CN102731965B - Quantum dot fluorescent material, its preparation method and LED fill/flash lamp - Google Patents
Quantum dot fluorescent material, its preparation method and LED fill/flash lamp Download PDFInfo
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- CN102731965B CN102731965B CN201210209749.8A CN201210209749A CN102731965B CN 102731965 B CN102731965 B CN 102731965B CN 201210209749 A CN201210209749 A CN 201210209749A CN 102731965 B CN102731965 B CN 102731965B
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Abstract
The invention discloses a quantum dot fluorescent material, which is prepared from the following raw materials of: by weight, 0.01-35 parts of a fluorescent material, 60-90 parts of a resin, and 2-35 parts of a filling material, wherein the fluorescent material comprises quantum dots or a compound of quantum dot and non-quantum dot fluorescent materials. Correspondingly, the invention discloses a preparation method of the above quantum dot fluorescent material. In addition, the invention also discloses a LED fill/flash lamp, which is prepared by steps of: coating the quantum dot fluorescent material on the surface of an unpacked LED chip, curing and packaging. According to the invention, the quantum dot fluorescent material and the LED fill/flash lamp prepared by the utilization of the quantum dot fluorescent material have characteristics of high color rendering index, low color temperature and strong luminous efficiency. By the adoption of the material and the lamp, color trueness of images acquired by image acquisition equipment can be substantially raised.
Description
Technical field
The present invention relates to benefit/flash light techniques field, particularly relate to a kind of quantum dot fluorescence material and preparation method thereof, and a kind of LED benefit/photoflash lamp.
Background technology
Along with the raising day by day of standard of living, the requirement of people to picture quality is also more and more higher, and environment light source often can not meet the requirement that image capture device gathers high quality graphic, and therefore, the application on image capture device of light compensating lamp or photoflash lamp is necessary.
LED benefit/photoflash lamp has specular removal, high energy-conservation, low voltage drive, safe to use, the life-span long, the feature of fast response time, especially more and more substitutes traditional benefit/photoflash lamp portable electronic products (as mobile phone, photographic camera) is upper.But the use on high-end image collecting device is also less.One of them chief reason is that conventional white light LED benefit/photoflash lamp adopts the fluorescent RE powder covering Yellow light-emitting low temperature or orange red light on the LED chip of blue light.The cold light of this blue light and gold-tinted combines and has lacked ruddiness, other objects such as such as human body skin are developed the color distortion under this group cold light, although by using other fluorescent RE powders can make up this disappearance a little, the image color quality of its imaging is still poor.In addition, the LED benefit/photoflash lamp adopting traditional rare earth fluorescent material to prepare, due to the natural characteristics of fluorescent RE powder " narrow-band absorption, narrowband excitation ", makes it limited to the utilization ratio of visible light energy, and luminous efficiency is not enough.And rare earth resources is very rare, unsuitable overexploitation utilizes.
In view of this, provide a kind of and can overcome the defect existed in prior art, improve the image color quality of imaging, and to improve luminous efficiency, reduce the LED benefit/photoflash lamp used rare earth material be problem demanding prompt solution in the industry.
Summary of the invention
The object of the invention is to, a kind of quantum dot fluorescence material and preparation method thereof is provided, it uses quantum dot as fluorescent material, comparatively conventional fluorescent powder is high for luminous efficiency, decrease the undue dependence to fluorescent RE powder simultaneously, alleviate the overexploitation to rare earth resources, be conducive to the destruction of reducing mining area ecological environment.
Simultaneously, another object of the present invention is to, a kind of LED benefit/photoflash lamp utilizing quantum dot fluorescent material to prepare is provided, it has that colour rendering index is high, colour temperature is low and the advantage such as light efficiency is strong, significantly improve image capture device gather the real colour degree of image, can be widely used on the equipment such as cell phone cameras photoflash lamp, camera flashlamp and pick up camera light compensating lamp, and reduce the use even avoided rare earth material.
In order to realize foregoing invention object, embodiments provide a kind of quantum dot fluorescence material, it is as follows in the main raw material formula of mass parts:
Fluorescent material 0.01 ~ 35;
Resin 60 ~ 90;
Filler 2 ~ 35;
Described fluorescent material forms by quantum dot or by the mixture of quantum dot and non-quantum point fluorescent material.
As the improvement of such scheme, when described fluorescent material is made up of the mixture of quantum dot and non-quantum point fluorescent material, the mass fraction of described quantum dot is 0.01 ~ 10 part, and the mass fraction of described non-quantum point fluorescent material is 0.01 ~ 27 part.
As the improvement of such scheme, described quantum dot is by carbon, silicon, germanium, tin, plumbous, cadmium, zinc, sulphur, selenium, tellurium, boron, aluminium, gallium, indium, nitrogen, phosphorus, arsenic, one or more the elementary composition nano semiconductor materials in antimony, the size of described at least one dimension of nano semiconductor material is within the scope of 1 ~ 100nm;
Described non-quantum point fluorescent material comprises fluorescent RE powder, organic fluorescent powder.
