WO2020228300A1 - 一种黄色荧光玻璃陶瓷的制备方法和应用 - Google Patents

一种黄色荧光玻璃陶瓷的制备方法和应用 Download PDF

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WO2020228300A1
WO2020228300A1 PCT/CN2019/122037 CN2019122037W WO2020228300A1 WO 2020228300 A1 WO2020228300 A1 WO 2020228300A1 CN 2019122037 W CN2019122037 W CN 2019122037W WO 2020228300 A1 WO2020228300 A1 WO 2020228300A1
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fluorescent glass
yellow fluorescent
glass ceramics
curing
slurry
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French (fr)
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肖文戈
刘畅
邱建荣
刘小峰
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Zhejiang University
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Zhejiang University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
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    • B33Y10/00—Processes of additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/006—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of microcrystallites, e.g. of optically or electrically active material
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
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    • B33Y70/00—Materials specially adapted for additive manufacturing
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    • B33Y70/00—Materials specially adapted for additive manufacturing
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    • B33Y80/00—Products made by additive manufacturing
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    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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    • C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
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    • C08F2/00—Processes of polymerisation
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    • C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F21K—NON-ELECTRIC LIGHT SOURCES USING LUMINESCENCE; LIGHT SOURCES USING ELECTROCHEMILUMINESCENCE; LIGHT SOURCES USING CHARGES OF COMBUSTIBLE MATERIAL; LIGHT SOURCES USING SEMICONDUCTOR DEVICES AS LIGHT-GENERATING ELEMENTS; LIGHT SOURCES NOT OTHERWISE PROVIDED FOR
