WO2021037226A1 - 荧光陶瓷及其制备方法、光源装置 - Google Patents

荧光陶瓷及其制备方法、光源装置 Download PDF

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WO2021037226A1
WO2021037226A1 PCT/CN2020/112198 CN2020112198W WO2021037226A1 WO 2021037226 A1 WO2021037226 A1 WO 2021037226A1 CN 2020112198 W CN2020112198 W CN 2020112198W WO 2021037226 A1 WO2021037226 A1 WO 2021037226A1
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powder
ceramic
fluorescent
sintering
ceramic matrix
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PCT/CN2020/112198
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English (en)
French (fr)
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李乾
简帅
王艳刚
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深圳市中光工业技术研究院
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Priority to EP20857295.8A priority Critical patent/EP3995471A4/en
Priority to JP2022506668A priority patent/JP7450701B2/ja
Publication of WO2021037226A1 publication Critical patent/WO2021037226A1/zh

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    • F21V9/00—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters
    • F21V9/30—Elements containing photoluminescent material distinct from or spaced from the light source

Definitions

  • the invention relates to the technical field of laser illumination and display, in particular to a fluorescent ceramic, a preparation method thereof, and a light source device.
  • Laser illumination display technology mainly uses blue laser to excite fluorescent materials to obtain fluorescence in other wavelength bands.
  • the requirements for the performance of fluorescent materials have also been continuously improved.
  • the current fluorescent materials have poor light conversion efficiency, luminous brightness, and thermal conductivity, and are difficult to carry blue lasers with higher power density.
  • the main technical problem to be solved by the present invention is to provide a fluorescent ceramic, a preparation method thereof, and a light source device, which can improve the luminous efficiency of the fluorescent ceramic.
  • a technical solution adopted by the present invention is to provide a fluorescent ceramic, which includes a ceramic matrix and a fluorescent powder dispersed in the ceramic matrix, wherein pores are formed in the crystal grains of the ceramic matrix.
  • a plurality of uniformly distributed pores are formed inside the crystal grains of the ceramic substrate.
  • the pore diameter is 0.1 ⁇ m-2 ⁇ m.
  • the particle size of the phosphor powder is 5 ⁇ m-30 ⁇ m.
  • the grain size of the ceramic substrate is 5 ⁇ m to 20 ⁇ m.
  • the preparation method includes: providing ceramic matrix raw material powder; sintering the ceramic matrix raw material powder to obtain the inside of the crystal grains. Forming a first powder with pores; mixing and sintering the first powder and the phosphor powder, and then retaining the pores in the crystal grains of the ceramic matrix.
  • the step of sintering the ceramic matrix raw material powder to obtain the first powder with pores formed inside the crystal grains includes: taking part of the ceramic matrix raw material powder for sintering to obtain the first powder The blank; wherein the remaining ceramic matrix raw material powder is the second powder; the first powder blank is crushed and ground to obtain the first powder with pores formed inside the crystal grains.
  • the step of taking part of the ceramic matrix raw material powder for sintering to obtain the first powder body includes: placing part of the ceramic matrix raw material powder at a temperature of 1600°C to 1800°C Sintering in an atmosphere of 2h-6h to obtain the first powder body.
  • the particle size of the first powder is larger than the particle size of the second powder.
  • the step of mixing and sintering the first powder body and the phosphor powder body includes: mixing and sintering the first powder body, the second powder body, the phosphor powder body and the sintering aid; wherein, the sintering aid It is at least one of magnesium oxide, yttrium oxide, lanthanum oxide, and titanium oxide.
  • the sintering aid includes at least titanium oxide.
  • the step of mixing and sintering the first powder, the second powder, the phosphor powder and the sintering aid includes: mixing the first powder, the second powder, the phosphor and the sintering aid
  • the first mixed powder body is mixed by ball milling to obtain the first mixed powder body; the first mixed powder body is placed in a vacuum or protective gas atmosphere for heat preservation and sintering to obtain the second mixed powder body; wherein the sintering temperature is 1300°C ⁇ 1600°C, the sintering pressure is 20MPa ⁇ 180MPa, and the sintering time is 0.5h ⁇ 4h;
  • the second mixed powder body is annealed in air atmosphere to obtain fluorescent ceramics; wherein, the annealing temperature is 1200°C ⁇ 1400°C, duration is 5h ⁇ 20h.