As the improvement of such scheme, described resin comprise in epoxy resin, organic silica gel class, esters of acrylic acid, polyurethanes, ethylene-vinyl acetate resin and polycarbonate resin one or more.
As the improvement of such scheme, described filler comprise in silicon-dioxide, calcium carbonate one or more.
The invention also discloses a kind of method preparing quantum dot fluorescent material, described quantum dot fluorescence material is prepared by following methods and obtains:
By quantum dot and the mixing of non-quantum point fluorescent material, maybe by there is the quantum dot of different emission by mechanical stirring or sonic oscillation mixing, obtain fluorescent material;
Described fluorescent material and resin, filler are mixed by mechanical stirring or sonic oscillation, obtains mixture;
By described mixture 20 ~ 30 DEG C, vacuumize 5 ~ 180min under 0.01 ~ 0.3MPa condition, obtain quantum dot fluorescence material;
Wherein, described quantum dot fluorescence material is as follows in the main raw material formula of mass parts:
Described fluorescent material 0.01 ~ 35;
Described resin 60 ~ 90;
Described filler 2 ~ 35;
Described fluorescent material forms by described quantum dot or by the mixture of described quantum dot and described non-quantum point fluorescent material.
The invention also discloses a kind of LED benefit/photoflash lamp, described LED benefit/photoflash lamp is the LED chip surface by quantum dot fluorescence coated materials not encapsulated, and makes through cure package;
Wherein, described quantum dot fluorescence material is as follows in the main raw material formula of mass parts:
Fluorescent material 0.01 ~ 35;
Resin 60 ~ 90;
Filler 2 ~ 35;
Described fluorescent material forms by quantum dot or by the mixture of quantum dot and non-quantum point fluorescent material.
As the improvement of such scheme, the mode of described LED benefit/photoflash lamp cure package comprises photocuring and thermofixation.
As the improvement of such scheme, described photocuring power is 50w ~ 15kw, and the time is 0.1s ~ 90s.
As the improvement of such scheme, described heat curing temperature is 60 DEG C ~ 180 DEG C, and the time is 10min ~ 80min.
Implement the embodiment of the present invention, there is following beneficial effect:
One, a kind of LED benefit/photoflash lamp utilizing quantum dot fluorescent material to prepare provided by the invention, the fluorescent substance of described LED benefit/photoflash lamp is with quantum dot fluorescence material for main raw material, and described quantum dot fluorescence materials'use quantum dot is as fluorescent material.Because quantum dot belongs to semiconductor nano material, its particle size is at 1 ~ 100nm, and therefore, it is compared with conventional fluorescent material, and quantum dot adjusts the light of different emission by changing single-material size of particles; Secondly, because quantum dot has the characteristic of " wide band absorption, narrowband excitation ", quantum dot uv-visible absorption spectrum is wider, and therefore, the exciting light of single wavelength can excite the quantum dot with different emission; And luminous efficiency comparatively conventional fluorescent powder is high, its white light colour developing parameter be 90, far above the colour developing parameter 75 of existing white light LEDs.In addition, quantum dot has good light stability and makes it can be good at being applied to imaging of tissue.
Therefore, the described quantum dot fluorescent material that utilizes replaces traditional rare earth fluorescent material, preparation and the LED benefit/photoflash lamp that obtains have that colour rendering index is high, colour temperature is low and the advantage such as light efficiency is strong, can significantly improve image capture device gather the real colour degree of image, the image color quality of effective raising imaging, develop the color true to nature, can be widely used on the equipment such as cell phone cameras photoflash lamp, camera flashlamp and pick up camera light compensating lamp.In addition, the present invention substitutes fluorescent RE powder even completely with quantum dot fluorescence material component, therefore reduces the use even avoided rare earth material.
Two, a kind of quantum dot fluorescence material that can be applicable to LED benefit/photoflash lamp provided by the invention and preparation method thereof, described fluorescent material uses quantum dot to replace traditional rare earth fluorescent material as fluorescent material, comparatively conventional fluorescent powder is high for luminous efficiency, have that colour rendering index is high, colour temperature is low and the feature such as light efficiency is strong, can significantly improve image capture device gather the real colour degree of image, decrease the undue dependence to fluorescent RE powder simultaneously, alleviate the overexploitation to rare earth resources, be conducive to the destruction of reducing mining area ecological environment.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below the present invention is described in further detail.
Embodiments provide a kind of quantum dot fluorescence material, it is as follows in the main raw material formula of mass parts:
Fluorescent material 0.01 ~ 35;
Resin 60 ~ 90;
Filler 2 ~ 35;
Preferably, described quantum dot fluorescence material is as follows in the main raw material formula of mass parts:
Fluorescent material 0.01 ~ 30;
Resin 65 ~ 85;
Filler 4 ~ 30.
Described fluorescent material forms by quantum dot or by the mixture of quantum dot and non-quantum point fluorescent material.
