CN106189166A - A kind of LED and preparation method thereof - Google Patents
A kind of LED and preparation method thereof Download PDFInfo
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- CN106189166A CN106189166A CN201610573871.1A CN201610573871A CN106189166A CN 106189166 A CN106189166 A CN 106189166A CN 201610573871 A CN201610573871 A CN 201610573871A CN 106189166 A CN106189166 A CN 106189166A
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Abstract
The application relates to lighting technical field, specifically, relates to a kind of LED and preparation method thereof.The LED of the application includes LED illuminator and the lampshade covering at outside LED chip, containing blue-light absorbers in the raw material of lampshade, containing the rare earth oxide that particle size range is 5～60nm in blue-light absorbers；The surface configuration of lampshade has environmental purification function layer, containing doped with rare-earth elements and the photocatalyst of titanium dioxide of boron element in environmental purification function layer.The LED of the application not only reduces the blue light harm to human eye, and just can reach the effect of the depollution of environment while using, and decreases the toxic gas harm to human body.
Description
Technical field
The application relates to lighting technical field, specifically, relates to a kind of LED and preparation method thereof.
Background technology
Conventional incandescent (tengsten lamp) power consumption is high, the life-span is short, under the overall situation that global resources are nervous, the most gradually by various countries
Government forbids producing, and substitute products are electronic energy-saving lamps therewith, although electronic energy-saving lamp improves energy-saving effect, but owing to using
The heavy metal element of many pollution environment, runs counter to again the main trend of environmental conservation.High speed development LED along with LED technology
Illumination is increasingly becoming the only choosing of novel green illumination.LED principle of luminosity, energy-saving and environmental protection aspect on be all far superior to
Traditional lighting products.
Owing to LED is cold light source, semiconductor lighting self does not has any pollution to environment, compared with electric filament lamp, fluorescent lamp,
Electric energy can reach more than 90%.Under same brightness, power consumption is only the 1/10 of ordinary incandescent lamp, the 1/ of fluorescent tube
2.The light sent yet with LED is shortwave high-energy light source, is blue, purple light, exposes for a long time in visible light
Likely the retina of people is caused damage among this light.
Photocatalyst is the total of a kind of photosemiconductor material with photo-catalysis function with Nano titanium dioxide as representative
Claiming, it coats substrate surface, under the effect of ultraviolet light, produces strong catalytic degradation function: air of effectively degrading
Middle toxic and harmful；Can effectively kill various bacteria, and the toxin that can antibacterial or fungus be discharged decomposes and innoxious place
Reason；It is also equipped with except functions such as formaldehyde, deodorization, anti-soil, purification air simultaneously.But, photocatalyst of titanium dioxide can away from for
3.2Ev, is equivalent to the energy that the light source of wavelength 387.5nm is carried, and this wavelength drops in the wave-length coverage of ultraviolet light.At the sun
In light energy, ultraviolet light proportion is still not as good as 1/10th.Therefore, the use of photocatalyst of titanium dioxide needs harmful
Ultraviolet source excite, use more inconvenience.Accordingly, it would be desirable to it just can be able to be improved away from being reduced in the range of visible ray
Its practicality.
In order to reduce the harm of blue light in LED and there is depollution of environment effect simultaneously, special proposition the application.
Summary of the invention
The primary goal of the invention of the application is to propose a kind of LED.
Second goal of the invention of the application is to propose the preparation method of this LED.
In order to complete the purpose of the application, the technical scheme of employing is:
The application relates to a kind of LED, and described LED includes LED illuminator and covers at the lamp outside described LED chip
Cover, containing blue-light absorbers in the raw material of described lampshade, containing the rare earth that particle size range is 5～60nm in described blue-light absorbers
Oxide；The surface configuration of described lampshade has environmental purification function layer, containing rare earth doped unit in described environmental purification function layer
Element and the photocatalyst of titanium dioxide of boron element.
Preferably, described lampshade is ball bubble or fluorescent tube；The raw material preparing described lampshade is resin, it is preferred that described resin
Selected from polycarbonate resin or polymethyl methacrylate.
Preferably, described blue-light absorbers is distributed in the raw material preparing described lampshade, and described rare earth oxide is selected from oxygen
Change cerium, lanthana, praseodymium oxide, preferential oxidation cerium；At least one in lanthanum, cerium, praseodymium or neodymium of described rare earth element, preferably
Cerium.
Preferably, in described rare earth oxide, the proportion of composing of particle size range is: particle diameter is the rare earth oxide of 5～15nm
25～50 weight portions, particle diameter is rare earth oxide 10～25 weight portion of 15～30nm, and particle diameter is the rare-earth oxidation of 30～50nm
Thing 20～25 weight portion, particle diameter is rare earth oxide 20～25 weight portion of 50～60nm.