    • F21K9/00—Light sources using semiconductor devices as light-generating elements, e.g. using light-emitting diodes [LED] or lasers
    • F21K9/60—Optical arrangements integrated in the light source, e.g. for improving the colour rendering index or the light extraction
    • F21K9/64—Optical arrangements integrated in the light source, e.g. for improving the colour rendering index or the light extraction using wavelength conversion means distinct or spaced from the light-generating element, e.g. a remote phosphor layer
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C35/0805—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation
    • B29C2035/0827—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation using UV radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
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  • the fluorescent glass ceramic of the present invention can obtain the required complex shape through 3D printing technology, and the size can reach several centimeters.
  • the preparation method of the yellow fluorescent ceramic glass ceramics of the present invention does not require special experimental conditions such as external pressure, strong current, high vacuum, etc., has low requirements on sintering equipment, simple synthesis and low cost.
  • Example 4 is a graph showing the variation of the luminous flux of the white light LED device packaged with yellow fluorescent glass ceramics and blue LD package with excitation light power in Example 2 of the present invention.
  • porous precursor obtained above into a high-temperature vacuum furnace and sinter it at 1150°C under vacuum (0.1Pa) for 2 hours to obtain a densified fluorescent glass ceramic, and then perform cutting and surface polishing treatments to obtain Fluorescent glass ceramic sheets of different sizes.