  • the phosphor accounts for 30% to 70% of the total mass of the first mixed powder body
  • the sintering aid accounts for 0.1% to 1% of the total mass of the first mixed powder body
  • the first The mass ratio of the powder to the second powder is 4:6 to 7:3.
  • another technical solution adopted by the present invention is to provide a light source device, which includes the fluorescent ceramic as described in the above embodiments.
  • the present invention provides a fluorescent ceramic, the ceramic matrix of the fluorescent ceramic has pores formed inside the crystal grains, when the fluorescent ceramic is irradiated by laser (such as blue laser), the incident The laser passing through the pores inside the crystal grains of the ceramic matrix will cause scattering, and the scattered laser can then excite more phosphors in the vicinity to emit light, thereby improving the luminous efficiency of the fluorescent ceramics.
  • laser such as blue laser
  • FIG. 1 is a schematic diagram of the structure of an embodiment of the fluorescent ceramic of the present invention.
  • FIG. 2 is a schematic diagram of the microstructure of an embodiment of the fluorescent ceramic of the present invention.
  • Fig. 3 is a schematic flow chart of an embodiment of a method for preparing fluorescent ceramics of the present invention
  • FIG. 4 is a schematic flow chart of another embodiment of the method for preparing fluorescent ceramics of the present invention.
  • FIG. 5 is a schematic structural view of an embodiment of the sintering process of the fluorescent ceramic of the present invention.
  • Fig. 6 is a schematic structural diagram of an embodiment of a light source device of the present invention.
  • Fluorescent materials used in laser lighting and display technology can be roughly divided into three categories.
  • the phosphor is encapsulated by organic polymers such as organic silica gel/organic resin.
  • organic polymers such as organic silica gel/organic resin.
  • the heat generated by the phosphor encapsulated by the organic matrix increases sharply during light conversion, causing its own temperature to rise sharply, which in turn leads to the aging of the encapsulated organic matrix such as silica gel/organic resin Yellowing, which in turn causes problems such as loss of light efficiency and reduced life span;
  • Fluorescent glass materials which mainly encapsulate phosphors in SiO2-based/borosilicate-based glass.
  • fluorescent glass Compared with organic resins, fluorescent glass has great improvements in heat resistance, high thermal stability, low color shift, etc., but its thermal conductivity is not significantly improved compared with organic resins; third, fluorescent ceramics. Compared with fluorescent materials encapsulated by organic matrix and inorganic glass matrix, fluorescent ceramics have significant advantages in terms of heat resistance and thermal conductivity. Fluorescent ceramics have become an important development direction of laser illumination display technology due to its excellent performance.
  • fluorescent ceramics There are two types of fluorescent ceramics. One is prepared by doping rare earth elements into transparent ceramics such as YAG (Y 3 Al 5 O 12 , yttrium aluminum garnet), which is a pure phase ceramic. The other is to encapsulate the phosphors in transparent ceramics with high thermal conductivity to form multi-phase PIA ceramics.
  • YAG Y 3 Al 5 O 12 , yttrium aluminum garnet
  • fluorescent ceramics For fluorescent ceramics, how to improve its luminous efficiency is crucial. Pure-phase ceramics in fluorescent ceramics (such as the first fluorescent ceramics mentioned above) are difficult to have a high utilization rate of excitation light due to their own structure; when they are excited, their luminous centers are relatively small, resulting in poor luminous efficiency . In contrast, fluorescent ceramics formed by encapsulating fluorescent powder in transparent ceramics can have a good utilization rate of excitation light. Therefore, the fluorescent ceramics of the multiphase structure have more advantages.
  • an embodiment of the present invention provides a fluorescent ceramic, which can improve the luminous efficiency of the fluorescent ceramic.
  • the fluorescent ceramic includes a ceramic matrix and a fluorescent powder dispersed in the ceramic matrix, wherein pores are formed in the crystal grains of the ceramic matrix. This will be explained in detail below.
