WO2018103481A1 - 陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器 - Google Patents

陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器 Download PDF

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WO2018103481A1
WO2018103481A1 PCT/CN2017/109317 CN2017109317W WO2018103481A1 WO 2018103481 A1 WO2018103481 A1 WO 2018103481A1 CN 2017109317 W CN2017109317 W CN 2017109317W WO 2018103481 A1 WO2018103481 A1 WO 2018103481A1
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phosphor
ceramic composite
alumina
coated
particle diameter
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PCT/CN2017/109317
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English (en)
French (fr)
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李乾
许颜正
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深圳市绎立锐光科技开发有限公司
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Priority to EP17879386.5A priority Critical patent/EP3553041B1/en
Priority to US16/468,112 priority patent/US11267762B2/en
Publication of WO2018103481A1 publication Critical patent/WO2018103481A1/zh
Priority to US17/647,810 priority patent/US11697621B2/en

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Abstract

一种陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器,其中,制备方法包括步骤:按Al 2O 3与荧光粉质量比(0.1~1):100,分别配置铝盐溶液与荧光粉;将荧光粉分散于pH值为4.5~5.5的缓冲溶液,得到悬浮液;用铝盐溶液对悬浮液进行滴定,得到包覆有Al 2O 3水合物薄膜的荧光粉;将包覆有Al 2O 3水合物薄膜的荧光粉进行煅烧,得到Al 2O 3包覆的荧光粉;将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好,得到混合氧化铝粉末;将Al 2O 3包覆的荧光粉与混合氧化铝粉末进行混合,得到混合粉末,其中,Al 2O 3包覆的荧光粉占混合粉末重量的40%~90%;对混合粉末进行预压制、烧结,得到陶瓷复合材料。

Description

陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器 技术领域
本发明涉及发光材料技术领域,特别涉及一种陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器。