Wherein, described quantum dot is by carbon, silicon, germanium, tin, plumbous, cadmium, zinc, sulphur, selenium, tellurium, boron, aluminium, gallium, indium, nitrogen, phosphorus, arsenic, one or more the elementary composition nano semiconductor materials in antimony, the size of described at least one dimension of nano semiconductor material is within the scope of 1 ~ 100nm;
Described non-quantum point fluorescent material comprises fluorescent RE powder, organic fluorescent powder.
When fluorescent material only adopts quantum dot, content R:G:B=3 ~ 7:10 ~ 15:6 ~ 11 of quantum dot.
Preferably, when fluorescent material only adopts quantum dot, the content R:G:B=5:13:8 of quantum dot.
It should be noted that, rgb color pattern is a kind of color standard of industry member, and namely RGB is the color representing red, green, blue three passages.Rgb color pattern is by obtaining color miscellaneous to the change of R (Red, red), G (Green, green), B (Blue, blue) three Color Channels and their superpositions each other.This standard almost include human eyesight can all colours of perception, be use one of the widest color system at present.
When described fluorescent material is made up of the mixture of quantum dot and non-quantum point fluorescent material, the mass fraction of described quantum dot is 0.01 ~ 10 part, and the mass fraction of described non-quantum point fluorescent material is 0.01 ~ 27 part.
Preferably, when described fluorescent material is made up of the mixture of quantum dot and non-quantum point fluorescent material, the mass fraction of described quantum dot is 0.01 ~ 5 part, and the mass fraction of described non-quantum point fluorescent material is 0.01 ~ 25 part.
Described resin comprise in epoxy resin, organic silica gel class, esters of acrylic acid, polyurethanes, ethylene-vinyl acetate resin and polycarbonate resin one or more;
Preferably, described resin is the one in epoxy resin, organic silica gel class, esters of acrylic acid, polyurethanes, ethylene-vinyl acetate resin and polycarbonate resin.
Further preferably, described resin is epoxy resin, acrylic resin adhesive, silicone resin or organic silicon resin adhesive.
Described resin be through the process of ultraviolet lamp photocuring or under the temperature condition of 10 DEG C ~ 180 DEG C through thermofixation process, the time of described photocuring or thermofixation is 3s ~ 150min.
Preferably, described resin be through the process of ultraviolet lamp photocuring or under the temperature condition of 20 DEG C ~ 150 DEG C through thermofixation process, the time of described photocuring or thermofixation is 5s ~ 120min.
Described filler comprise silicon-dioxide, calcium carbonate one or more.
Preferably, described filler is silicon-dioxide or calcium carbonate.
Quantum dot fluorescence materials'use quantum dot of the present invention replaces traditional rare earth fluorescent material as fluorescent material, comparatively conventional fluorescent powder is high for quantum dot light emitting efficiency, have that colour rendering index is high, colour temperature is low and the feature such as light efficiency is strong, can significantly improve image capture device gather the real colour degree of image.Decrease the undue dependence to fluorescent RE powder simultaneously, alleviate the overexploitation to rare earth resources, be conducive to the destruction of reducing mining area ecological environment.
The present invention is a kind of, and to can be applicable to the preparation method of the quantum dot fluorescence material of LED benefit/photoflash lamp specific as follows:
When described fluorescent material is made up of quantum dot, the preparation method of described quantum dot fluorescence material comprises:
Step one, by the described quantum dot with different emission by mechanical stirring or sonic oscillation mixing, obtain fluorescent material;
Step 2, by described fluorescent material and resin, filler by mechanical stirring or sonic oscillation mixing, obtain mixture;
Step 3, by described mixture 20 ~ 30 DEG C, vacuumize 5 ~ 180min under 0.01 ~ 0.3MPa condition, obtain quantum dot fluorescence material.
Preferably, by described mixture 25 DEG C, vacuumize 10 ~ 60min under 0.1MPa condition, obtain quantum dot fluorescence material.
When described fluorescent material is made up of the mixture of quantum dot and non-quantum point fluorescent material, the preparation method of described quantum dot fluorescence material comprises:
Step one, by described quantum dot and non-quantum point fluorescent material mixing, obtain fluorescent material;
Step 2, by described fluorescent material and resin, filler by mechanical stirring or sonic oscillation mixing, obtain mixture;
Step 3, by described mixture 20 ~ 30 DEG C, vacuumize 5 ~ 180min under 0.01 ~ 0.3MPa condition, obtain quantum dot fluorescence material.
Preferably, by described mixture 25 DEG C, vacuumize 10 ~ 60min under 0.1MPa condition, obtain quantum dot fluorescence material.
Correspondingly, embodiments provide a kind of LED benefit/photoflash lamp, described LED benefit/photoflash lamp is LED chip surface quantum dot fluorescence coated materials do not encapsulated, and makes through cure package;
Described quantum dot fluorescence material is as follows in the main raw material formula of mass parts:
Fluorescent material 0.01 ~ 35;
Resin 60 ~ 90;
Filler 2 ~ 35.
