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CN104945878A - Preparation method of high-light-transmittance high-thermal-conductivity LED (light-emitting diode) lens - Google Patents

Preparation method of high-light-transmittance high-thermal-conductivity LED (light-emitting diode) lens Download PDF

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CN104945878A
CN104945878A CN201510372526.7A CN201510372526A CN104945878A CN 104945878 A CN104945878 A CN 104945878A CN 201510372526 A CN201510372526 A CN 201510372526A CN 104945878 A CN104945878 A CN 104945878A
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led lens
thermal conductivity
graphene
transmission rate
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陈晓松
刘日鑫
周慧
熊煦
唐惠东
肖雪军
李珊珊
徐亮成
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Changzhou Vocational Institute of Engineering
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K9/04Ingredients treated with organic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/04Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
    • G02B1/041Lenses
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

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Abstract

The invention relates to a preparation method of a high-light-transmittance high-thermal-conductivity LED (light-emitting diode) lens, which comprises the following steps: nano graphene surface modification, resin drying, mixing, extrusion granulation, injection molding and heat treatment. The nano graphene for modifying the traditional resin LED lens material can effectively enhance the light transmittance and thermal conductivity. When being applied to LEDs, the lens prepared from the modified resin can widen the application range of LEDs, and has longer service life. Compared with the preparation process of the traditional resin LED lens, the preparation technique of the high-light-transmittance high-thermal-conductivity LED lens does not have special requirements, and can perform production by using the original processing equipment.

Description

一种高透光率、高导热性的LED透镜的制备方法A kind of preparation method of LED lens with high light transmittance and high thermal conductivity

技术领域technical field

本发明属于照明领域,涉及一种高透光率、高导热性的LED透镜的制备方法。The invention belongs to the lighting field and relates to a method for preparing an LED lens with high light transmittance and high thermal conductivity.

背景技术Background technique

LED(Light Emitting Diode)是一类电致发光的固体器件,它可直接将电能转化为光能。由于具有发光效率高、使用寿命长、节能环保等优点,近年来已逐渐取代传统白炽灯、卤钨灯、日光灯管及冷阴极荧光灯等,在照明领域和液晶显示背光源方面得到越来越广泛的应用。而LED透镜是与LED紧密联系在一起有助于提升LED的出光效率、改变LED光场分布的光学系统,紧贴LED放置。用于制备LED透镜的树脂材料主要是聚碳酸酯(PC)或聚甲基丙烯酸甲酯(PMMA),通过注塑成型制得LED透镜。LED (Light Emitting Diode) is a kind of electroluminescent solid-state device, which can directly convert electrical energy into light energy. Due to the advantages of high luminous efficiency, long service life, energy saving and environmental protection, etc., it has gradually replaced traditional incandescent lamps, tungsten halogen lamps, fluorescent tubes and cold cathode fluorescent lamps in recent years, and has been widely used in the field of lighting and LCD backlight. Applications. The LED lens is an optical system that is closely connected with the LED to help improve the light output efficiency of the LED and change the light field distribution of the LED, and is placed close to the LED. The resin material used to prepare the LED lens is mainly polycarbonate (PC) or polymethyl methacrylate (PMMA), and the LED lens is made by injection molding.

PC和PMMA属于有机高分子材料,导热性和耐热性较差,制成LED透镜长时间使用或用于大功率LED中,在光源的持续作用下,热量会在材料中累积从而使其使用温度不断升高。当温度升高到一定程度时,PC和PMMA会变形黄变,最终影响LED透镜的透光率和使用寿命。PC and PMMA are organic polymer materials with poor thermal conductivity and heat resistance. They are made of LED lenses that are used for a long time or used in high-power LEDs. Under the continuous action of the light source, heat will accumulate in the material so that it can be used The temperature keeps rising. When the temperature rises to a certain level, PC and PMMA will deform and turn yellow, which will eventually affect the light transmittance and service life of the LED lens.

有关PC和PMMA透明材料导热性的改进研究,尤其是用纳米石墨烯改善其作为LED透镜材料使用的导热性的研究尚未见报道。Research on improving the thermal conductivity of PC and PMMA transparent materials, especially the use of nano-graphene to improve the thermal conductivity of its use as LED lens materials has not been reported.