背景技术
在照明显示领域,波长转换装置的荧光粉封装主要是有机树脂、有机硅胶和无机玻璃的封装,该类技术方案的波长转换装置导热差、耐热差。为解决这一问题,有技术将荧光粉与可透光的无机陶瓷烧结在一起,获得的陶瓷复合材料具有很高的热导率性能和耐热性能。
目前,对于荧光粉封装于Al2O3的陶瓷复合材料而言,普遍存在着荧光粉相与Al2O3相之间结合力较弱的问题,导致其机械性能不高。并且,陶瓷复合材料大多还存在光效偏低,加工过程中易出现荧光粉颗粒拔出、表面难抛光等问题,从而影响陶瓷复合材料的性能。
发明内容
本发明的主要目的是提供一种陶瓷复合材料的制备方法,旨在制得高光效、高热导率、高机械性能的陶瓷复合材料。
为实现上述目的,本发明提出的陶瓷复合材料的制备方法包括以下步骤:
按Al2O3与荧光粉质量比(0.1~1):100,分别配置铝盐溶液与荧光粉;
将所述荧光粉分散于pH值为4.5~5.5的缓冲溶液,得到悬浮液;
用所述铝盐溶液对所述悬浮液进行滴定,得到包覆有Al2O3水合物薄膜的荧光粉;
将所述包覆有Al2O3水合物薄膜的荧光粉进行煅烧,得到Al2O3包覆的荧光粉;
将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好,得到混合氧化铝粉末;
将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合,得到混合粉末,其中,所述Al2O3包覆的荧光粉占所述混合粉末重量的40%~90%;
对所述混合粉末进行预压制、烧结,得到所述陶瓷复合材料。
可选地,所述荧光粉包含Ca3Al2Si3O12、Ca3Sc2Si3O12、Gd3Al5O12、Gd3Ga5O12、Tb3Al5O12、Tb3Ga5O12、Y3Al5O12、Y3Ga5O12、Lu3Al5O12、Lu3Ga5O12及Y3Mg2AlSi2O12的掺杂有Ce3+的荧光粉中的至少一种。
可选地,所述荧光粉的粒径范围是13μm~20μm。
可选地,所述铝盐溶液的浓度为0.01mol/L~1mol/L。
可选地,在所述用所述铝盐溶液对所述悬浮液进行滴定的步骤中,所述悬浮液的温度为40℃~70℃,搅拌速率为100r/min~300r/min,滴定速度为5mL/min~50mL/min。
可选地,所述煅烧过程中,煅烧温度为300℃~600℃,煅烧时间为2h~5h。
可选地,所述预压制过程在5MPa~15MPa压强下进行。
可选地,所述烧结过程在氩气气氛下进行,烧结温度为1250℃~1550℃,烧结压力为30MPa~200MPa,保温时间为30min~360min。
可选地,在所述将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好的步骤中,还加入粒径为0.01μm~0.1μm的氧化铝粉末,所述0.01μm~0.1μm的氧化铝粉末与所述0.1μm~1μm的氧化铝粉末的摩尔比为(0.1~1):100。
可选地,所述将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合的步骤包括:
将所述混合氧化铝粉末分散于质量百分浓度为1wt%~3wt%的PEG4000-乙醇溶液中,并置于球磨罐中,球磨6h~24h;
将所述Al2O3包覆的荧光粉加入所述球磨罐中,继续球磨30min~60min。
本发明还提出一种陶瓷复合材料,该陶瓷复合材料包括氧化铝基质、均匀分布于所述氧化铝基质的荧光粉、及均匀分布于所述氧化铝基质的散射中心,所述氧化铝基质为氧化铝陶瓷,所述散射中心为氧化铝颗粒,且所述氧化铝颗粒的粒径范围是1μm~10μm,荧光粉的粒径范围是13μm~20μm。
本发明还提出一种波长转换器,该波长转换器包括如上所述的陶瓷复合 材料。