Preferably, described quantum dot fluorescence material is as follows in the main raw material formula of mass parts:
Fluorescent material 0.01 ~ 30;
Resin 65 ~ 85;
Filler 4 ~ 30.
Described fluorescent material forms by quantum dot or by the mixture of quantum dot and non-quantum point fluorescent material.
It should be noted that, coating method of the present invention mainly adopts the mode of a glue or spraying, but is not limited thereto.
Wherein, described quantum dot is by carbon, silicon, germanium, tin, plumbous, cadmium, zinc, sulphur, selenium, tellurium, boron, aluminium, gallium, indium, nitrogen, phosphorus, arsenic, one or more the elementary composition nano semiconductor materials in antimony, the size of described at least one dimension of nano semiconductor material is within the scope of 1 ~ 100nm;
Described non-quantum point fluorescent material comprises fluorescent RE powder, organic fluorescent powder.
When fluorescent material only adopts quantum dot, content R:G:B=3 ~ 7:10 ~ 15:6 ~ 11 of quantum dot.
Preferably, when fluorescent material only adopts quantum dot, the content R:G:B=5:13:8 of quantum dot.
It should be noted that, rgb color pattern is a kind of color standard of industry member, and namely RGB is the color representing red, green, blue three passages.Rgb color pattern is by obtaining color miscellaneous to the change of R (Red, red), G (Green, green), B (Blue, blue) three Color Channels and their superpositions each other.This standard almost include human eyesight can all colours of perception, be use one of the widest color system at present.
When described fluorescent material is made up of the mixture of quantum dot and non-quantum point fluorescent material, the mass fraction of described quantum dot is 0.01 ~ 10 part, and the mass fraction of described non-quantum point fluorescent material is 0.01 ~ 27 part.
Preferably, when described fluorescent material is made up of the mixture of quantum dot and non-quantum point fluorescent material, the mass fraction of described quantum dot is 0.01 ~ 5 part, and the mass fraction of described non-quantum point fluorescent material is 0.01 ~ 25 part.
Described resin comprise in epoxy resin, organic silica gel class, esters of acrylic acid, polyurethanes, ethylene-vinyl acetate resin and polycarbonate resin one or more;
Preferably, described resin is the one in epoxy resin, organic silica gel class, esters of acrylic acid, polyurethanes, ethylene-vinyl acetate resin and polycarbonate resin.
Further preferably, described resin is epoxy resin, acrylic resin adhesive, silicone resin or organic silicon resin adhesive.
Described resin be through the process of ultraviolet lamp photocuring or under the temperature condition of 10 DEG C ~ 180 DEG C through thermofixation process, the time of described photocuring or thermofixation is 3s ~ 150min.
Preferably, described resin be through the process of ultraviolet lamp photocuring or under the temperature condition of 20 DEG C ~ 150 DEG C through thermofixation process, the time of described photocuring or thermofixation is 5s ~ 120min.
Described filler comprise silicon-dioxide, calcium carbonate one or more.
Preferably, described filler is silicon-dioxide or calcium carbonate.
Further, the mode of described LED benefit/photoflash lamp cure package adopts photocuring or thermofixation, and wherein, the power of described photocuring is 50w ~ 15kw, and cure times is 0.1s ~ 90s; The temperature of described thermofixation is 60 DEG C ~ 180 DEG C, and the time of thermofixation is 10min ~ 80min.
Preferably, the mode of described LED benefit/photoflash lamp cure package adopts photocuring or thermofixation, and wherein, the power of described photocuring is 100w ~ 10kw, and cure times is 1s ~ 60s; The temperature of described thermofixation is 80 DEG C ~ 150 DEG C, and the time of thermofixation is 20min ~ 60min.
Further, when described fluorescent material is made up of quantum dot, described quantum dot fluorescence material is prepared by following methods and obtains:
The described quantum dot with different emission is mixed by mechanical stirring or sonic oscillation, obtains fluorescent material; Described fluorescent material and resin, filler are mixed by mechanical stirring or sonic oscillation, obtains mixture; By described mixture 20 ~ 30 DEG C, vacuumize 5 ~ 180min under 0.01 ~ 0.3MPa condition, obtain quantum dot fluorescence material;
Preferably, by described mixture 25 DEG C, vacuumize 10 ~ 60min under 0.1MPa condition, obtain quantum dot fluorescence material.
When described fluorescent material is made up of the mixture of quantum dot and non-quantum point fluorescent material, described quantum dot fluorescence material is prepared by following methods and obtains:
By described quantum dot and the mixing of non-quantum point fluorescent material, obtain fluorescent material; Described fluorescent material and resin, filler are mixed by mechanical stirring or sonic oscillation, obtains mixture; By described mixture 20 ~ 30 DEG C, vacuumize 5 ~ 180min under 0.01 ~ 0.3MPa condition, obtain quantum dot fluorescence material.
Preferably, by described mixture 25 DEG C, vacuumize 10 ~ 60min under 0.1MPa condition, obtain quantum dot fluorescence material.