同时,石墨烯层间有着强大的分子间作用力,各片层很容易堆叠在一起,并且难与有机高分子材料混合,但石墨烯的突出性能只有在各片层保持分离且均匀分散于高分子材料中时才能充分显现,因此必须对石墨烯进行表面修饰,从而改善其在PC或PMMA中的均匀分散。At the same time, there is a strong intermolecular force between graphene layers, and the layers are easy to stack together, and it is difficult to mix with organic polymer materials. Therefore, graphene must be surface-modified to improve its uniform dispersion in PC or PMMA.

因此,有必要探寻一种合理的改性方法,改善PC和PMMA的导热性能,避免材料结构变形和黄变,同时适度提高其透光率。用其制备LED透镜,可拓宽透镜的应用领域,并延长其使用寿命。Therefore, it is necessary to explore a reasonable modification method to improve the thermal conductivity of PC and PMMA, avoid material structural deformation and yellowing, and moderately increase its light transmittance. Using it to prepare LED lenses can broaden the application field of the lens and prolong its service life.

发明内容Contents of the invention

本发明要解决的技术问题是:基于上述问题,本发明提供一种高透光率、高导热性的LED透镜的制备方法。The technical problem to be solved by the present invention is: based on the above problems, the present invention provides a method for preparing an LED lens with high light transmittance and high thermal conductivity.

本发明解决其技术问题所采用的一个技术方案是:一种高透光率、高导热性的LED透镜的制备方法,包括以下步骤:A technical solution adopted by the present invention to solve the technical problem is: a method for preparing a LED lens with high light transmittance and high thermal conductivity, comprising the following steps:

(1)纳米石墨烯表面修饰:通过超声修饰的方法利用表面修饰剂对纳米石墨烯进行表面修饰;(1) Surface modification of graphene nanometers: surface modification of graphene nanometers with surface modifiers by means of ultrasonic modification;

(2)树脂干燥:控制PC或PMMA含水率为0~0.03%;(2) Resin drying: control the moisture content of PC or PMMA to 0-0.03%;

(3)混料:经表面修饰的纳米石墨烯与干燥的PC或PMMA粉料置于高速混合机中初混;(3) Mixing: the surface-modified nano-graphene and dry PC or PMMA powder are placed in a high-speed mixer for initial mixing;

(4)挤出造粒:将步骤(3)得到的初混料用双螺杆挤出机挤出造粒;(4) Extrusion granulation: the initial mixture that step (3) obtains is extruded granulation with a twin-screw extruder;

(5)注塑成型:将步骤(4)得到的粒料用精密注射机注塑成型;(5) Injection molding: injection molding of the pellets obtained in step (4) with a precision injection machine;

(6)热处理:将步骤(5)得到的注塑制品热处理。(6) Heat treatment: heat-treat the injection molded product obtained in step (5).

进一步地,步骤(1)中纳米石墨烯的表面修饰剂为偶联剂、油酸或阳离子表面活性剂中的一种或几种,表面修饰剂总用量为纳米石墨烯的2~20wt%。Further, in the step (1), the surface modifier of graphene nanometer is one or more of coupling agent, oleic acid or cationic surfactant, and the total amount of surface modifier is 2-20wt% of graphene nanometer.

进一步地,偶联剂为硅烷偶联剂或钛酸酯偶联剂中的一种或两种,阳离子表面活性剂为十六烷基三甲基溴化铵、十六烷基溴化吡啶或2-烷基咪唑啉中的一种或几种。Further, the coupling agent is one or both of silane coupling agent or titanate coupling agent, and the cationic surfactant is cetyltrimethylammonium bromide, cetylpyridinium bromide or One or more of 2-alkyl imidazolines.

进一步地,步骤(1)中超声修饰方法为将表面修饰剂溶于无水乙醇,加入纳米石墨烯,置于超声波清洗机中超声修饰,功率为40~500W,频率为50~200Hz,时间为20min~2h。Further, the ultrasonic modification method in step (1) is to dissolve the surface modification agent in absolute ethanol, add nano-graphene, and place it in an ultrasonic cleaning machine for ultrasonic modification, with a power of 40-500W, a frequency of 50-200Hz, and a time of 20min~2h.