本发明的技术方案,通过液相沉淀法,可先将微量细小粒径的Al2O3颗粒(即Al2O3薄膜)包覆于荧光粉颗粒表面,之后通过将产物与中等粒径的Al2O3颗粒、较大粒径的Al2O3颗粒进行混合,可使得包覆于荧光粉颗粒表面的微量细小粒径的Al2O3颗粒(即Al2O3薄膜)在烧结中能够率先进入液相,使得陶瓷复合材料的烧结性能得以改善,并可有效提高陶瓷复合材料中荧光粉相与Al2O3相之间的结合力。同时,通过溶解-再析出机制,可有效抑制中等粒径的Al2O3颗粒在烧结过程中的异常长大,提升Al2O3基体的各项性能。而较大粒径的Al2O3颗粒,则可作为陶瓷复合材料中的散射粒子。从而,制备得到高光效、高热导率、高机械性能的陶瓷复合材料。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
另外,各个实施例之间的技术方案可以相互结合,但是必须是以本领域普通技术人员能够实现为基础,当技术方案的结合出现相互矛盾或无法实现时应当认为这种技术方案的结合不存在,也不在本发明要求的保护范围之内。
本发明提出一种陶瓷复合材料的制备方法,旨在制得高光效、高热导率、高机械性能、蓝光透过率可调的陶瓷复合材料,以应用于高性能激光光源。
该陶瓷复合材料的制备方法,包括以下步骤:
步骤S100,按Al2O3与荧光粉质量比(0.1~1):100,分别配置铝盐溶液与荧光粉。其中,
所述荧光粉包含Ca3Al2Si3O12、Ca3Sc2Si3O12、Gd3Al5O12、Gd3Ga5O12、Tb3Al5O12、Tb3Ga5O12、Y3Al5O12、Y3Ga5O12、Lu3Al5O12、Lu3Ga5O12及Y3Mg2AlSi2O12的掺杂有Ce3+的荧光粉中的至少一种。并且,所述荧光粉的粒径范围为13μm~20μm,优选为15μm~17μm。
所述铝盐溶液的浓度为0.01mol/L~1mol/L,优选为0.2mol/L~0.5mol/L。
所述铝盐溶液可选用硝酸铝溶液。
应当理解的,在实际配置铝盐溶液与荧光粉时,首先确定Al2O3与荧光粉的质量比,并称取一定质量的荧光粉;之后,根据荧光粉的质量以及Al2O3与荧光粉的质量比,计算得到所需Al2O3的质量,再经换算即可得到Al3+的摩尔数;继而根据Al3+的摩尔数换算出对应的铝盐的质量;最后,称取对应质量的铝盐进行配置,即可得到铝盐溶液,完成分别配置铝盐溶液与荧光粉的步骤。
步骤S200,将所述荧光粉分散于pH值为4.5~5.5的缓冲溶液,得到悬浮液。其中,所述缓冲溶液可选用柠檬酸-氢氧化钠溶液,且所述柠檬酸-氢氧化钠溶液中柠檬酸的浓度可为0.8mol/L~1.2mol/L。
并且,将荧光粉分散于缓冲溶液之前,预先向缓冲溶液中加入1wt%~3wt%的PEG4000。
步骤S300,用所述铝盐溶液对所述悬浮液进行滴定,得到包覆有Al2O3水合物薄膜的荧光粉。其中,
滴定过程中,悬浮液的温度为40℃~70℃,搅拌速率为100r/min~300r/min,滴定速度为5mL/min~50mL/min。
滴定完毕后,持续保温和搅拌1h~2h,并可选用氢氧化钠溶液将pH值调整到6~7的范围。
步骤S400,将所述包覆有Al2O3水合物薄膜的荧光粉进行煅烧,得到Al2O3包覆的荧光粉。其中,
煅烧步骤前,包括:
将包覆有Al2O3水合物薄膜的荧光粉进行离心分离;
将分离所得的包覆有Al2O3水合物薄膜的荧光粉进行水洗、脱水3-5次,并在75℃~85℃下烘干。
在煅烧过程中,煅烧温度为300℃~600℃,煅烧时间为2h~5h。
需要说明的是,此时,荧光粉表面包覆的为细小粒径的Al2O3颗粒。
步骤S500,将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好,得到混合氧化铝粉末。其中,
粒径为0.1μm~1μm的氧化铝粉末(即中等粒径的Al2O3颗粒)优选粒径范围是0.1μm~0.3μm。
粒径为1μm~10μm的氧化铝粉末(即较大粒径的Al2O3颗粒)优选粒径范围是3μm~5μm。
进一步地,在混合氧化铝粉末中,还可加入粒径为0.01μm~0.1μm的氧化铝粉末,其优选粒径范围是0.02μm~0.05μm,并且,粒径为0.01μm~0.1μm的氧化铝粉末与粒径为0.1μm~1μm的氧化铝粉末的摩尔比为(0.1~1):100。