A kind of LED benefit/photoflash lamp utilizing quantum dot fluorescent material to prepare provided by the invention, described LED benefit/photoflash lamp adopts quantum dot fluorescence material to be main raw material, described quantum dot fluorescence materials'use quantum dot as fluorescent material to replace traditional rare earth fluorescent material.Compared with fluorescent RE powder, quantum dot has incomparable luminescent properties, the fluorescent emission of such as size adjustable, the narrow and emmission spectrum of symmetry, wide and continuous print absorption spectrum, fabulous light stability.By regulating different sizes, the quantum dot of different emission can be obtained.Narrow and the fluorescent emission of symmetry makes quantum dot become a kind of material of desirable multi-color marking.Due to wide and continuous print absorption spectrum, just can excite the different fluorescence quantum of a series of wavelength with a laser source simultaneously.The light stability that quantum dot is good makes it can be good at being applied to imaging of tissue.
LED benefit/photoflash lamp the present invention being utilized quantum dot fluorescent material to prepare below and existing LED mend/and photoflash lamp does the contrast of main technical details, under the same conditions the results detailed in following table:
| Technical parameter | The present invention | Prior art |
| Luminous efficiency | 85-110 | 90-120 |
| Colour rendering index | 85-96 | 65-75 |
| Colour temperature | 3900-5800 | 5800-6500 |
It should be noted that, the detection method of above-mentioned technology contrast is: by the LED light supplement lamp of 1w be cured, carry out optical performance test, test light flux, colour rendering index, light efficiency, the parameters such as colour temperature with distant place constant current temp .-control integrating ball.
As from the foregoing, the described LED benefit/photoflash lamp utilizing quantum dot fluorescent material to prepare has that colour rendering index is high, colour temperature is low and the advantage such as light efficiency is strong, can significantly improve image capture device gather the real colour degree of image, effectively can improve the image color quality of imaging, develop the color true to nature, can be widely used on the equipment such as cell phone cameras photoflash lamp, camera flashlamp and pick up camera light compensating lamp.
The present invention is further illustrated below with specific embodiment, the preparation of quantum dot is set forth by embodiment 1 to 3, the preparation of quantum dot fluorescence material is set forth by embodiment 4 to 10, and set forth the preparation containing quantum dot fluorescent material LED benefit/photoflash lamp by embodiment 11 to 18, to be expressly understood the present invention, specific as follows:
One, the preparation of quantum dot:
Embodiment 1
There is according to document one-step synthesis quantum dot (the Single-step synthesis of quantum dots with chemical composition gradients of chemical constitution gradient-structure, Chemistry of Materials, 2008,20,531-539.) prepare the red quantum point that emission wavelength is 610nm.By 0.4mmol Cadmium oxide, 4mmol zinc acetate, 17.6mmol oleic acid and 20ml 1-octadecylene are put into 100ml flask and are mixed, be heated to 150 DEG C and vacuumize 20 minutes, then in a nitrogen atmosphere mixing liquid is heated to 310 DEG C, tri octyl phosphine injection of solution 3ml being dissolved with 1mmol selenium powder and 2.3mmol sulphur powder enters in the mixing liquid in flask, 300 DEG C are continued reaction 90 minutes, be cooled to after room temperature until system and add acetone, centrifugally to be precipitated, then chloroform dissolution precipitation is used, repeated precipitation dissolves three times, finally obtain quantum dot solid, or quantum dot solid dispersal is for subsequent use in toluene.
Embodiment 2
There is according to document CdSe@ZnS efficient LED (the Highly efficient green-light-emitting diodes based on CdSe@ZnS quantum dots with a chemical-composition gradient of chemical constitution gradient-structure, Advanced Materials, 2009,21,1690-1694.) prepare the green quantum dot that emission wavelength is 524nm.By 0.1mmol Cadmium oxide, 4mmol zinc acetate, 5ml oleic acid, 15ml 1-octadecylene is put into 100ml flask and is mixed, be heated to 150 DEG C and vacuumize 30 minutes, then in a nitrogen atmosphere mixing liquid is heated to 300 DEG C, tri octyl phosphine injection of solution 2ml being dissolved with 0.2mmol selenium powder and 3mmol sulphur powder enters in the mixing liquid in flask, 300 DEG C of reactions are after 10 minutes, add 0.5ml 1-spicy thioalcohol, 300 DEG C are continued reaction 2 hours, be cooled to after room temperature until system and add acetone, centrifugally to be precipitated, then chloroform dissolution precipitation is used, repeated precipitation dissolves three times, finally obtain quantum dot solid, or quantum dot solid dispersal is for subsequent use in chloroform.