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Abstract

一种黄色荧光玻璃陶瓷的制备方法和应用。将单体、交联剂和填充溶剂混合均匀,加入气相二氧化硅并搅拌均匀,再加入紫外光引发剂和紫外线吸收剂充分搅拌;加入黄色荧光粉(Y,Gd)AG:Ce并充分搅拌和除泡;将浆料导入模具紫外照射固化成型,或者3D打印,获得坯体;将坯体放入高温炉加热,获得包覆荧光粉的多孔二氧化硅玻璃,再放入高温真空炉致密化烧结,从而得到致密化的荧光玻璃陶瓷;最后切割和表面抛光处理。

Description

一种黄色荧光玻璃陶瓷的制备方法和应用 技术领域
本发明属于发光材料和3D打印等技术领域,具体涉及一种黄色荧光玻璃陶瓷的制备方法和应用。
背景技术
白光LED由于具有能耗低、寿命长、体积小等诸多优点,而被公认为第四代照明光源。目前商用化的白光LED一般采用InGaN蓝光LED芯片激发黄色荧光粉(Y,Gd) 3Al 5O 12:Ce((Y,Gd)AG:Ce)的方案。这种荧光粉方案需要环氧树脂、有机硅树脂等高分子材料进行固化封装,而它们的热导率低且高温下易老化,因此发光过程中产生的热量无法快速扩散,导致白光LED的效率降低,存在色漂移、寿命短等问题。特别是以大功率蓝光LED芯片或者LD(激光二极管)作为激发光源时,上述问题尤为严重。因此,为了进一步提高白光LED的稳定性,并将其拓展到路灯、投影显示、汽车前大灯等高功率照明与显示领域,研发一种热导率高、物理化学稳定性优异的荧光转换材料是目前发光材料领域和固态照明产业均需亟待解决的问题。
为此,人们提出了三种替代传统荧光粉的方案:单晶(CN100389504C),透明陶瓷(US20090105065、CN102249660B和CN102832328B),和玻璃陶瓷(CN103496852B、CN107162427B和CN103159407B)。前两种虽然具有很高的热导率和优异的物理化学稳定性,但是其工艺复杂,成本高。荧光玻璃陶瓷由于兼具合成简单、物理化学稳定性较好等优点,是目前发光材料领域的研究重点。近年来,人们相继开发出了多种体系的荧光玻璃陶瓷,例如CN103496852B、CN107176791B和US20130334957A1。尽管这些荧光玻璃陶瓷的内量子效率高(>70%)、烧结温度低(<1000℃),但是其母体玻璃中含有价格高的成分,且物理化学稳定性仍不能满足LED器件在高功率、高热、高湿等条件下的长时间运行。石英玻璃是二氧化硅单一成分的非晶态材料,由于Si-O化学键能很大,结构很紧密,因此,石英玻璃具有高的紫外及可见光透过率和优异的物理化学稳定性。传统“荧光粉+玻璃微粉”混合烧结制备的以石英玻璃为母体的荧光玻璃陶瓷,由于石英玻璃在高温(>1500℃)下对荧光粉的强腐蚀作用而导致量子效率很低。王连军等人(CN103159407B)采用放电等离子体 烧结制备出了基于YAG:Ce与硅基介孔材料的高效荧光玻璃陶瓷。然而,该方法依靠强电流和高压来抑制母体玻璃对荧光粉的腐蚀,其所需设备昂贵,样品尺寸有限且形状仅限于块体,因而大大限制了其实际生产和应用。
3D打印是一种以数字模型文件为基础,采用流体状、粉末状等可固化、粘合、熔合材料,通过逐层打印来构造物体的技术。它可以实现快速个性化制造,制造出传统制造业无法完成的形状,已广泛应用于模具制造、工业设计等领域。本发明通过将3D打印技术应用于制备荧光玻璃陶瓷,从而实现快速制备尺寸大、形状复杂、量子效率高、物理化学稳定性优异的荧光玻璃陶瓷,并将其应用于高功率LED或者LD照明与显示领域。
发明内容
本发明的目的在于针对现有技术中的不足,提供一种黄色荧光玻璃陶瓷的制备方法。该方法可以结合3D打印技术,快速制备尺寸大、形状复杂、量子效率高、物理化学稳定性优异的荧光玻璃陶瓷。
本发明所采用的技术方案如下:
(1)浆料制备:
将55~75体积份数的单体、1~8体积份数的交联剂和15~40体积份数的填充溶剂混合均匀,获得混合溶液;然后加入气相二氧化硅并搅拌均匀,气相二氧化硅与混合溶液的体积比为3:7~5:5,再加入0.05~1wt%的紫外光引发剂和0.002~0.05wt%的紫外线吸收剂,充分搅拌;最后,加入黄色荧光粉(Y,Gd)AG:Ce并充分搅拌和除泡,黄色荧光粉与气相二氧化硅质量比为1:100~15:100,获得浆料;
(2)固化成形:将浆料导入所需形状的模具中在紫外灯下照射20~60s进行固化成型,或者将浆料通过光固化式3D打印机进行打印固化成型,获得坯体;
(3)排脂:将坯体放入高温炉中,缓慢加热到600~1000℃,在空气中保温1~10h,使有机物充分分解并排出,获得包覆荧光粉的多孔二氧化硅玻璃,作为多孔前驱体;