  • FIG. 1 is a schematic structural diagram of an embodiment of the fluorescent ceramic of the present invention.
  • the fluorescent ceramic includes a ceramic base 11 and fluorescent powder 12 dispersed in the ceramic base 11. It can be seen that the fluorescent powder body 12 is encapsulated in the ceramic substrate 11, and the fluorescent ceramic has a multi-phase structure, which has a high excitation light utilization rate, which is beneficial to improve the luminous efficiency of the fluorescent ceramic.
  • the material of the ceramic base 11 may be alumina or the like, the phosphor 12 is encapsulated in the ceramic base 11, and the ceramic base 11 is transparent, which does not hinder the phosphor 12 from emitting light.
  • the microstructure of the fluorescent ceramic based on alumina ceramic is shown in FIG. 2, and the fluorescent powder 21 is uniformly distributed in the continuous medium alumina phase 22 (ie, the ceramic matrix). Since alumina belongs to the trigonal crystal system, it has birefringence. The laser is scattered in the fluorescent ceramic due to birefringence, and the scattered laser in the fluorescent ceramic can then excite more phosphors in the vicinity, which shows higher luminous efficiency. This is also the reason why the luminous efficiency of multiphase ceramics (such as PIA ceramics) is better than that of pure phase ceramics (such as YAG ceramics), which is especially significant when the thickness of fluorescent ceramics is thinner.
  • multiphase ceramics such as PIA ceramics
  • pure phase ceramics such as YAG ceramics
  • pores 13 are formed inside the crystal grains of the ceramic substrate 11.
  • the powder 12 emits light, thereby improving the luminous efficiency of the fluorescent ceramic.
  • the pores 13 inside the crystal grains of the fluorescent ceramic described in this embodiment are not located at the boundary of the crystal grains, but are located in the region near the middle of the crystal grains.
  • the pore 13 is located at the boundary of the crystal grains, which easily causes intergranular fracture of the ceramic and greatly reduces the strength of the ceramic.
  • the pores 13 are located in the region near the middle of the crystal grains, which can effectively prevent the ceramic strength from being reduced.
  • the grain size of the ceramic substrate 11 is preferably 5 ⁇ m to 20 ⁇ m, for example, 10 ⁇ m or the like.
  • a plurality of uniformly distributed pores 13 are formed inside the crystal grains of the ceramic base 11.
  • the pores 13 inside the crystal grains of the ceramic substrate 11 are uniformly distributed, so that the incident laser light can reach the pores 13 and be scattered, thereby further increasing the scattering of the incident laser light, and thereby improving the luminous efficiency of the fluorescent ceramic.
  • the pore size of the pores 13 is preferably 0.1 ⁇ m to 2 ⁇ m, for example, 1 ⁇ m or the like.
  • the phosphor body 12 may be Ce:YAG yellow phosphor or Ce:LuAG green phosphor, etc., and its particle size is preferably 5 ⁇ m-30 ⁇ m, such as 15 ⁇ m.
  • the fluorescent powder in the fluorescent ceramic provided by the present invention is excited by laser light (for example, blue laser light) to emit light.
  • laser light for example, blue laser light
  • pores are formed inside the crystal grains of the ceramic matrix.
  • FIG. 3 is a schematic flowchart of an embodiment of a method for preparing a fluorescent ceramic of the present invention. It should be noted that the preparation method of the fluorescent ceramic described in this embodiment is not limited to the following steps:
  • a ceramic matrix raw material powder is provided for preparing fluorescent ceramics.
  • the ceramic matrix raw material powder is used to form the ceramic matrix of fluorescent ceramics.
  • the ceramic matrix raw material powder is sintered to obtain the first powder, and the first powder is used in the subsequent preparation process of the fluorescent ceramic to form the ceramic matrix of the fluorescent ceramic.
  • pores are formed inside the crystal grains of the first powder body, which are used to increase the scattering of incident laser light, so as to improve the luminous efficiency of the fluorescent ceramic.
  • the first powder and phosphor powder obtained in the above steps are mixed and sintered, that is, a secondary sintering is performed to obtain a ceramic matrix and a fluorescent powder dispersed in the ceramic matrix.