Embodiment 3
According to nanocrystalline (the Gram-scale one-pot synthesis of highly luminescent blue emitting Cd1-xZnxS/ZnS nanocrystals of the high blue emission Cd1-xZnxS/ZnS of document one-step synthesis gram level, Chemistry of Materials, 2008,20,5307-5313.) prepare the blue quantum dot that emission wavelength is 443nm.By 1mmol Cadmium oxide, 10mmol zinc acetate, 7ml oleic acid, 15ml 1-octadecylene is put into 100ml flask and is mixed, be heated to 150 DEG C and vacuumize 30 minutes, then in a nitrogen atmosphere mixing liquid is heated to 300 DEG C, tributylphosphine injection of solution 3ml being dissolved with 1.7mmol sulphur enters in the mixing liquid in flask, 310 DEG C of reactions are after 8 minutes, drip the tributylphosphine solution that 4ml is dissolved with 8mmol sulphur, 300 DEG C are continued reaction 30 hours, be cooled to after room temperature until system and add acetone, centrifugally to be precipitated, then chloroform dissolution precipitation is used, repeated precipitation dissolves three times, finally obtain quantum dot solid, or quantum dot solid dispersal is for subsequent use in chloroform.
Two, the preparation of quantum dot fluorescence material
Embodiment 4
Select the formula of following quantum dot fluorescence material (setting quantum dot fluorescence quality of materials as 100 parts):
Quantum dot: solid quantum dot 0.01 part in embodiment 1
Fluorescent RE powder: yellow fluorescent powder 24.99 parts
Resin: epoxy resin 70 parts
Filler: silicon-dioxide 5 parts
By quantum dot and fluorescent RE powder mixing, then add resin and filler, mixed by mechanical stirring, under 25 DEG C of conditions, 0.1Mp vacuumizes 10min, is prepared into quantum dot fluorescence material.
Embodiment 5
Select the formula of following quantum dot fluorescence material (setting quantum dot fluorescence quality of materials as 100 parts):
Quantum dot: solid quantum dot 2.5 parts in embodiment 1
Fluorescent RE powder: yellow fluorescent powder 0.5 part
Resin: acrylic resin adhesive 67 parts
Filler: silicon-dioxide 30 parts
By quantum dot and fluorescent RE powder mixing, then add resin and filler, mixed by sonic oscillation, at 25 DEG C, 0.1MP vacuumizes 20min, prepares quantum dot fluorescent material.
Embodiment 6
Select the formula of following quantum dot fluorescence material (setting quantum dot fluorescence quality of materials as 100 parts):
Quantum dot: solid quantum dot 1 part in embodiment 1
Fluorescent RE powder: yellow fluorescent powder 18 parts
Resin: silicone resin 73 parts
Filler: 8 parts, calcium carbonate
By quantum dot and fluorescent RE powder mixing, then add resin and filler, mixed by mechanical stirring, at 25 DEG C, 0.1Mp vacuumizes 60min, prepares quantum dot fluorescent material.
Embodiment 7
Select the formula of following quantum dot fluorescence material (setting quantum dot fluorescence quality of materials as 100 parts):
Quantum dot: embodiment 1, the quantum dot of preparation in 2 and 3, configure white light by three primary colours, the total number of quantum dot is: 25 parts, the wherein content R:G:B=5:13:8 of quantum dot, that is the content embodiment 1 of quantum dot: embodiment 2: embodiment 3=5:13:8.
Resin: organic silicon resin adhesive 65 parts
Filler: 10 parts, calcium carbonate
Mixed by mechanical stirring by the quantum dot of preparation in embodiment 1,2 and 3, then add resin and filler, even by mechanically mixing, at 25 DEG C, 0.1Mp vacuumizes 90min, prepares quantum dot fluorescence material.
Embodiment 8
Select the formula of following quantum dot fluorescence material (setting quantum dot fluorescence quality of materials as 100 parts):
Quantum dot: quantum dot 10 parts in embodiment 1
Fluorescent RE powder: yellow fluorescent powder 15 parts
Resin: silicone resin 65 parts
Filler: silica 10 part
By quantum dot and fluorescent RE powder mixing, then add resin and filler, even by mechanically mixing, at 25 DEG C, 0.1Mp vacuumizes 120min, prepares quantum dot fluorescence material.
Embodiment 9
Select the formula of following quantum dot fluorescence material (setting quantum dot fluorescence quality of materials as 100 parts):
Quantum dot: solid quantum dot 5 parts in embodiment 1
Fluorescent RE powder: yellow fluorescent powder 27 parts
Resin: acrylic resin adhesive 60 parts
Filler: silicon-dioxide 8 parts
By quantum dot and fluorescent RE powder mixing, then add resin and filler, mixed by sonic oscillation, at 25 DEG C, 0.1MP vacuumizes 180min, prepares quantum dot fluorescent material.
Embodiment 10
Select the formula of following quantum dot fluorescence material (setting quantum dot fluorescence quality of materials as 100 parts):
Quantum dot: solid quantum dot 3 parts in embodiment 1
Fluorescent RE powder: yellow fluorescent powder 5 parts
Resin: silicone resin 90 parts
Filler: 2 parts, calcium carbonate
By quantum dot and fluorescent RE powder mixing, then add resin and filler, mixed by mechanical stirring, at 25 DEG C, 0.1Mp vacuumizes 100min, prepares quantum dot fluorescent material.