(4)烧结:将多孔前驱体放入高温真空炉中,在1050~1300℃和真空条件下进行致密化烧结0.5~6h,从而得到致密化的荧光玻璃陶瓷;
(5)抛光:将荧光玻璃陶瓷进行切割和表面抛光处理,最终获得所需尺寸的黄色荧光玻璃陶瓷,获得具有特定形状的、致密化的黄色荧光玻璃陶瓷。
优选地,所述的单体为甲基丙烯酸羟乙酯、丙烯酸羟乙酯、丙烯酸4-羟丁酯中的至少一种。
优选地,所述的交联剂为聚乙二醇二苯甲酸酯200、聚乙二醇二苯甲酸酯400中的至少一种。
优选地,所述的填充溶剂为二乙二醇二苯甲酸酯、苯氧乙醇、苯甲酸乙酯中的至少一种。
优选地,所述紫外光引发剂为819、651、184、1173中的至少一种。
优选地,所述紫外线吸收剂为1130、384、400、苏丹红G中的至少一种。
优选地,所述气相二氧化硅的平均粒径不大于50nm。
所述致密化烧结条件为真空条件,真空度为0.1Pa,使用旋片式真空泵即可获得。
本发明步骤(4)中的高温真空炉为普通的炉子,不需要等离子体的高压,仅需要0.1pa真空压力即可,在0.1pa真空压力就能实现黄色荧光玻璃陶瓷的制备,无需更高精度的更低的真空压力。
所述的坯体成型方法并不限于光固化方法,也可以通过将光固化剂改为热固化剂而采用热固化方法,甚至还可以直接使用PVA与气相二氧化硅混合制备步骤(1)中的浆料并采用热固化成型。
本发明制成的黄色荧光玻璃陶瓷在基于高功率蓝光LED或LD的固态照明与显示领域的应用。
高功率是指激发光功率密度大于1W/mm 2。
本发明上述提供的坯体成型方法是采用光固化方法。然而,该坯体的成型方法也可以采用热固化方法,此时可以将步骤(1)中的光固化剂改为相应的热固化剂,此外,还可以直接使用PVA与气相二氧化硅混合制备步骤(1)中的浆料并直接固化成型。
本发明所述的荧光玻璃陶瓷可以通过3D打印技术,获得所需的复杂形状,且尺寸可达到若干厘米。
本发明所述的黄色荧光玻璃陶瓷具有极好的化学稳定性,能在高热高湿条件下长时间经受高密度激发光辐照而不变性。
本发明所述的黄色荧光玻璃陶瓷可以直接与半导体固态光源封装出高亮度白光照明器件。
本发明的有益效果:
本发明涉及的黄色荧光陶玻璃陶瓷的制备方法,不需要外加压力、强电流和高真空等特殊实验条件,对烧结设备要求低,合成简单、成本低。
此外,本发明制成的浆料可以用于3D打印技术,可以快速制备出各种形状复杂的荧光玻璃陶瓷,例如常见的半球形、灯泡形、灯管形等,加上石英玻璃 具有极低的热膨胀系数、较高的热导率和优异的物理化学稳定性,可以封装出稳定性优异的高功率白光器件,并最大限度地满足照明器件的光学优化和艺术设计,真正实现荧光转换体与灯罩的一体化。
附图说明
图1为本发明实施例2中黄色荧光玻璃陶瓷的XRD谱图;
图2为本发明实施例2中黄色荧光玻璃陶瓷的激发和发射光谱图;
图3为本发明实施例2中黄色荧光玻璃陶瓷与蓝光LD封装的白光LED器件的光谱及参数图;
图4为本发明实施例2中黄色荧光玻璃陶瓷与蓝光LD封装的白光LED器件的光通量随激发光功率的变化曲线图。
图5为本发明实施例6中白光LED器件的电致发光光谱及参数图。
图6为本发明实施例6中帽子形黄色荧光玻璃陶瓷和白光LED器件。
具体实施方式
下面结合附图和具体实施例对本发明作进一步说明。
本发明实施例如下:
实施例中使用的黄色荧光粉(Y,Gd)AG:Ce,纳米级气相二氧化硅,以及其他有机原料都是市售的。
实施例1
将67vol%的甲基丙烯酸羟乙酯、3vol%的聚乙二醇二苯甲酸酯200和30vol%的二乙二醇二苯甲酸酯混合均匀;然后,加入平均粒径为50nm的气相二氧化硅并搅拌均匀,气相二氧化硅与溶液的体积比为4:6;在上述浆料中加入0.05wt%的紫外光引发剂819和0.03wt%的紫外线吸收剂剂苏丹红G,充分搅拌;最后,加入黄色荧光粉(Y,Gd)AG:Ce并充分搅拌和除泡,荧光粉与二氧化硅质量比为1:100。
将上述浆料导入硅胶模具中在1000W的365nm紫外灯下照射20s进行固化成型。将该坯体放入高温箱式炉中,缓慢加热(1℃/min)到800℃,在空气中保温3h,使有机物充分分解并排出,获得包覆荧光粉的多孔二氧化硅玻璃。
将上述得到的多孔前驱体放入高温真空炉中,在1250℃、真空(约0.1Pa)下烧结2h,即得到致密化的荧光玻璃陶瓷,并对其进行切割和表面抛光等处理,即可得到不同尺寸的荧光玻璃陶瓷片。
实施例2
将67vol%的甲基丙烯酸羟乙酯、3vol%的聚乙二醇二苯甲酸酯200和 30vol%的二乙二醇二苯甲酸酯混合均匀;然后,加入平均粒径为50nm的气相二氧化硅并搅拌均匀,气相二氧化硅与溶液的体积比为4:6;在上述浆料中加入0.05wt%的紫外光引发剂819和0.03wt%的紫外线吸收剂剂苏丹红G,充分搅拌;最后,加入黄色荧光粉(Y,Gd)AG:Ce并充分搅拌和除泡,荧光粉与二氧化硅质量比为5:100。