步骤S600,将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合,得到混合粉末,其中,所述Al2O3包覆的荧光粉占所述混合粉末重量的40%~90%。其中,
优选地,Al2O3包覆的荧光粉占总粉末重量的50%~70%。
所述将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合的步骤包括:
将所述混合氧化铝粉末分散于质量百分浓度为1wt%~3wt%的PEG4000-乙醇溶液中,并置于球磨罐中,球磨6h~24h;
将所述Al2O3包覆的荧光粉加入所述球磨罐中,继续球磨30min~60min。
步骤S700,对所述混合粉末进行预压制、烧结,得到所述陶瓷复合材料。其中,
所述预压制过程在5MPa~15MPa压强下进行。
所述烧结过程在氩气气氛下进行,烧结温度为1250℃~1550℃,烧结压力为30MPa~200MPa,保温时间为30min~360min。其中,烧结压力优选为40MPa~100MPa。
需要说明的是,适当的控制烧结温度,可使得混合粉末在烧结过程中,细小粒径的Al2O3颗粒和中等粒径的Al2O3颗粒能够充分进入液相进行烧结,较大粒径的Al2O3颗粒则只有部分参与烧结,或不参与烧结,而荧光粉则不参与烧结。其中,荧光粉的晶型及晶粒尺寸不发生改变,较大粒径的Al2O3颗粒的 晶型会由其他相转变为α相,而其尺寸会因为溶解再析出机制而增大。
本发明技术方案中的溶解再析出机制为:烧结过程中,细小粒径的Al2O3颗粒会率先进入液相,并充分熔化,中等粒径的Al2O3颗粒会部分进入液相,并且,粒径越小的颗粒越容易进入液相。这些液相会在颗粒间隙中流动,成为物质迁移的主要方式。当这些液相流过大颗粒表面时,会在其表面析出Al2O3小晶粒(小颗粒表面也可析出Al2O3小晶粒的可能,只是在大颗粒表面析出的可能更大,程度更高),此时,Al2O3小晶粒析出分两种类型:
一是在荧光粉颗粒表面析出,但是由于荧光粉并不参与烧结,这些析出的Al2O3小晶粒会和周围的Al2O3晶粒通过烧结颈连接-融合-长大,成为与荧光粉颗粒紧密相连的氧化铝相;
二是在较大粒径的Al2O3颗粒表面析出,这些Al2O3小晶粒的部分(根据温度的不同,程度会不同)会与较大粒径的Al2O3颗粒相结合(被较大粒径的Al2O3颗粒吞并)变成更大的颗粒,同时吸收大量的能量。而较大粒径的Al2O3颗粒的继续长大,实际上就削弱了中等粒径的Al2O3颗粒的异常长大现象,促使占绝大部分比例的中等粒径的Al2O3颗粒长大的均匀性,从而使得光学和机械性能得以有效提高。
烧结后的陶瓷中,细小粒径的Al2O3颗粒和中等粒径的Al2O3颗粒为陶瓷的连续基质,具有一定的透光性能,荧光粉和较大粒径的Al2O3颗粒则成为分散于陶瓷的连续基质中的颗粒,对光具有散射作用。其中,荧光粉具有对如445nm~460nm的短波长的蓝光的吸收作用,较大粒径的Al2O3颗粒则对短波长至可见光波长范围内的光具有散射和反射作用。并且,通过调整较大粒径的Al2O3颗粒的含量,可改变蓝光的穿透和散射程度,进而可改变陶瓷复合材料的色温。
因此,可以理解的,本发明技术方案,通过液相沉淀法,可先将微量细小粒径的Al2O3颗粒(即Al2O3薄膜)包覆于荧光粉颗粒表面,之后通过将产物与中等粒径的Al2O3颗粒、较大粒径的Al2O3颗粒进行混合,可使得包覆于荧光粉颗粒表面的微量细小粒径的Al2O3颗粒(即Al2O3薄膜)在烧结中能够率先进入液相,使得陶瓷复合材料的烧结性能得以改善,并可有效提高陶瓷复合材料中荧光粉相与Al2O3相之间的结合力。同时,通过溶解-再析出机制,可有效抑制中等粒径的Al2O3颗粒在烧结过程中的异常长大,提升Al2O3基体的各项性 能。而较大粒径的Al2O3颗粒,则可作为陶瓷复合材料中的散射粒子。从而,制备得到高光效、高热导率、高机械性能、蓝光透过率可调的陶瓷复合材料。
以下通过具体实施例对本发明技术方案进行具体说明。