Three, the LED benefit/photoflash lamp utilizing quantum dot fluorescent material to prepare
Embodiment 11
Quantum dot fluorescence material embodiment 4 prepared, is coated on 1W blue-light LED chip by the mode of a glue, under 80 DEG C of conditions, solidifies 30min, prepares the LED benefit/photoflash lamp of quantum dot fluorescent material.
Embodiment 12
Quantum dot fluorescence material embodiment 5 prepared, be coated on 1W blue-light LED chip by the mode of spraying, Uv solidifies 10s, prepares the LED benefit/photoflash lamp of quantum dot fluorescent material.
Embodiment 13
Quantum dot fluorescence material embodiment 6 prepared, is coated on 1W blue-light LED chip by the mode of a glue, under 150 DEG C of conditions, solidifies 30min, prepares the LED benefit/photoflash lamp of quantum dot fluorescent material.
Embodiment 14
Quantum dot fluorescence material embodiment 6 prepared, is coated on 1W blue-light LED chip by the mode of a glue, under 100 DEG C of conditions, solidifies 60min, prepares the LED benefit/photoflash lamp of quantum dot fluorescent material.
Embodiment 15
Quantum dot fluorescence material embodiment 7 prepared, is coated on 1W blue-light LED chip by the mode of a glue, under 100 DEG C of conditions, solidifies 60min, prepares the LED benefit/photoflash lamp of quantum dot fluorescent material.
Embodiment 16
Quantum dot fluorescence material embodiment 8 prepared, is coated on 1W blue-light LED chip by the mode of a glue, under 120 DEG C of conditions, solidifies 60min, prepares the LED benefit/photoflash lamp of quantum dot fluorescent material.
Embodiment 17
Quantum dot fluorescence material prepared by embodiment 9, be coated on 1W blue-light LED chip by the mode of spraying, Uv solidifies 80s, prepare the LED benefit/photoflash lamp of quantum dot fluorescent material.
Embodiment 18
Quantum dot fluorescence material embodiment 10 prepared, is coated on 1W blue-light LED chip by the mode of a glue, under 180 DEG C of conditions, solidifies 80min, prepares the LED benefit/photoflash lamp of quantum dot fluorescent material.
By quantum dot fluorescence material LED benefit/photoflash lamp prepared by embodiment 11 to 18, mend with existing mobile phone on the market/photoflash lamp replaces mutually, such as Samsung (W899, I9300 etc.), Nokia (800, E63 etc.), colour rendering index significantly rises to about 90 from 70-80, the real colour degree of shooting image significantly improves, and develops the color true to nature.
Enumerate the technical parameter of embodiment 11 to 18 below, specific as follows:
| Technical parameter | Embodiment 11 | Embodiment 12 | Embodiment 13 | Embodiment 14 | Embodiment 15 | Embodiment 16 | Embodiment 17 | Embodiment 18 |
| Luminous efficiency | 111.6 | 109.4 | 103.5 | 105.6 | 97.5 | 99.8 | 102.1 | 101.9 |
| Colour rendering index | 86.7 | 90.5 | 91.3 | 92.2 | 95.7 | 92.5 | 93.2 | 92.4 |
| Colour temperature | 5853 | 5736 | 5624 | 5427 | 3652 | 5062 | 5627 | 5752 |
It should be noted that, the detection method of above-mentioned technology contrast is: by the LED light supplement lamp of 1w be cured, carry out optical performance test, test light flux, colour rendering index, light efficiency, the parameters such as colour temperature with distant place constant current temp .-control integrating ball.
In sum, implement the embodiment of the present invention, there is following beneficial effect:
One, a kind of LED benefit/photoflash lamp utilizing quantum dot fluorescent material to prepare provided by the invention, the fluorescent substance of described LED benefit/photoflash lamp is with quantum dot fluorescence material for main raw material, and described quantum dot fluorescence materials'use quantum dot is as fluorescent material.Because quantum dot belongs to semiconductor nano material, its particle size is at 1 ~ 100nm, and therefore, it is compared with conventional fluorescent material, and quantum dot adjusts the light of different emission by changing single-material size of particles; Secondly, because quantum dot has the characteristic of " wide band absorption, narrowband excitation ", quantum dot uv-visible absorption spectrum is wider, and therefore, the exciting light of single wavelength can excite the quantum dot with different emission; And luminous efficiency comparatively conventional fluorescent powder is high, its white light colour developing parameter be 90, far above the colour developing parameter 75 of existing white light LEDs.In addition, quantum dot has good light stability and makes it can be good at being applied to imaging of tissue.
Therefore, the described quantum dot fluorescent material that utilizes replaces traditional rare earth fluorescent material, preparation and the LED benefit/photoflash lamp that obtains have that colour rendering index is high, colour temperature is low and the advantage such as light efficiency is strong, can significantly improve image capture device gather the real colour degree of image, the image color quality of effective raising imaging, develop the color true to nature, can be widely used on the equipment such as cell phone cameras photoflash lamp, camera flashlamp and pick up camera light compensating lamp.In addition, the present invention substitutes fluorescent RE powder even completely with quantum dot fluorescence material component, therefore reduces the use even avoided rare earth material.