进一步地,步骤(2)中光学级PC在110~120℃干燥12~24小时,光学级PMMA在80~85℃干燥4~5小时。Further, in step (2), the optical-grade PC is dried at 110-120°C for 12-24 hours, and the optical-grade PMMA is dried at 80-85°C for 4-5 hours.

进一步地,步骤(3)中混合料中经表面修饰的纳米石墨烯含量为PC或PMMA的1~25wt%,高速混合机转速300~500r/min,混合时间5~10min。Further, in step (3), the content of surface-modified graphene nanometers in the mixture is 1-25wt% of PC or PMMA, the speed of the high-speed mixer is 300-500r/min, and the mixing time is 5-10min.

进一步地,步骤(4)中PC料的挤出造粒温度为250~270℃,螺杆转速为50~80r/min;PMMA料的挤出造粒温度为150~230℃,螺杆转速为20~30r/min。Further, in the step (4), the extrusion granulation temperature of the PC material is 250-270°C, and the screw speed is 50-80r/min; the extrusion granulation temperature of the PMMA material is 150-230°C, and the screw speed is 20-80r/min. 30r/min.

进一步地,步骤(5)中PC料的注塑温度为250~320℃,注塑压力为60~120MPa,模温为80~120℃;PMMA料的注塑温度为180~240℃,注塑压力为80~130MPa,模温为40~80℃。Further, the injection temperature of PC material in step (5) is 250-320°C, the injection pressure is 60-120MPa, and the mold temperature is 80-120°C; the injection temperature of PMMA material is 180-240°C, and the injection pressure is 80-120°C. 130MPa, the mold temperature is 40-80°C.

进一步地,步骤(6)中PC制品在100~135℃下处理0.5~8小时,PMMA制品在70~80℃下处理3~6小时;PC注塑制品热处理可在同一温度段连续处理,也可分温度段连续处理。Further, in step (6), the PC product is treated at 100-135°C for 0.5-8 hours, and the PMMA product is treated at 70-80°C for 3-6 hours; the heat treatment of the PC injection molded product can be processed continuously at the same temperature section, or Continuous processing in different temperature sections.

本发明的有益效果是:利用纳米石墨烯改性传统树脂类LED透镜材料,能有效提高其透光率和导热性能;改性后的树脂制备的透镜应用于LED,可拓宽LED的应用领域,同时可延长LED透镜的使用寿命;高透光率、高导热性LED透镜的制备工艺相对于传统的树脂类LED透镜的制备无特殊要求,可用原有的加工设备生产。The beneficial effects of the present invention are: the use of nano-graphene to modify the traditional resin LED lens material can effectively improve its light transmittance and thermal conductivity; the lens prepared by the modified resin is applied to the LED, which can broaden the application field of the LED. At the same time, the service life of the LED lens can be extended; the preparation process of the high light transmittance and high thermal conductivity LED lens has no special requirements compared with the preparation of the traditional resin LED lens, and can be produced by the original processing equipment.

具体实施方式Detailed ways

现在结合具体实施例对本发明作进一步说明,以下实施例旨在说明本发明而不是对本发明的进一步限定。The present invention will now be further described in conjunction with specific examples, and the following examples are intended to illustrate the present invention rather than further limit the present invention.