实施例1:
称取适量的粒径为13μm~20μm的YAG:Ce3+荧光粉。
按照Al2O3与YAG:Ce3+荧光粉质量比1:100的比例,称取相应量的Al(NO3)3·9H2O配制成1mol/L的硝酸铝溶液。
配制pH值为5.0、浓度为1.0mol/L的柠檬酸-氢氧化钠溶液,继而加入2wt%的PEG4000,并进行超声溶解。之后,加入YAG:Ce3+荧光粉,超声分散后,加入磁力搅拌子,并置于磁力搅拌器上搅拌均匀,得到荧光粉悬浮液。
将荧光粉悬浮液加热至50℃,在搅拌速率为150r/min条件下持续搅拌,之后,用滴管将硝酸铝溶液以为30mL/min的滴定速度匀速滴入荧光粉悬浮液中。滴定完毕后持续保温和搅拌1h,并用氢氧化钠溶液将pH值调整到6.5,得到包覆有Al2O3水合物薄膜的YAG:Ce3+荧光粉。
使用包覆有Al2O3水合物薄膜的YAG:Ce3+荧光粉进行离心分离,水洗、脱水3次,并在80℃下烘干,之后在500℃条件下煅烧5h,得到Al2O3包覆的YAG:Ce3+荧光粉。
选用高纯度超细Al2O3粉末(粒径为0.1~1μm)与高纯度Al2O3粉末(粒径为1~10μm),按摩尔比100:1配置成混合Al2O3粉末。
配制1wt%的PEG4000-乙醇溶液,继而将混合Al2O3粉末加入其中,超声分散后,置于聚四氟乙烯球磨罐中,并加入适量的高纯氧化锆球,球磨12h。之后,将占总粉末重量50%的Al2O3包覆的YAG:Ce3+荧光粉加入该球磨罐中,继续球磨40min。
将球磨后的浆料进行真空干燥,粉碎,过筛后,得到混合粉末。
称取适量的混合粉末,装入石墨模具中,在10MPa压强下进行预压制。之后将石墨模具放入热压烧结炉内,在氩气气氛下,在烧结温度为1250℃,烧结压力为100MPa时,保温60min。
烧结完成后,卸除压力并随炉冷却,即可得到陶瓷复合材料YAG:Ce3+-Al2O3
实施例2:
称取适量的粒径为13μm~20μm的YAG:Ce3+荧光粉。
按照Al2O3与YAG:Ce3+荧光粉质量比1:1000的比例,称取相应量的Al(NO3)3·9H2O配制成0.5mol/L的硝酸铝溶液。
配制pH值为5.0、浓度为1.0mol/L的柠檬酸-氢氧化钠溶液,继而加入3wt%的PEG4000,并进行超声溶解。之后,加入YAG:Ce3+荧光粉,超声分散后,加入磁力搅拌子,并置于磁力搅拌器上搅拌均匀,得到荧光粉悬浮液。
将荧光粉悬浮液加热至65℃,在搅拌速率为280r/min条件下持续搅拌,之后,用滴管将硝酸铝溶液以为45mL/min的滴定速度匀速滴入荧光粉悬浮液中。滴定完毕后持续保温和搅拌1h,并用氢氧化钠溶液将pH值调整到7.0,得到包覆有Al2O3水合物薄膜的YAG:Ce3+荧光粉。
使用包覆有Al2O3水合物薄膜的YAG:Ce3+荧光粉进行离心分离,水洗、脱水5次,并在85℃下烘干,之后在320℃条件下煅烧5h,得到Al2O3包覆的YAG:Ce3+荧光粉。
选用高纯度超细Al2O3粉末(粒径为0.01~0.1μm)、高纯度超细Al2O3粉末(粒径为0.1~1μm)、及高纯度Al2O3粉末(粒径为1~10μm),按摩尔比1:100:3配置成混合Al2O3粉末。
配制2wt%的PEG4000-乙醇溶液,继而将混合Al2O3粉末加入其中,超声分散后,置于聚四氟乙烯球磨罐中,并加入适量的高纯氧化锆球,球磨24h。之后,将占总粉末重量70%的Al2O3包覆的YAG:Ce3+荧光粉加入该球磨罐中,继续球磨60min。
将球磨后的浆料进行真空干燥,粉碎,过筛后,得到混合粉末。
称取适量的混合粉末,装入石墨模具中,在15MPa压强下进行预压制。之后将石墨模具放入热压烧结炉内,在氩气气氛下,在烧结温度为1500℃,烧结压力为60MPa时,保温300min。
烧结完成后,卸除压力并随炉冷却,即可得到陶瓷复合材料YAG:Ce3+-Al2O3
实施例3:
称取适量的粒径为13μm~20μm的LuAG:Ce3+荧光粉。