Preferably, described environmental purification function layer contains: anatase titanium dioxide powder body 90～98 weight portion, preferably 95
～97 weight portions；Rare earth oxide powder body 0.5～3 weight portion, preferably 1～1.5 weight portions；Triethyl borate 0.5～1.5
Weight portion, preferably 1～1.5 weight portions.
Preferably, also doped with carbon in the photocatalyst of titanium dioxide of described doped with rare-earth elements and boron element；Preferably
, possibly together with graphene oxide 0.6～0.9 weight portion, preferably 0.75～0.9 weight portion in described environmental purification function layer.
Preferably, in the raw material of described lampshade, the mass percent of blue-light absorbers is 0.3～2.5%, and described environment is clean
The thickness changing functional layer is 5～30 μm.
The application further relates to the preparation method of this LED, at least comprises the following steps:
(1) in proportion rare earth oxide is joined in organic solvent I, be subsequently adding coupling agent, after being dispersed through, obtain institute
State blue-light absorbers；The mass percent concentration of rare earth oxide described in described blue-light absorbers is 30%～50%；Described
Organic solvent I is selected from dimethylbenzene and the mixed solvent of Ketohexamethylene, it is preferred that the volume ratio of described dimethylbenzene and Ketohexamethylene is 4:1
～5:1；
(2) anatase titanium dioxide powder body, rare earth oxide powder body and triethyl borate are mixed in proportion laggard
Row grinds, and grinds 6～15 hours, obtain the nano-powder that particle diameter is below 10nm under conditions of 60～100 DEG C；To be prepared into
To nano-powder be scattered in organic solvent II formation colloidal sol, i.e. prepare containing the coating of described photocatalyst of titanium dioxide；Institute
State organic solvent II selected from ethyl acrylate and the mixed solvent of Ketohexamethylene, described nano-powder quality hundred in described colloidal sol
Proportion by subtraction content is 30～40%；Preferably, the volume ratio of ethyl acrylate and Ketohexamethylene is 6～8:2～4；
(3) blue-light absorbers that step (1) prepares is joined in resin, be uniformly mixing to obtain mixed material, will
Described mixed material is heated to 50～70 DEG C of dischargings, and is prepared as described lampshade；
(4) coating containing described photocatalyst of titanium dioxide prepared described cover surface application step (2),
Solidify 10～25 minutes under the uviol lamp of 100～150W；
(5) the described lampshade after solidification is assembled in described LED illuminator, obtains described LED.
Preferably, in step (3), under the conditions of 180～260 DEG C, described blue light absorption agent solution is divided 2～3 times and drip
It is added in described resin, then stirring 5～10 minutes.
Preferably, in step (3), described lampshade is ball bubble or fluorescent tube, after described mixed material discharging, 180～
Under the conditions of 260 DEG C, prepare fluorescent tube by extrusion in extruder, or prepare ball bubble by injection blow molding machine.
The technical scheme of the application at least has a following beneficial effect:
The LED of the application is added with blue-light absorbers, the rare earth oxide particle diameter in blue-light absorbers 10～
60nm range, owing to surface characteristic and the lattice defect of nanoparticle are distinct, characteristic of correspondence absworption peak also has relatively
Big difference.Along with diminishing of rare earth oxide particle diameter, its characteristic of correspondence absworption peak generation red shift, can be to 420～450nm
Blue light has preferably absorption, and absorbance is up to about 80%；Along with the increase of rare earth oxide particle diameter, its characteristic absorption peak occurs
Blue shift, until ultraviolet spectral region, can realize the absorption of the ultraviolet light more than 95% to 320～380nm.
The LED surface of the application is also coated with environmental purification function layer, containing doping in described environmental purification function layer
Rare earth element and the photocatalyst of titanium dioxide of boron element.Ordinary titanium dioxide photocatalyst is only in the ultraviolet of below 388nm wavelength
Competence exertion effect under light, the doping type photocatalyst of titanium dioxide of the application, in addition to have preferably response to ultraviolet light, to 460
～the visible ray of the broad range of 510nm also has extraordinary response, may be implemented in normal light and irradiate lower PARA FORMALDEHYDE PRILLS(91,95), benzene series
Thing, chloride, effective decomposition of nitrogen oxides, the most also have preferable antibiotic and sterilizing effect.
The LED of the application not only reduces the blue light harm to human eye, and just can reach ring while using
The effect that border purifies, decreases the toxic gas harm to human body.
Accompanying drawing explanation
Fig. 1 is the uv-visible absorption spectra figure of embodiment 1.
Below in conjunction with specific embodiment, the application is expanded on further.Should be understood that these embodiments are merely to illustrate the application
Rather than restriction scope of the present application.