将上述浆料导入硅胶模具中在1000W的365nm紫外灯下照射20s进行固化成型。将该坯体放入高温箱式炉中,缓慢加热(1℃/min)到800℃,在空气中保温3h,使有机物充分分解并排出,获得包覆荧光粉的多孔二氧化硅玻璃。
将上述得到的多孔前驱体放入高温真空炉中,在1250℃、真空(0.1Pa)下烧结2h,即得到致密化的荧光玻璃陶瓷,并对其进行切割和表面抛光等处理,即可得到不同尺寸的荧光玻璃陶瓷片。本实施例所制备的荧光玻璃陶瓷的内量子效率为73%。将荧光玻璃陶瓷片放入高压水热釜中进行加速老化试验,以去离子水当溶剂,在200℃下反应10h后,其发光强度未发生变化,且玻璃基体保持完好。
附图1是本实施例制备的样品的XRD图谱。从附图1可知,该荧光玻璃陶瓷同时包含YAG的立方晶相和石英玻璃的非晶相。
附图2是本实施例制备的样品的激发和发射光谱。从附图2可知,该荧光玻璃陶瓷在420~500nm的蓝光激发下,发射出峰值波长为550nm的宽带黄光。
附图3是采用本实施例制备的荧光玻璃陶瓷片,结合功率可调蓝光LD封装的高功率白光器件的光谱及参数。该器件在2.23W的激发光下,可以获得355lm的白光,其相关色温(Tc)为6523,显色指数(Ra)为73.6,CIE坐标为(0.32,0.31)。
制成的白光LED器件的光通量随激发光功率的变化如图4所示。
实施例3
将67vol%的甲基丙烯酸羟乙酯、3vol%的聚乙二醇二苯甲酸酯200和30vol%的二乙二醇二苯甲酸酯混合均匀;然后,加入平均粒径为50nm的气相二氧化硅并搅拌均匀,气相二氧化硅与溶液的体积比为4:6;在上述浆料中加入0.05wt%的紫外光引发剂819和0.03wt%的紫外线吸收剂剂苏丹红G,充分搅拌;最后,加入黄色荧光粉(Y,Gd)AG:Ce并充分搅拌和除泡,荧光粉与二氧化硅质量比为15:100。
将上述浆料导入硅胶模具中在1000W的365nm紫外灯下照射20s进行固化成型。将该坯体放入高温箱式炉中,缓慢加热(1℃/min)到800℃,在空气中保温3h,使有机物充分分解并排出,获得包覆荧光粉的多孔二氧化硅玻璃。
将上述得到的多孔前驱体放入高温真空炉中,在1250℃、真空(0.1Pa)下烧结2h,即得到致密化的荧光玻璃陶瓷,并对其进行切割和表面抛光等处理,即可得到不同尺寸的荧光玻璃陶瓷片。
实施例4
将67vol%的甲基丙烯酸羟乙酯、3vol%的聚乙二醇二苯甲酸酯200和30vol%的二乙二醇二苯甲酸酯混合均匀;然后,加入平均粒径为10nm的气相二氧化硅并搅拌均匀,气相二氧化硅与溶液的体积比为4:6;在上述浆料中加入0.05wt%的紫外光引发剂819和0.03wt%的紫外线吸收剂剂苏丹红G,充分搅拌;最后,加入黄色荧光粉(Y,Gd)AG:Ce并充分搅拌和除泡,荧光粉与二氧化硅质量比为5:100。
将上述浆料导入硅胶模具中在1000W的365nm紫外灯下照射20s进行固化成型。将该坯体放入高温箱式炉中,缓慢加热(1℃/min)到800℃,在空气中保温3h,使有机物充分分解并排出,获得包覆荧光粉的多孔二氧化硅玻璃。
将上述得到的多孔前驱体放入高温真空炉中,在1150℃、真空(0.1Pa)下烧结2h,即得到致密化的荧光玻璃陶瓷,并对其进行切割和表面抛光等处理,即可得到不同尺寸的荧光玻璃陶瓷片。
实施例5
将67vol%的甲基丙烯酸羟乙酯、3vol%的聚乙二醇二苯甲酸酯200和30vol%的二乙二醇二苯甲酸酯混合均匀;然后,加入平均粒径为10nm的气相二氧化硅并搅拌均匀,气相二氧化硅与溶液的体积比为4:6;在上述浆料中加入0.05wt%的紫外光引发剂819和0.03wt%的紫外线吸收剂剂苏丹红G,充分搅拌;最后,加入黄色荧光粉(Y,Gd)AG:Ce并充分搅拌和除泡,荧光粉与二氧化硅质量比为5:100。
将上述浆料导入硅胶模具中在1000W的365nm紫外灯下照射20s进行固化成型。将该坯体放入高温箱式炉中,缓慢加热(1℃/min)到800℃,在空气中保温3h,使有机物充分分解并排出,获得包覆荧光粉的多孔二氧化硅玻璃。
将上述得到的多孔前驱体放入高温真空炉中,在1150℃、真空(0.1Pa)下烧结2h,即得到致密化的荧光玻璃陶瓷,并对其进行切割和表面抛光等处理,即可得到不同尺寸的荧光玻璃陶瓷片。
实施例6
将67vol%的甲基丙烯酸羟乙酯、3vol%的聚乙二醇二苯甲酸酯200和30vol%的二乙二醇二苯甲酸酯混合均匀;然后,加入平均粒径为50nm的气相二氧化硅并搅拌均匀,气相二氧化硅与溶液的体积比为4:6;在上述浆料中加入 0.05wt%的紫外光引发剂819和0.03wt%的紫外线吸收剂剂苏丹红G,充分搅拌;最后,加入黄色荧光粉(Y,Gd)AG:Ce并充分搅拌和除泡,荧光粉与二氧化硅质量比为5:100。