按照Al2O3与LuAG:Ce3+荧光粉质量比1:500的比例,称取相应量的Al(NO3)3·9H2O配制成0.3mol/L的硝酸铝溶液。
配制pH值为5.0、浓度为1.0mol/L的柠檬酸-氢氧化钠溶液,继而加入1wt%的PEG4000,并进行超声溶解。之后,加入LuAG:Ce3+荧光粉,超声分散后,加入磁力搅拌子,并置于磁力搅拌器上搅拌均匀,得到荧光粉悬浮液。
将荧光粉悬浮液加热至40℃,在搅拌速率为110r/min条件下持续搅拌,之后,用滴管将硝酸铝溶液以为15mL/min的滴定速度匀速滴入荧光粉悬浮液中。滴定完毕后持续保温和搅拌1h,并用氢氧化钠溶液将pH值调整到7.0,得到包覆有Al2O3水合物薄膜的LuAG:Ce3+荧光粉。
使用包覆有Al2O3水合物薄膜的LuAG:Ce3+荧光粉进行离心分离,水洗、脱水4次,并在80℃下烘干,之后在300℃条件下煅烧5h,得到Al2O3包覆的LuAG:Ce3+荧光粉。
选用高纯度超细Al2O3粉末(粒径为0.1~1μm)与高纯度Al2O3粉末(粒径为1~10μm),按摩尔比20:1配置成混合Al2O3粉末。
配制3wt%的PEG4000-乙醇溶液,继而将混合Al2O3粉末加入其中,超声分散后,置于聚四氟乙烯球磨罐中,并加入适量的高纯氧化锆球,球磨8h。之后,将占总粉末重量45%的Al2O3包覆的LuAG:Ce3+荧光粉加入该球磨罐中,继续球磨30min。
将球磨后的浆料进行真空干燥,粉碎,过筛后,得到混合粉末。
称取适量的混合粉末,装入石墨模具中,在5MPa压强下进行预压制。之后将石墨模具放入热压烧结炉内,在氩气气氛下,在烧结温度为1300℃,烧结压力为50MPa时,保温180min。
烧结完成后,卸除压力并随炉冷却,即可得到陶瓷复合材料LuAG:Ce3+-Al2O3
需要说明的是,利用实施例1-3所述的制备方法进行陶瓷复合材料的制备,氧化铝颗粒的三元体系有助于陶瓷复合材料的烧结过程,其中,小颗粒氧化铝可起到助溶剂的作用,而大颗粒氧化铝不仅可起到提高粉末装填时的填充效率之作用,在烧结时还能够改善液相烧结和防止晶粒的异常长大。并且,大颗粒氧化铝对光还具有散射作用,通过调整大颗粒氧化铝的含量可以改变 陶瓷复合材料对于激发蓝光的透射性能和反射性能,可以调整陶瓷复合材料的色温。此外,三元体系在进行烧结时,还有利于提高荧光粉颗粒和氧化铝基质之间结合程度,改善陶瓷复合材料的机械性能。
因此,利用实施例1-3所述的制备方法进行陶瓷复合材料的制备,可制得高光效、高热导率、高机械性能、蓝光透过率可调的陶瓷复合材料,可应用于高性能激光光源,特别是小型化的激光光源系统。
本发明还提出一种陶瓷复合材料,该陶瓷复合材料包括氧化铝基质、均匀分布于所述氧化铝基质的荧光粉、及均匀分布于所述氧化铝基质的散射中心,其中氧化铝基质为连续的陶瓷,所述散射中心为氧化铝颗粒,且所述氧化铝颗粒的粒径范围是1μm~10μm,荧光粉的粒径范围是13μm~20μm。
该陶瓷复合材料耐高温、导热性能好,而且机械性能优异。
本发明还提出一种波长转换器,该波长转换器包括如前所述的陶瓷复合材料。由于本波长转换器采用了前述所有实施例的全部技术方案,因此至少具有前述实施例的技术方案所带来的所有有益效果,在此不再一一赘述。该波长转换器可以应用于固定安装的环境,也可以应用于运动装置中(例如波长转换色轮)。该波长转换器可以应用到照明领域,如各种灯具——路灯、探照灯、舞台灯、汽车大灯;该波长转换器也可以应用到显示系统上,如投影机、电视机等,均能满足其使用需求。
以上所述仅为本发明的优选实施例,并非因此限制本发明的专利范围,凡是在本发明的发明构思下,利用本发明说明书内容所作的等效结构变换,或直接/间接运用在其他相关的技术领域均包括在本发明的专利保护范围内。

Claims (12)

  1. 一种陶瓷复合材料的制备方法,其特征在于,包括以下步骤:
    按Al2O3与荧光粉质量比(0.1~1):100,分别配置铝盐溶液与荧光粉;
    将所述荧光粉分散于pH值为4.5~5.5的缓冲溶液,得到悬浮液;