Detailed description of the invention
The application proposes a kind of LED, including LED illuminator and cover at the lampshade outside described LED chip, in lampshade
Containing blue-light absorbers, containing the rare earth oxide that particle size range is 5～60nm in blue-light absorbers；The surface configuration of lampshade has
Environmental purification function layer, containing doped with rare-earth elements and the photocatalyst of titanium dioxide of boron element in environmental purification function layer.This Shen
LED please cannot be only used for absorbing harm, the ultraviolet light of wave-length coverage 320～460nm and blue light to human eye, and has
There is environmental purification function, it is achieved PARA FORMALDEHYDE PRILLS(91,95), benzene homologues, chloride, effective decomposition of nitrogen oxides, the most also have the most anti-
Bacterium bactericidal action.
As a kind of improvement of the application LED, lampshade can be ball bubble or fluorescent tube；Prepare the raw material of lampshade can be glass or
Person's resin, for the ease of the doping of blue-light absorbers, preferably resin.
As a kind of improvement of the application LED, resin is selected from polycarbonate resin (PC) or polymethyl methacrylate
(PMMA) at least one in.
As a kind of improvement of the application LED, blue-light absorbers can coat cover surface, it is possible to is distributed in above-mentioned tree
In fat, in order to improve the optical absorption of blue-light absorbers, avoiding it to come off, blue-light absorbers is preferably distributed by the application simultaneously
In resin.Wherein, rare earth oxide is selected from cerium oxide, lanthana, praseodymium oxide, preferential oxidation cerium；In photocatalyst of titanium dioxide
At least one in lanthanum, cerium, praseodymium or neodymium of the rare earth element of doping, and preferably cerium.
As a kind of improvement of the application LED, in rare earth oxide, the proportion of composing of particle size range is: particle diameter be 5～
Rare earth oxide 25～50 weight portion of 15nm；Particle diameter is rare earth oxide 10～25 weight portion of 15～30nm；Particle diameter is 30
～rare earth oxide 20～25 weight portion of 50nm；Particle diameter is rare earth oxide 20～25 weight portion of 50～60nm.For grain
The nanometer rare earth oxide particle that footpath is different, owing to surface characteristic and lattice defect are distinct, characteristic of correspondence absworption peak is also
There is bigger difference.The application, by the precise controlling to rare earth oxide particle diameter, makes the rare earth oxide of relatively small particle to 420
～the blue light of 450nm has preferably absorption；The rare earth oxide making greater particle size realizes the absorption to 320～380nm ultraviolet lights.
Thus extend the width of the application compositions absorption spectrum.
As a kind of improvement of the application LED, environmental purification function layer contains: anatase titanium dioxide powder body 90～
98 weight portions, preferably 95～97 weight portions；Rare earth oxide powder body 0.5～3 weight portion, preferably 1～1.5 weight portions；Boron
Triethylenetetraminehexaacetic acid ester 0.5～1.5 weight portion, preferably 1～1.5 weight portions.
As a kind of improvement of the application LED, D95≤5 μm of anatase titanium dioxide powder body, rare earth oxide
D95≤5 μm of powder body.The minima of above-mentioned diameter of particle does not limits, illustrative, and the minima of diameter of particle can be 0.01 μm.
For the ease of raw material nanorize more complete, quick during following process, the particle diameter of the application preferred feedstock is less than
In 5 μm.
As a kind of improvement of the application LED, sharp titanium phase content >=90% of anatase titanium dioxide powder body.
As a kind of improvement of the application LED, also can adulterate in photocatalyst of titanium dioxide carbon again；Pass through carbon
Doping, can further improve the photocatalysis efficiency of photocatalyst of titanium dioxide and change as the one of the application photocatalyst of titanium dioxide
Enter, when carrying out carbon doping, raw material during preparation adds graphene oxide.Graphene electron conductivity is high, TiO2With graphite
The transfer of light induced electron will occur after alkene is compound on the interface of bi-material, thus inhibit TiO2Interior electron-hole
Compound, improve TiO2Photocatalysis efficiency.Graphene (Graphene) is the only one layer of atomic thickness being made up of carbon atom
Two dimensional crystal, graphene oxide (graphene oxide) is the oxide of Graphene, after oxidized, oxygen-containing functional group on it
Increasing and make character relatively Graphene more active, graphene oxide is owing to its specific area is big, surface can be big, and it is for polar compounds
Thing has stronger adsorption, thus can be enriched in around photocatalyst of titanium dioxide by harmful substance, increases reactant
Concentration, and it can be avoided that the intermediate product in catalytic reaction process is free or volatilization, thus catalytic reaction fast has been effectively ensured
Speed is carried out.
As a kind of improvement of the application LED, possibly together with graphene oxide 0.6～0.9 weight in environmental purification function layer
Amount part, preferably 0.75～0.9 weight portion.