实施例1Example 1

将相对于纳米石墨烯总量2wt%的硅烷偶联剂KH560、1wt%的油酸和1.5wt%的十六烷基三甲基溴化铵溶于无水乙醇,加入一定量的纳米石墨烯,置于超声清洗机中,设定频率60Hz、功率80W,超声处理1h,烘干。将光学级PC粉末在120℃常压热风干燥12小时后,与5wt%表面修饰后的纳米石墨烯用高速混合机高速混合8min,高速混合机转子转速设定为500r/min。混合料用双螺杆挤出机挤出造粒,挤出温度为250~265℃,螺杆转速为60r/min。改性粒料注塑成型,注塑温度为280~300℃,注塑压力为80MPa,模温为100℃。注塑样品置于热风循环干燥箱中加热到100~105℃保持20min,继续加热到120~125℃保持30min,随干燥箱一起冷却至室温。上述用表面修饰纳米石墨烯改性的PC材料与未改性PC材料相比,其性能如下表所示:The silane coupling agent KH560, the oleic acid of 1wt% and the hexadecyltrimethylammonium bromide of 1.5wt% are dissolved in dehydrated alcohol with respect to the nano graphene total amount 2wt%, add a certain amount of nano graphene , placed in an ultrasonic cleaning machine, set the frequency at 60 Hz, and the power at 80 W, ultrasonically treated for 1 hour, and dried. After drying the optical-grade PC powder at 120° C. for 12 hours with hot air under normal pressure, it was mixed with 5 wt % surface-modified nano-graphene for 8 minutes at high speed in a high-speed mixer, and the rotor speed of the high-speed mixer was set at 500 r/min. The mixture is extruded and granulated with a twin-screw extruder, the extrusion temperature is 250-265°C, and the screw speed is 60r/min. The modified pellets are injection molded, the injection temperature is 280-300°C, the injection pressure is 80MPa, and the mold temperature is 100°C. The injection molded sample is placed in a hot air circulation drying oven and heated to 100-105°C for 20 minutes, then heated to 120-125°C for 30 minutes, and cooled to room temperature together with the drying oven. Compared with the unmodified PC material, the performance of the above-mentioned PC material modified with surface-modified nano-graphene is shown in the following table:

实施例2Example 2

将相对于纳米石墨烯总量2wt%的硅烷偶联剂KH560、1wt%的油酸和1.5wt%的十六烷基三甲基溴化铵溶于无水乙醇,加入一定量的纳米石墨烯,置于超声清洗机中,设定频率60Hz、功率80W,超声处理1h,烘干。将光学级PMMA粉末在85℃常压热风干燥5小时后,与5wt%表面修饰后的纳米石墨烯用高速混合机高速混合5min,高速混合机转子转速设定为500r/min。混合料用双螺杆挤出机挤出造粒,挤出温度为170~200℃,螺杆转速为30r/min。改性粒料注塑成型,注塑温度为190~220℃,注塑压力为100MPa,模温为60℃。注塑样品置于热风循环干燥箱中加热到75~80℃保持6小时,随干燥箱一起冷却至室温。上述用表面修饰纳米石墨烯改性的PMMA材料与未改性PMMA材料相比,其性能如下表所示:The silane coupling agent KH560, the oleic acid of 1wt% and the hexadecyltrimethylammonium bromide of 1.5wt% are dissolved in dehydrated alcohol with respect to the nano graphene total amount 2wt%, add a certain amount of nano graphene , placed in an ultrasonic cleaning machine, set the frequency at 60 Hz, and the power at 80 W, ultrasonically treated for 1 hour, and dried. After drying the optical grade PMMA powder at 85°C with hot air under normal pressure for 5 hours, it was mixed with 5wt% surface-modified nano-graphene for 5 minutes at high speed with a high-speed mixer, and the rotor speed of the high-speed mixer was set at 500r/min. The mixture is extruded and granulated by a twin-screw extruder, the extrusion temperature is 170-200°C, and the screw speed is 30r/min. The modified pellets are injection molded, the injection temperature is 190-220°C, the injection pressure is 100MPa, and the mold temperature is 60°C. The injection molded samples were placed in a hot air circulation drying oven and heated to 75-80°C for 6 hours, and then cooled to room temperature together with the drying oven. The above-mentioned PMMA material modified with surface-modified nano-graphene is compared with the unmodified PMMA material, and its performance is shown in the following table:

以上述依据本发明的理想实施例为启示,通过上述的说明内容,相关工作人员完全可以在不偏离本项发明技术思想的范围内,进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容,必须要根据权利要求范围来确定其技术性范围。Inspired by the above-mentioned ideal embodiment according to the present invention, through the above-mentioned description content, relevant workers can make various changes and modifications within the scope of not departing from the technical idea of the present invention. The technical scope of the present invention is not limited to the content in the specification, but must be determined according to the scope of the claims.

