agent, the concrete ratio of each component is as described in Table 1.Implementation step is as follows:
A) sieve material, selects with 150 object testing sieves the polycarbonate powder that particle diameter is 30-90um;
B) get the raw materials ready, taking particle diameter by example in table 1 22 constituent mass ratio is 30-90um polycarbonate, yellow fluorescent powder and red fluorescence powder;
C) batch mixing, will take polycarbonate powder and fluorescent material and insert in frequency conversion planetary ball mill and mix, frequency conversion planetary ball mill rotating speed is 160-250r/min, and mixing time is 1-5h, obtains compound;
D) dry, compound is put into vacuum constant temperature loft drier dry, drying temperature is 50-120 DEG C, and time of drying is 3-20h, obtains dry compound.The maximum moisture content <0.020% of polycarbonate powder;
E) auxiliary agent is joined, antioxidant 264, light diffusing agent is taken by example in table 1 22 constituent mass ratio, wherein antioxidant 264 can change mass ratio according to actual demand within the scope of 0.1%-1%, and light diffusing agent can change mass ratio according to actual demand within the scope of 0.5%-1%;
F) mix, by the compound of drying and auxiliary agent mixing, obtain the raw material mixed;
G) banburying, joins in Banbury mixer by the raw material mixed in F, banburying 8-20 minute, and banburying temperature is 200-300 DEG C, and Banbury mixer rotating speed is 20-60r/min;
H) shaping, material after banburying is put into the vulcanizer compression moulding of being furnished with mould, vulcanizer temperature is 150-280 DEG C, pressure is 10-30MPa, deflation time is 30-500 second, and curing time is 30-500 second, and obtaining thickness is 0.5-50mm, diameter is 50-100mm, and the effigurate fluorescent transparent polycarbonate of tool;
I) anneal, in type fluorescent transparent polycarbonate is positioned over Slow cooling under certain temperature, obtains hard column fluorescent transparent polycarbonate;
J) be 0.5-2mm by obtained fluorescent transparent polycarbonate with being laser-cut into thickness, diameter is the fluorescent transparent polycarbonate sheet of 50-100mm, and by the end face 11 of fluorescent transparent polycarbonate sheet and bottom surface 12 polishing;
K) with laser, the end face 11 of fluorescent transparent polycarbonate sheet is etched into the grating with special construction, wherein special construction can be cylindricality, trilateral, trapezoidal, obtains the LED fluorescent transparent polycarbonate sheet 1 with special optical structure.
The LED fluorescent transparent polycarbonate sheet 1 with special optical structure is encapsulated in LED the LED lamp bead/fitting structure obtaining adjustable color.
Embodiment 23:
Only by step B in embodiment 22) and E) in batching become by example in table 1 23 constituent mass than batching, all the other are all same as the description of embodiment 22.
Embodiment 24:
Only by step B in embodiment 22) and E) in batching become by example in table 1 24 constituent mass than batching, all the other are all same as the description of embodiment 22.
Embodiment 25:
Only by step B in embodiment 22) and E) in batching become by example in table 1 25 constituent mass than batching, all the other are all same as the description of embodiment 22.
Embodiment 26:
Only by step B in embodiment 22) and E) in batching become by example in table 1 26 constituent mass than batching, all the other are all same as the description of embodiment 22.
Embodiment 27:
Only by step B in embodiment 22) and E) in batching become by example in table 1 27 constituent mass than batching, all the other are all same as the description of embodiment 22.
Fluorescent material in above-mentioned example all can be bought from commercially available channel.
This fluorescent transparent polycarbonate sheet can be good at the colour temperature and the solution glare problem that change LED, and this present invention is relatively simple simultaneously, and reliability is high, can be widely used in LED and manufacture.