As a kind of improvement of the application LED, in lampshade the percent mass percentage ratio of blue-light absorbers be 0.3～
2.5%, the thickness of environmental purification function layer is 5～40 μm.
The application further relates to the preparation method of this LED, at least comprises the following steps:
(1) in proportion rare earth oxide is joined in organic solvent I, be subsequently adding coupling agent, after being dispersed through, obtain institute
State blue-light absorbers；The mass percent concentration of blue-light absorbers middle rare earth is 30%～50%, and organic solvent I is selected from
Dimethylbenzene and the mixed solvent of Ketohexamethylene；
(2) anatase titanium dioxide powder body, rare earth oxide powder body and triethyl borate are mixed in proportion laggard
Row grinds, and grinds 6～15 hours, obtain the nano-powder that particle diameter is below 10nm under conditions of 60～100 DEG C；To be prepared into
To nano-powder be scattered in organic solvent II formation colloidal sol, organic solvent II is selected from ethyl acrylate and the mixing of Ketohexamethylene
Solvent, nano-powder mass percentage content in colloidal sol is 30～40%；I.e. prepare the painting containing photocatalyst of titanium dioxide
Material；
(3) blue-light absorbers that step (1) prepares is joined in resin, be uniformly mixing to obtain mixed material, will
Described mixed material is heated to 50～70 DEG C of dischargings, and is prepared as described lampshade；
(4) coating prepared in cover surface application step (2), under the uviol lamp of 100～150W solidify 10～
25 minutes；
(5) the described lampshade after solidification is assembled in described LED illuminator, obtains described LED.
As a kind of improvement of the application preparation method, in step (1), the volume ratio of dimethylbenzene and Ketohexamethylene is 4:1
～5:1.
In step (1), the application, can be on nanometer rare earth oxide particle and the boundary of organic solvent by adding coupling agent
Erect " molecular bridge " between face, the material of two kinds of character great disparities is linked together, improves rare earth oxide in organic solvent
Dispersibility.As a kind of improvement of the application preparation method, coupling agent is selected from silane coupler or titanate coupling agent.Silane
Coupling agent be selected from KH550, KH560, KH570, KH792, DL602, DL171, titanate coupling agent selected from NDZ101, NDZ105,
NDZ201、NDZ311.The addition of coupling agent is the 3～5% of rare earth oxide weight.
As a kind of improvement of the application preparation method, in step (1) and step (3), it is separated into ultrasonic vibration dispersion,
Temperature is 30～40 DEG C, and the time is 30～60min.Ultrasonic disperse can be carried out in common supersonic generator, and frequency is led to
Often 20～40KHz.
As a kind of improvement of the application preparation method, in step (2), it is ground to use high energy ball mill to grind
Mill, the application is ground at a temperature of 60～100 DEG C for a long time by employing high energy ball mill, thus by raw mill extremely
The nano-powder of below 10nm.The higher grinding temperature that the application has selected, its purpose is to improve the efficiency ground.
As a kind of improvement of the application preparation method, in step (2), first graphene oxide is configured to graphite oxide
Alkene solution, is then added drop-wise to graphene oxide solution in nano-powder；Preferably, described graphene oxide solution aoxidizes stone
The mass percentage content of ink alkene is 25～35%, preferably 30%.
As a kind of improvement of the application preparation method, in step (2), the volume ratio of ethyl acrylate and Ketohexamethylene is
6～8:2～4.
As a kind of improvement of the application preparation method, in step (3), under the conditions of 180～260 DEG C, blue light is inhaled
Receive agent solution to be added drop-wise at twice in resin, stir 5～10 minutes, mixing speed preferably 60～2500r/min.
It is further preferred that first stirring at low speed 2～5 minutes, then high-speed stirred 3～5 minutes；The speed of stirring at low speed is
100～600r/min, the speed of high-speed stirred is 600～1800r/min.
As a kind of improvement of the application preparation method, in step (3), after mixed material discharging, 180～260
Under the conditions of DEG C, prepare fluorescent tube by extrusion in extruder, or prepare ball bubble by injection blow molding machine.
Below by detailed description of the invention, the technical scheme of the application is made further explanation, it should be appreciated that with
Lower composition and content are merely exemplary, are not construed as limiting scope of the present application.
Embodiment 1
A kind of LED, including LED illuminator and cover at the fluorescent tube outside LED chip, containing blue light absorption in its lampshade
Agent, containing the rare earth oxide that particle size range is 5～60nm in blue-light absorbers；The surface configuration of lampshade has environmental purification function
Layer, containing doped with rare-earth elements and the photocatalyst of titanium dioxide of boron element in environmental purification function layer.