    用所述铝盐溶液对所述悬浮液进行滴定,得到包覆有Al2O3水合物薄膜的荧光粉;
    将所述包覆有Al2O3水合物薄膜的荧光粉进行煅烧,得到Al2O3包覆的荧光粉;
    将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好,得到混合氧化铝粉末;
    将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合,得到混合粉末,其中,所述Al2O3包覆的荧光粉占所述混合粉末重量的40%~90%;
    对所述混合粉末进行预压制、烧结,得到所述陶瓷复合材料。
  2. 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,所述荧光粉包含Ca3Al2Si3O12、Ca3Sc2Si3O12、Gd3Al5O12、Gd3Ga5O12、Tb3Al5O12、Tb3Ga5O12、Y3Al5O12、Y3Ga5O12、Lu3Al5O12、Lu3Ga5O12及Y3Mg2AlSi2O12的掺杂有Ce3+的荧光粉中的至少一种。
  3. 如权利要求2所述的陶瓷复合材料的制备方法,其特征在于,所述荧光粉的粒径范围是13μm~20μm。
  4. 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,所述铝盐溶液的浓度为0.01mol/L~1mol/L。
  5. 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,在所述用所述铝盐溶液对所述悬浮液进行滴定的步骤中,所述悬浮液的温度为40℃~70℃,搅拌速率为100r/min~300r/min,滴定速度为5mL/min~50mL/min。
  6. 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,所述煅烧过程中,煅烧温度为300℃~600℃,煅烧时间为2h~5h。
  7. 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,所述预压制过程在5MPa~15MPa压强下进行。
  8. 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,所述烧结过程在氩气气氛下进行,烧结温度为1250℃~1550℃,烧结压力为30MPa~200MPa,保温时间为30min~360min。
  9. 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,在所述将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好的步骤中,还加入粒径为0.01μm~0.1μm的氧化铝粉末,所述0.01μm~0.1μm的氧化铝粉末与所述0.1μm~1μm的氧化铝粉末的摩尔比为(0.1~1):100。
  10. 如权利要求1-9任一项所述的陶瓷复合材料的制备方法,其特征在于,所述将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合的步骤包括:
    将所述混合氧化铝粉末分散于质量百分浓度为1wt%~3wt%的PEG4000-乙醇溶液中,并置于球磨罐中,球磨6h~24h;
    将所述Al2O3包覆的荧光粉加入所述球磨罐中,继续球磨30min~60min。
  11. 一种陶瓷复合材料,其特征在于,包括氧化铝基质、均匀分布于所述氧化铝基质的荧光粉、及均匀分布于所述氧化铝基质的散射中心,所述氧化铝基质为氧化铝陶瓷,所述散射中心为氧化铝颗粒,且所述氧化铝颗粒的粒径范围是1μm~10μm,所述荧光粉的粒径范围是13μm~20μm。
  12. 一种波长转换器,其特征在于,包括如权利要求11所述的陶瓷复合材料。
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