Table 1 each embodiment constituent mass per-cent
| Polycarbonate | Yellow fluorescent powder | Red fluorescence powder | Antioxidant 1010 | Irgasfos 168 | Antioxidant 264 | Light diffusing agent | |
| Example 1 | 93% | 5% | — | 0.5% | 1% | — | 0.5% |
| Example 2 | 88% | 10% | — | 0.5% | 1% | — | 0.5% |
| Example 3 | 83% | 15% | — | 0.5% | 1% | — | 0.5% |
| Example 4 | 78% | 20% | — | 0.5% | 1% | — | 0.5% |
| Example 5 | 73% | 25% | — | 0.5% | 1% | — | 0.5% |
| Example 6 | 68% | 30% | — | 0.5% | 1% | — | 0.5% |
| Example 7 | 53% | 45% | — | 0.5% | 1% | — | 0.5% |
| Example 8 | 94% | 5% | — | — | — | 0.5% | 0.5% |
| Example 9 | 89% | 10% | — | — | — | 0.5% | 0.5% |
| Example 10 | 84% | 15% | — | — | — | 0.5% | 0.5% |
| Example 11 | 79% | 20% | — | — | — | 0.5% | 0.5% |
| Example 12 | 74% | 25% | — | — | — | 0.5% | 0.5% |
| Example 13 | 69% | 30% | — | — | — | 0.5% | 0.5% |
| Example 14 | 54% | 45% | — | — | — | 0.5% | 0.5% |
| Example 15 | 92.5% | 5% | 0.5% | 0.5% | 1% | — | 0.5% |
| Example 16 | 87% | 10% | 1% | 0.5% | 1% | — | 0.5% |
| Example 17 | 81.5% | 15% | 1.5% | 0.5% | 1% | — | 0.5% |
| Example 18 | 76% | 20% | 2% | 0.5% | 1% | — | 0.5% |
| Example 19 | 70.5% | 25% | 2.5% | 0.5% | 1% | — | 0.5% |
| Example 20 | 65% | 30% | 3% | 0.5% | 1% | — | 0.5% |
| Example 21 | 48.5% | 45% | 4.5% | 0.5% | 1% | — | 0.5% |
| Example 22 | 93.5% | 5% | 0.5% | — | — | 0.5% | 0.5% |
| Example 23 | 88% | 10% | 1% | — | — | 0.5% | 0.5% |
| Example 24 | 82.5% | 15% | 1.5% | — | — | 0.5% | 0.5% |
| Example 25 | 77% | 20% | 2% | — | — | 0.5% | 0.5% |
| Example 26 | 71.5% | 25% | 2.5% | — | — | 0.5% | 0.5% |
| Example 27 | 66% | 30% | 3% | — | — | 0.5% | 0.5% |
| Example 28 | 49.5% | 45% | 4.5% | — | — | 0.5% | 0.5% |
The present invention is described by embodiment, but the present invention is not construed as limiting, with reference to description of the invention, other changes of the disclosed embodiments, as the professional person for this area easily expects, such change should belong within the scope of the claims in the present invention restriction.
Claims (1)
1., for a preparation method for the fluorescent transparent polycarbonate grating of LED, it is characterized in that comprising the following steps:
A) sieve material, selects with 150 object testing sieves the polycarbonate powder that particle diameter is 30-90um;
B) get the raw materials ready, taking particle diameter is in mass ratio 30-90um polycarbonate powder, fluorescent material, wherein polycarbonate 48%-94.4%, and fluorescent material 5%-49.5% obtains raw material;
C) batch mixing, inserts the raw material taken in frequency conversion planetary ball mill and mixes, and frequency conversion planetary ball mill rotating speed is 160-250r/min, and mixing time is 1-5h, obtains compound;
D) dry, compound is put into vacuum constant temperature loft drier dry, drying temperature is 50-120 DEG C, and time of drying is 3-20h, obtains dry compound, the maximum moisture content <0.020% of polycarbonate powder;
E) join auxiliary agent, take oxidation inhibitor four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and three (2,4-di-tert-butyl-phenyl) phosphorous acid ester in mass ratio; Or oxidation inhibitor butylated hydroxytoluene, light diffusing agent, wherein oxidation inhibitor 0.1%-1.5%, light diffusing agent 0.5%-1% mix and obtain auxiliary agent;
F) mix, by the compound of drying and auxiliary agent mixing, obtain the raw material mixed;
G) banburying, joins in Banbury mixer by the raw material mixed in F, banburying 8-20 minute, and banburying temperature is 200-300 DEG C, and Banbury mixer rotating speed is 20-60r/min;
H) shaping, material after banburying is put into the vulcanizer compression moulding of being furnished with mould, vulcanizer temperature is 150-280 DEG C, pressure is 10-30MPa, deflation time is 30-500 second, and curing time is 30-500 second, and obtaining thickness is 0.5-50mm, diameter is 50-100mm, and the effigurate fluorescent transparent polycarbonate material of tool;
I) anneal, under in type fluorescent transparent polycarbonate material being positioned over certain temperature, Slow cooling is annealed, and obtains hard column fluorescent transparent polycarbonate material;
J) the hard column fluorescent transparent polycarbonate material prepared being cut into thickness is 0.5-2mm, and diameter is the fluorescent transparent polycarbonate sheet of 50-100mm, and by two surface finish of fluorescent transparent polycarbonate sheet;
K) delete after above-mentioned fluorescent transparent polycarbonate sheet wherein a surface finish with laser ablation Cheng Guang, raster shape is cylindricality, trilateral, trapezoidal, obtains having under the exciting of short wavelength, short wavelength can be converted to long wavelength and to obtain the LED fluorescent transparent polycarbonate sheet that specific refractory power is the special optical structure of 1.50 ~ 1.85 high refractive index.
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| CN103311417A (en) * | 2013-06-04 | 2013-09-18 | 左洪波 | Phosphor coating method for high-power LEDs |
| CN105431487A (en) * | 2013-06-30 | 2016-03-23 | 三菱瓦斯化学株式会社 | Polycarbonate resin composition, and fluorescence detection/analysis substrate produced using polycarbonate resin composition |
| CN104566190A (en) * | 2014-11-25 | 2015-04-29 | 苏州新区佳合塑胶有限公司 | Automobile brake lamp shade preparing method |
| CN105674210A (en) * | 2016-03-08 | 2016-06-15 | 安徽康佳绿色照明技术有限公司 | 60-degree lens of LED lamp and manufacturing method of 60-degree lens of LED lamp |
| CN107013882B (en) * | 2017-03-06 | 2019-06-25 | 华南农业大学 | A kind of plant lamp turning photoreactivation translucent cover and its application |
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