Wherein:
(1) preparation method of blue-light absorbers is:
In the mixed solvent (volume ratio 4:1) of dimethylbenzene and Ketohexamethylene, add coupling agent, be subsequently adding rare earth oxide,
And relax, hybrid mode uses shakes 40min with supersonic generator at 40 DEG C, by mixed system until forming reddish yellow
The homogeneous fluid composition that color is transparent, obtains blue-light absorbers；Wherein, the mass percent of blue-light absorbers middle rare earth
Concentration is 50%, and the addition of coupling agent is the 5% of rare earth oxide weight.Silane coupler and titanate esters in embodiment are even
Connection agent is Nanjing Chuan Shi auxiliary chemicals company limited and produces.Wherein, kind and the particle diameter of rare earth oxide is distributed such as table 1 institute
Show.
(2) preparation method of photocatalyst of titanium dioxide is:
Mix after anatase titanium dioxide powder body, rare earth oxide powder body and triethyl borate are weighed in proportion
Close；Wherein, sharp titanium phase content >=90% of anatase titanium dioxide powder body；Anatase titanium dioxide selects D95 to be about 5 μm
Powder body, rare earth oxide selects D95 to be the powder body about 5 μm；High energy ball mill is used to grind 12 under conditions of 60 DEG C
Hour, obtain the nano-powder that particle diameter is below 10nm；The nano-powder prepared is scattered in ultrasonic disperser
In the mixed solvent of acrylic acid ethanol/Ketohexamethylene (volume ratio is 70:30), the frequency of ultrasonic disperse is 30KHz；I.e. prepare dioxy
Changing titanium photo-catalytic coating, nano-powder mass percentage content in coating is 40%.Wherein, photocatalyst of titanium dioxide coating
Composition as shown in table 2.
(3) preparation method of LED is:
1, the blue-light absorbers prepared is joined in PC resin, the percent mass hundred of blue-light absorbers in PC resin
Proportion by subtraction is 2%；It is uniformly mixing to obtain mixed material, mixed material is heated to 60 DEG C of dischargings, under the conditions of 240 DEG C, by squeezing
Go out extrusion in machine and prepare fluorescent tube；
2, at the surface coating photocatalyst of titanium dioxide coating that fluorescent tube or ball steep, spend for thick 10 μm, at the uviol lamp of 150W
Lower solidification 20 minutes；
3, the fluorescent tube after solidification is assembled in the LED illuminator of 5W, obtains LED.
Comparative example D1 is also without photocatalyst of titanium dioxide coating without blue-light absorbers.
Table 1: the formula (unit: weight portion) of blue-light absorbers
Table 2: the formula (unit: weight portion) of photocatalyst of titanium dioxide
By the absorption characteristic of ultraviolet-visible spectrometer test resulting composition, result is as shown in table 3.In visible light wave
In long scope (460～510nm), the method in QB/T2761-2006 is used to detect above-mentioned film PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia and TVOC
Degradation rate, result is as shown in table 4～7:
Table 3: visible-uv absorption rate
| Numbering | 420～450nm absorbances | 320～380nm absorbances |
| 1-1 | 80% | 95% |
| 1-2 | 82% | 96% |
| 1-3 | 79% | 92% |
| D1 | 0% | 0% |
Table 4: Degradation Formaldehyde rate
Table 5: benzene degradation rate
| 12 hours degradation rates of benzene | 24 hours degradation rates of benzene | 36 hours degradation rates of benzene | |
| 1-1 | 77.2% | 95.6% | 96.4% |
| 1-2 | 77.6% | 94.5% | 95.2% |
| 1-3 | 78.3% | 95.6% | 96.7% |
| D1 | 0% | 0% | 0% |
Table 6: ammonia degradation rate
| 12 hours degradation rates of ammonia | 24 hours degradation rates of ammonia | 36 hours degradation rates of ammonia | |
| 1-1 | 65.3% | 87.5% | 90.1% |
| 1-2 | 66.2% | 86.4% | 91.4% |
| 1-3 | 67.3% | 88.1% | 90.9% |
| D1 | 0% | 0% | 0% |
Table 7:TVOC degradation rate
| TVOC12 hour degradation rate | TVOC24 hour degradation rate | TVOC36 hour degradation rate | |
| 1-1 | 74.1% | 92.2% | 95.3% |
| 1-2 | 73.7% | 91.3% | 94.6% |
| 1-3 | 73.8% | 91.7% | 94.2% |
| D1 | 0% | 0% | 0% |
Fig. 1 is the uv-visible absorption spectra figure of embodiment 1.As seen from Figure 1, this fluorescent tube light to 420～450nm
Absorbance is about 80%, to the uv absorption rate of wavelength 320～380nm up to more than 95%.Find through long term test,
Photocatalyst of titanium dioxide film in the LED of the application, under conditions of without damage, is placed more than 3 years, and it is to above-mentioned substance
Degradation property keep constant.