Claims (9)

1. a preparation method for the LED lens of high transmission rate, high thermal conductivity, is characterized in that: comprise the following steps:
(1) nano-graphene finishing: utilize coating materials to carry out finishing to nano-graphene by the method for ultrasonic modification;
(2) resin drying: control PC or PMMA water ratio are 0 ~ 0.03%;
(3) batch mixing: nano-graphene and dry PC or the PMMA powder of surface modification are placed in high-speed mixer and just mix;
(4) extruding pelletization: the first batch mixing twin screw extruder extruding pelletization that step (3) is obtained;
(5) injection moulding: the pellet precise injection machine injection moulding that step (4) is obtained;
(6) thermal treatment: the injection-molded item thermal treatment that step (5) is obtained.
2. the preparation method of the LED lens of a kind of high transmission rate according to claim 1, high thermal conductivity, it is characterized in that: in described step (1), the coating materials of nano-graphene is one or more in coupling agent, oleic acid or cats product, and the total consumption of coating materials is 2 ~ 20wt% of nano-graphene.
3. the preparation method of the LED lens of a kind of high transmission rate according to claim 2, high thermal conductivity, it is characterized in that: described coupling agent is one or both in silane coupling agent or titanate coupling agent, and cats product is one or more in cetyl trimethylammonium bromide, cetyl pyridinium bromide or 2-alkyl imidazoline.
4. the preparation method of the LED lens of a kind of high transmission rate according to claim 1, high thermal conductivity, it is characterized in that: in described step (1), ultrasonic modifying method is for be dissolved in dehydrated alcohol by coating materials, add nano-graphene, be placed in the ultrasonic modification of Ultrasonic Cleaners, power is 40 ~ 500W, frequency is 50 ~ 200Hz, and the time is 20min ~ 2h.
5. the preparation method of the LED lens of a kind of high transmission rate according to claim 1, high thermal conductivity, it is characterized in that: in described step (2), optical grade PC was 110 ~ 120 DEG C of dryings 12 ~ 24 hours, and optical grade PMMA was 80 ~ 85 DEG C of dryings 4 ~ 5 hours.
6. the preparation method of the LED lens of a kind of high transmission rate according to claim 1, high thermal conductivity, it is characterized in that: in described step (3), in compound, the nano-graphene content of surface modification is the 1 ~ 25wt% of PC or PMMA, high-speed mixer rotating speed 300 ~ 500r/min, mixing time 5 ~ 10min.
7. the preparation method of the LED lens of a kind of high transmission rate according to claim 1, high thermal conductivity, is characterized in that: in described step (4), the extruding pelletization temperature of PC material is 250 ~ 270 DEG C, and screw speed is 50 ~ 80r/min; The extruding pelletization temperature of PMMA material is 150 ~ 230 DEG C, and screw speed is 20 ~ 30r/min.
8. the preparation method of the LED lens of a kind of high transmission rate according to claim 1, high thermal conductivity, it is characterized in that: in described step (5), the injection temperature of PC material is 250 ~ 320 DEG C, injection pressure is 60 ~ 120MPa, and mould temperature is 80 ~ 120 DEG C; The injection temperature of PMMA material is 180 ~ 240 DEG C, and injection pressure is 80 ~ 130MPa, and mould temperature is 40 ~ 80 DEG C.
9. the preparation method of the LED lens of a kind of high transmission rate according to claim 1, high thermal conductivity, it is characterized in that: in described step (6), PC goods process 0.5 ~ 8 hour at 100 ~ 135 DEG C, and PMMA goods process 3 ~ 6 hours at 70 ~ 80 DEG C; The thermal treatment of PC injection-molded item can process continuously in same temperature section, and temperature section also can be divided to process continuously.
CN201510372526.7A 2015-06-30 2015-06-30 Preparation method of high-light-transmittance high-thermal-conductivity LED (light-emitting diode) lens Pending CN104945878A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107365470A (en) * 2017-06-29 2017-11-21 上海金山锦湖日丽塑料有限公司 A kind of high heat-resisting HI high impact PMMA resins and preparation method thereof
CN108864679A (en) * 2018-07-18 2018-11-23 望江县天长光学仪器有限公司 A kind of preparation method of wear-resisting lens

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107365470A (en) * 2017-06-29 2017-11-21 上海金山锦湖日丽塑料有限公司 A kind of high heat-resisting HI high impact PMMA resins and preparation method thereof
CN107365470B (en) * 2017-06-29 2019-09-17 上海金山锦湖日丽塑料有限公司 A kind of high heat resistance HI high impact PMMA resin and preparation method thereof
CN108864679A (en) * 2018-07-18 2018-11-23 望江县天长光学仪器有限公司 A kind of preparation method of wear-resisting lens

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Application publication date: 20150930