将上述浆料导入LCD光固化式3D打印机(光源波长为405nm)的料槽中,通过软件控制打印出预先设计的形状和尺寸(如帽子形,见附图6)。将该坯体放入高温箱式炉中,缓慢加热(1℃/min)到600℃,在空气中保温3h,使有机物充分分解并排出,获得包覆荧光粉的多孔二氧化硅玻璃。
将上述得到的多孔前驱体放入高温真空炉中,在1250℃、真空(0.1Pa)下烧结2h,即得到致密化的荧光玻璃陶瓷,并对其进行抛光处理,获得具有复杂形状的荧光玻璃陶瓷转换体,其内量子效率(IQE)为79%。
附图6为本实施例制备的帽子型的坯体和荧光玻璃陶瓷转换体及其封装的白光LED器件。此帽子形荧光玻璃陶瓷转换体的底部尺寸设计为与市购的1W蓝光LED芯片相同,因此,可以直接用于封装白光LED器件。附图5为该白光LED器件的电致发光光谱及参数。该器件的光效(LE)为96lm/W,相关色温(Tc)为5096,显色指数(Ra)为64.5,CIE坐标为(0.35,0.41)。
显然,上述实施例仅仅是为了清楚的说明所作的举例,在上述说明的基础上还可以做出其他形式的变动或变化。因此,由此所引申出的显而易见的变化或变动仍属于本发明的保护范围之内。本发明提供的一种黄色荧光玻璃陶瓷的制备方法所采用的有机溶剂为光固化型,然而,也可以使用热固化型有机溶剂,并通过热固化得到所需坯体。
由本发明实施可见,本发明方法工艺简单,可结合3D打印技术快速制备出形状复杂、物理化学性能稳定的荧光玻璃陶瓷,可利用黄色荧光玻璃陶瓷与高功率LED或者LD封装出高亮度白光器件,可应用于高功率照明和显示领域。

Claims (10)

  1. 一种黄色荧光玻璃陶瓷的制备方法,其特征在于,包括以下步骤:
    (1)浆料制备:将单体、交联剂和填充溶剂混合均匀获得混合溶液;然后加入气相二氧化硅并搅拌均匀,气相二氧化硅与混合溶液的体积比为3:7~5:5,再加入0.05~1wt%的紫外光引发剂和0.002~0.05wt%的紫外线吸收剂,充分搅拌;最后,加入黄色荧光粉(Y,Gd)AG:Ce并充分搅拌和除泡,黄色荧光粉与气相二氧化硅质量比为1:100~15:100,获得浆料;
    (2)固化成形:将浆料导入所需形状的模具中在紫外灯下照射20~60s进行固化成型,或者将浆料通过光固化式3D打印机进行打印固化成型,获得坯体;
    (3)排脂:将坯体放入高温炉中,加热到600~1000℃,在空气中保温1~10h,使有机物充分分解并排出,获得包覆荧光粉的多孔二氧化硅玻璃,作为多孔前驱体;
    (4)烧结:将多孔前驱体放入高温真空炉中,在1050~1300℃和真空条件下进行致密化烧结0.5~6h,从而得到致密化的荧光玻璃陶瓷;
    (5)抛光:将荧光玻璃陶瓷进行切割和表面抛光处理,最终获得所需尺寸的黄色荧光玻璃陶瓷。
  2. 根据权利要求1所述的一种黄色荧光玻璃陶瓷的制备方法,其特征在于:
    所述步骤(1)中,将55~75体积份数的单体、1~8体积份数的交联剂和15~40体积份数的填充溶剂混合均匀。
  3. 根据权利要求1所述的一种黄色荧光玻璃陶瓷的制备方法,其特征在于:
    所述的单体为甲基丙烯酸羟乙酯、丙烯酸羟乙酯、丙烯酸4-羟丁酯中的至少一种。
  4. 根据权利要求1所述的一种黄色荧光玻璃陶瓷的制备方法,其特征在于:
    所述的交联剂为聚乙二醇二苯甲酸酯200、聚乙二醇二苯甲酸酯400中的至少一种。
  5. 根据权利要求1所述的一种黄色荧光玻璃陶瓷的制备方法,其特征在于:
    所述的填充溶剂为二乙二醇二苯甲酸酯、苯氧乙醇、苯甲酸乙酯中的至少一种。
  6. 根据权利要求1所述的一种黄色荧光玻璃陶瓷的制备方法,其特征在于:
    所述紫外光引发剂为819、651、184、1173中的至少一种,所述紫外线吸收剂为1130、384、400、苏丹红G中的至少一种。
  7. 根据权利要求1所述的一种黄色荧光玻璃陶瓷的制备方法,其特征在于:
    所述气相二氧化硅的平均粒径不大于50nm。
  8. 根据权利要求1所述的一种黄色荧光玻璃陶瓷的制备方法,其特征在于:
    所述的坯体成型方法并不限于光固化方法,也可以通过将光固化剂改为热固化剂而采用热固化方法,甚至还可以直接使用PVA与气相二氧化硅混合制备步骤(1)中的浆料并采用热固化成型。
  9. 一种黄色荧光玻璃陶瓷,其特征在于,权利要求1-8任一所述制备方法制成的黄色荧光玻璃陶瓷。
  10. 一种权利要求9所述的黄色荧光玻璃陶瓷在基于高功率蓝光LED或LD的固态照明与显示领域的应用。
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