Embodiment 2
A kind of LED, including LED illuminator and cover at the ball bubble outside LED chip, containing blue light absorption in its lampshade
Agent, containing the rare earth oxide that particle size range is 5～60nm in blue-light absorbers；The surface configuration of lampshade has environmental purification function
Layer, containing doped with rare-earth elements and the photocatalyst of titanium dioxide of boron element in environmental purification function layer.
Wherein: the formula agent preparation method of blue-light absorbers is:
In the mixed solvent (volume ratio 4:1) of dimethylbenzene and Ketohexamethylene, add coupling agent, be subsequently adding rare earth oxide,
And relax, hybrid mode uses shakes 40min with supersonic generator at 35 DEG C, by mixed system until forming reddish yellow
The homogeneous fluid composition that color is transparent, obtains blue-light absorbers；Wherein, the mass percent of blue-light absorbers middle rare earth
Concentration is 30%, and the addition of coupling agent is the 3% of rare earth oxide weight.Silane coupler and titanate esters in embodiment are even
Connection agent is Nanjing Chuan Shi auxiliary chemicals company limited and produces.Wherein, kind and the particle diameter of rare earth oxide is distributed such as table 8 institute
Show.
The preparation method of photocatalyst of titanium dioxide is:
Mix after anatase titanium dioxide powder body, rare earth oxide powder body and triethyl borate ratio are weighed
Close；Wherein, sharp titanium phase content >=90% of anatase titanium dioxide powder body；Anatase titanium dioxide selects D95 to be about 5 μm
Powder body, rare earth oxide selects D95 to be the powder body about 5 μm；High energy ball mill is used to grind 10 under conditions of 90 DEG C
Hour, obtain the nano-powder that particle diameter is below 10nm；Weigh graphene oxide in proportion, be prepared as graphene oxide solution,
Then graphene oxide solution is added drop-wise in nano-powder；The mass percentage content of graphene oxide is 30%；
The nano-powder prepared is scattered in ultrasonic disperser acrylic acid ethanol/Ketohexamethylene, and (volume ratio is
In mixed solvent 70:30), the frequency of ultrasonic disperse is 30KHz；I.e. preparing photocatalyst of titanium dioxide coating, nano-powder exists
Mass percentage content in coating is 30%.Wherein, the composition of photocatalyst of titanium dioxide coating is as shown in table 9.
The preparation method of LED is:
1, the blue-light absorbers prepared is joined in PMMA resin, the quality hundred of blue-light absorbers in PMMA resin
Dividing percentage ratio is 2%；It is uniformly mixing to obtain mixed material, mixed material is heated to 60 DEG C of dischargings, under the conditions of 240 DEG C, or
Prepare ball by injection blow molding machine to steep；
2, at the surface coating photocatalyst of titanium dioxide coating that fluorescent tube or ball steep, thickness is 8 μm, under the uviol lamp of 130W
Solidify 25 minutes；
3, the ball bubble after solidification is assembled in the LED illuminator of 5W, obtains LED.
Table 8: the formula (unit: weight portion) of blue-light absorbers
Table 9: the formula (unit: weight portion) of photocatalyst of titanium dioxide
By the absorption characteristic of ultraviolet-visible spectrometer test resulting composition, result is as shown in table 10.In visible light wave
In long scope (460～510nm), the method in QB/T2761-2006 is used to detect above-mentioned film PARA FORMALDEHYDE PRILLS(91,95), benzene, ammonia and TVOC
Degradation rate, result is as shown in table 11～14:
Table 10: visible-uv absorption rate
| Numbering | 420～450nm absorbances | 320～380nm absorbances |
| 2-1 | 78% | 92% |
| 2-2 | 75% | 89% |
| 2-3 | 72% | 85% |
Table 11: Degradation Formaldehyde rate
| Numbering | 12 hours degradation rates of formaldehyde | 24 hours degradation rates of formaldehyde | 36 hours degradation rates of formaldehyde |
| 2-1 | 72.1% | 92.3% | 95.6% |
| 2-2 | 73.2% | 93.2% | 94.8% |
| 2-3 | 74.5% | 94.4% | 95.9% |
Table 12: benzene degradation rate
| Numbering | 12 hours degradation rates of benzene | 24 hours degradation rates of benzene | 36 hours degradation rates of benzene |
| 2-1 | 78.4% | 96.1% | 97.7% |
| 2-2 | 78.8% | 95.2% | 96.5% |
| 2-3 | 79.2% | 96.7% | 97.9% |
Table 13: ammonia degradation rate
| Numbering | 12 hours degradation rates of ammonia | 24 hours degradation rates of ammonia | 36 hours degradation rates of ammonia |
| 2-1 | 67.3% | 89.2% | 92.5% |
| 2-2 | 68.4% | 88.9% | 93.2% |
| 2-3 | 69.1% | 89.5% | 92.9% |
Table 14:TVOC degradation rate
| Numbering | TVOC12 hour degradation rate | TVOC24 hour degradation rate | TVOC36 hour degradation rate |
| 2‐1 | 75.5% | 94.2% | 97.8% |
| 2-2 | 74.6% | 95.6% | 98.3% |
| 2-3 | 75.7% | 94.4% | 97.9% |
Comparative example 1
In the blue-light absorbers of comparative example 1-1 and 1-2, the solvent of use, coupling agent, rare earth oxide are in solvent and idol
Join the content in agent, ultrasonic time with embodiment 1.Wherein, the rare earth oxide particle diameter of use is more than 60nm, rare earth oxide
Kind and particle diameter distribution are as shown in Table 15.