Two, a kind of fluorescent material that can be applicable to LED benefit/photoflash lamp provided by the invention, described fluorescent material uses quantum dot to replace traditional rare earth fluorescent material as fluorescent material, comparatively conventional fluorescent powder is high for luminous efficiency, have that colour rendering index is high, colour temperature is low and the feature such as light efficiency is strong, can significantly improve image capture device gather the real colour degree of image, decrease the undue dependence to fluorescent RE powder simultaneously, alleviate the overexploitation to rare earth resources, be conducive to the destruction of reducing mining area ecological environment.
Above disclosedly be only a kind of preferred embodiment of the present invention, certainly can not limit the interest field of the present invention with this, therefore according to the equivalent variations that the claims in the present invention are done, still belong to the scope that the present invention is contained.
Claims (4)
1. LED benefit/photoflash lamp, is characterized in that, described LED benefit/photoflash lamp is the LED chip surface by quantum dot fluorescence coated materials not encapsulated, and makes through cure package;
Wherein, described quantum dot fluorescence material is as follows in the main raw material formula of mass parts:
Fluorescent material 0.01 ~ 35;
Resin 60 ~ 90;
Filler 2 ~ 35;
Described fluorescent material forms by quantum dot or by the mixture of quantum dot and non-quantum point fluorescent material;
The mode of described LED benefit/photoflash lamp cure package comprises photocuring and thermofixation;
Described photocuring power is 50w ~ 15kw, and the time is 0.1s ~ 90s;
Described heat curing temperature is 60 DEG C ~ 180 DEG C, and the time is 10min ~ 80min;
When described fluorescent material is made up of the mixture of quantum dot and non-quantum point fluorescent material, the mass fraction of described quantum dot is 0.01 ~ 10 part, and the mass fraction of described non-quantum point fluorescent material is 0.01 ~ 27 part;
When fluorescent material only adopts quantum dot, content R: G: B=3 ~ 7: 10 ~ 15: 6 ~ 11 of quantum dot.
2. LED benefit/photoflash lamp as claimed in claim 1, it is characterized in that, described quantum dot is by carbon, silicon, germanium, tin, plumbous, cadmium, zinc, sulphur, selenium, tellurium, boron, aluminium, gallium, indium, nitrogen, phosphorus, arsenic, one or more the elementary composition nano semiconductor materials in antimony, the size of described at least one dimension of nano semiconductor material is within the scope of 1 ~ 100nm;
Described non-quantum point fluorescent material comprises fluorescent RE powder, organic fluorescent powder.
3. LED benefit/photoflash lamp as claimed in claim 1, is characterized in that, described resin comprise in epoxy resin, organic silica gel class, esters of acrylic acid, polyurethanes, ethylene-vinyl acetate resin and polycarbonate resin one or more.
4. LED benefit/photoflash lamp as claimed in claim 1, is characterized in that, described filler comprise in silicon-dioxide, calcium carbonate one or more.
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| CN103772872B (en) * | 2013-12-27 | 2016-06-01 | Tcl集团股份有限公司 | Quantum dot/acrylic ester polymer nano crystal composite and preparation method and Colours conversion films |
| CN104078537A (en) * | 2014-06-25 | 2014-10-01 | 南京工业大学 | Method for preparing LED by means of quantum dot composite fluorescent particles |
| CN104311979A (en) * | 2014-09-19 | 2015-01-28 | 金发科技股份有限公司 | Ethylene-vinyl acetate copolymer anti-counterfeiting film and preparation method thereof |
| CN106243739A (en) * | 2016-05-23 | 2016-12-21 | 史玉桂 | Preparation method of LED lamp piece with formaldehyde and toluene removing function |
| CN105990504A (en) * | 2016-07-06 | 2016-10-05 | 华南师范大学 | White LED with quantum dots cured and packaged by UV adhesive as fluorescence conversion material, and preparation method and applications thereof |
| US20190044034A1 (en) * | 2017-08-07 | 2019-02-07 | Sabic Global Technologies B.V. | Stable quantum dot extrusion film |
| CN107676740B (en) * | 2017-09-06 | 2019-09-20 | 深圳市华星光电技术有限公司 | A kind of quantum dot film, backlight module and display |
| CN107828042A (en) * | 2017-10-24 | 2018-03-23 | 中山市品诚光电实业有限公司 | A kind of power supply apparatus polyurethane high molecule material sealing technology |
| CN107663279B (en) * | 2017-10-31 | 2019-10-18 | 北京化工大学 | A kind of silica modified carbon dots fluorescent powder and fluorescence silicon rubber |
| CN107910425A (en) * | 2017-11-03 | 2018-04-13 | 深圳市迈科光电有限公司 | Photoflash and its packaging plastic |
| CN116814106A (en) * | 2023-07-05 | 2023-09-29 | 广东红海湾发电有限公司 | Fluorescent marking material for high-temperature-resistant flame-retardant photovoltaic cable and preparation method thereof |
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