Table 15: the formula (unit: weight portion) of blue-light absorbers
In the blue-light absorbers of comparative example 1-3～1-10, the solvent of use, coupling agent, rare earth oxide are in solvent and idol
Join the content in agent, ultrasonic time with embodiment 1.The kind of rare earth oxide and particle diameter distribution are as shown in table 16.Comparative example 1-
11 and 1-12 be respectively Jiangxi Luo Te Chemical Co., Ltd. produce blue light absorption powder and UV absorbent UV 320, by its with
The solid content of 30% is scattered in dimethylbenzene.
Table 16: the formula (unit: weight portion) of blue-light absorbers
According to the photocatalyst of titanium dioxide coating of 1-1 in embodiment 1, and continue to prepare LED according to the method for embodiment 1
Lamp, by ultraviolet-visible spectrometer test gained comparative example 1-1～the absorption characteristic of 1-12, result is as shown in table 17:
Table 17: visible-uv absorption rate
Comparative example 1-1 and 1-2 explanation, when rare earth oxide particle diameter reduces more than 60nm, blue light absorption rate, and along with rare earth
The increase of oxide diameter sizes, rate of absorbing UV rises inconspicuous.Embodiment 1～6 is compareed with comparative example 1-3～1-10, explanation
If the particle diameter of rare earth oxide not value in four intervals, it will cause the decline of absorbance in a certain scope.Contrast
Example 1-11 and 1-12 explanation, commercially available blue light absorption powder and UV absorbent only have preferably suction to single blue light or ultraviolet light
Receive, but blue light and ultraviolet light cannot be absorbed simultaneously.
Comparative example 2
It is first according to the formula of 1-1 in embodiment 1 and prepares blue-light absorbers, then prepare two by the method in embodiment 1
Titanium dioxide photocatalyst coating, difference is, the composition of photocatalyst of titanium dioxide coating is as shown in table 18.
Table 18: photocatalyst of titanium dioxide formulation for coating material (unit: weight portion)
And continue to prepare LED according to the method for embodiment 1, use the method detection LED pair in QB/T2761-2006
The degradation rate of formaldehyde, benzene, ammonia and TVOC；Testing result is as shown in table 19～22:
Table 19: Degradation Formaldehyde rate
| Numbering | 12 hours degradation rates of formaldehyde | 24 hours degradation rates of formaldehyde | 36 hours degradation rates of formaldehyde |
| Comparative example 2-1 | 0% | 0% | 0% |
| Comparative example 2-2 | 34.6% | 43.8% | 50.2% |
| Comparative example 2-3 | 47.8% | 60.7% | 67.3% |
| Comparative example 2-4 | 22.7% | 26.7% | 25.2% |
| Comparative example 2-5 | 54.3% | 64.5% | 71.4% |
| Comparative example 2-6 | 45.7% | 53.5% | 58.1% |
Table 20: benzene degradation rate
| Numbering | 12 hours degradation rates of benzene | 24 hours degradation rates of benzene | 36 hours degradation rates of benzene |
| Comparative example 2-1 | 0% | 0% | 0% |
| Comparative example 2-2 | 28.4% | 34.2% | 38.8% |
| Comparative example 2-3 | 50.2% | 56.4% | 62.9% |
| Comparative example 2-4 | 21.0% | 27.5% | 30.1% |
| Comparative example 2-5 | 57.5% | 63.4% | 73.6% |
| Comparative example 2-6 | 52.7% | 58.8% | 61.1% |
Table 21: ammonia degradation rate
| Numbering | 12 hours degradation rates of ammonia | 24 hours degradation rates of ammonia | 36 hours degradation rates of ammonia |
| Comparative example 2-1 | 0% | 0% | 0% |
| Comparative example 2-2 | 15.5% | 17.4% | 19.3% |
| Comparative example 2-3 | 42.3% | 51.5% | 56.2% |
| Comparative example 2-4 | 13.5% | 22.6% | 27.1% |
| Comparative example 2-5 | 44.2% | 49.1% | 52.5% |
| Comparative example 2-6 | 42.3% | 47.5% | 54.2% |
Table 22:TVOC degradation rate
Although the application is open as above with preferred embodiment, but is not for limiting claim, any this area skill
Art personnel, on the premise of conceiving without departing from the application, can make some possible variations and amendment, therefore the application
Protection domain should be defined in the range of standard with the application claim.
Claims (10)
1. a LED, described LED includes LED illuminator and covers at the lampshade outside described LED chip, and its feature exists
In, containing blue-light absorbers in the raw material of described lampshade, containing the rare earth that particle size range is 5～60nm in described blue-light absorbers
Oxide；The surface configuration of described lampshade has environmental purification function layer, containing rare earth doped unit in described environmental purification function layer
Element and the photocatalyst of titanium dioxide of boron element.
LED the most according to claim 1, it is characterised in that described lampshade is ball bubble or fluorescent tube；Prepare described lampshade
Raw material is resin, it is preferred that described resin is selected from polycarbonate resin or polymethyl methacrylate.
LED the most according to claim 1, it is characterised in that described blue-light absorbers is distributed in prepares described lampshade
In raw material, described rare earth oxide is selected from cerium oxide, lanthana, praseodymium oxide, preferential oxidation cerium；Described rare earth element selected from lanthanum,
At least one in cerium, praseodymium or neodymium, preferably cerium.
LED the most according to claim 1, it is characterised in that the proportion of composing of described rare earth oxide particle size range is:
LED the most according to claim 1, it is characterised in that contain in described environmental purification function layer:
Anatase titanium dioxide powder body 90～98 weight portion, preferably 95～97 weight portions；
Rare earth oxide powder body 0.5～3 weight portion, preferably 1～1.5 weight portions；
Triethyl borate 0.5～1.5 weight portion, preferably 1～1.5 weight portions.
LED the most according to claim 1, it is characterised in that described doped with rare-earth elements and the titanium dioxide of boron element
Also doped with carbon in photocatalyst；Preferably, possibly together with graphene oxide 0.6～0.9 weight in described environmental purification function layer
Amount part, preferably 0.75～0.9 weight portion.
LED the most according to claim 1, it is characterised in that the quality hundred of blue-light absorbers in the raw material of described lampshade
Proportion by subtraction is 0.3～2.5%, and the thickness of described environmental purification function layer is 5～30 μm.
8. the preparation method of the LED as described in claim 1～7 any claim, it is characterised in that at least include
Following steps:
(1) in proportion rare earth oxide is joined in organic solvent I, be subsequently adding coupling agent, after being dispersed through, obtain described indigo plant
Light absorber；The mass percent concentration of rare earth oxide described in described blue-light absorbers is 30%～50%；Described organic
Solvent I is selected from dimethylbenzene and the mixed solvent of Ketohexamethylene, it is preferred that the volume ratio of described dimethylbenzene and Ketohexamethylene is 4:1～5:
1；
(2) grind after anatase titanium dioxide powder body, rare earth oxide powder body and triethyl borate being mixed in proportion
Mill, grinds 6～15 hours under conditions of 60～100 DEG C, obtains the nano-powder that particle diameter is below 10nm；By prepare
Nano-powder is scattered in organic solvent II formation colloidal sol, i.e. prepares the coating containing described photocatalyst of titanium dioxide；Described have
Machine solvent II is selected from ethyl acrylate and the mixed solvent of Ketohexamethylene, described nano-powder mass percent in described colloidal sol
Content is 30～40%；Preferably, the volume ratio of ethyl acrylate and Ketohexamethylene is 6～8:2～4；
(3) blue-light absorbers that step (1) prepares is joined in resin, be uniformly mixing to obtain mixed material, by described
Mixed material is heated to 50～70 DEG C of dischargings, and is prepared as described lampshade；
(4) coating containing described photocatalyst of titanium dioxide prepared described cover surface application step (2), 100
～solidify 10～25 minutes under the uviol lamp of 150W；
(5) the described lampshade after solidification is assembled in described LED illuminator, obtains described LED.
Preparation method the most according to claim 8, it is characterised in that in step (3), under the conditions of 180～260 DEG C,
Described blue light absorption agent solution is divided 2～3 times and is added drop-wise in described resin, then stirring 5～10 minutes.
Preparation method the most according to claim 8, it is characterised in that in step (3), described lampshade is ball bubble or lamp
Pipe, after described mixed material discharging, under the conditions of 180～260 DEG C, prepares fluorescent tube by extrusion in extruder, or logical
Cross injection blow molding machine and prepare ball bubble.
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| CN112029335A (en) * | 2020-09-16 | 2020-12-04 | 贵溪市清亮照明科技有限公司 | Blue-light-removing coating for LED |
| CN112029380A (en) * | 2020-09-08 | 2020-12-04 | 贵溪市清亮照明科技有限公司 | Blue light removing coating |
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