  • the phosphor is excited by the laser and emits light, realizing the luminous function of the fluorescent ceramic.
  • the pores obtained by the primary sintering will remain inside the crystal grains of the ceramic matrix, and then a fluorescent ceramic with pores in the crystal grains is obtained.
  • FIG. 4 is a schematic flowchart of another embodiment of the method for preparing fluorescent ceramics of the present invention. It should be noted that the preparation method of the fluorescent ceramic described in this embodiment is not limited to the following steps:
  • a ceramic matrix raw material powder having a second particle size is provided, and the ceramic matrix raw material powder is pretreated to obtain a first powder having a first particle size.
  • the ceramic matrix raw material powder may include: taking part of the ceramic matrix raw material powder for sintering to obtain a first powder body, and the remaining ceramic matrix raw material powder is the second powder.
  • the first powder body is crushed and ground to obtain the first powder body with pores formed in the crystal grains.
  • the ceramic matrix raw material powder, the first powder and the second powder are of the same material.
  • the part of the ceramic matrix raw material powder taken is placed in the crucible (the material of the crucible is the same as the ceramic matrix raw material powder and the first powder, which can avoid the chemical reaction between the ceramic matrix raw material powder, the first powder and the crucible , It is beneficial to maintain the stable composition of the ceramic matrix raw material powder and the first powder), tapping and compacting treatment; then sintering in the muffle furnace for 2h-6h, the sintering temperature is 1600°C ⁇ 1800°C; after the sintering is finished After cooling, the sintered mass in the first powder body is crushed and pulverized by ball milling to the first particle size to obtain the first powder, which is bottled for use, and the pretreatment of the ceramic matrix raw material powder is completed .
  • the first powder, the second powder, the phosphor powder and the sintering aid obtained by the pretreatment are ball-milled and mixed (ball-milling belongs to the understanding of those skilled in the art and will not be repeated here),
  • the mass ratio of the first powder to the second powder is 4:6 to 7:3
  • the phosphor accounts for 30% to 70% of the total mass of the first mixed powder body
  • the sintering aid accounts for the first 0.1% to 1% of the total mass of the mixed powder body.
  • the inventor has concluded through a large amount of experimental data that when the first powder, second powder, phosphor and sintering aid are added in the above-mentioned amounts, the prepared fluorescent ceramics can perform well in all aspects. performance.
  • the particle size of the first powder is larger than the particle size of the second powder, that is, the first particle size is larger than the second particle size.
  • the second powder with a smaller grain size is mixed and sintered with the first powder with a larger grain size.
  • the second powder can better fuse with the first powder during the secondary sintering process, and the second powder
  • the crystal grains of a powder are connected to form a continuous phase, so that the ceramic matrix of the finally produced fluorescent ceramic is a continuous phase, so that the fluorescent ceramic has good thermal conductivity, is conducive to heat dissipation, and has good structural strength.
  • the first particle size may be 5 ⁇ m to 10 ⁇ m
  • the second particle size may be 0.05 ⁇ m to 0.5 ⁇ m.
  • the sintering aid may be at least one of magnesium oxide, yttrium oxide, lanthanum oxide, and titanium oxide.
  • the sintering aid is preferably titanium oxide, and the addition of titanium oxide as the sintering aid will facilitate the formation of intracrystalline pores in the ceramic matrix.
  • the formation of intracrystalline pores is mainly due to the fact that a large number of crystal lattice defects appear on ceramic substrates (such as alumina-based ceramic substrates) based on variable valence titanium ions, and also form a solid solution with the ceramic substrate to promote grain boundary migration to form intracrystalline pores.
  • the pores change from interface diffusion to bulk diffusion. The diffusion process requires higher energy and is difficult to discharge, and it is easier to form intracrystalline pores.
  • the first mixed powder body obtained by mixing is filled into a graphite grinding tool, and the first mixed powder body is pre-compressed under a relatively small pressure, and then the first mixed powder body is filled with
  • the graphite abrasive tool is placed in an SPS hot-pressing furnace, and is heat-retained and sintered in a vacuum or protective gas atmosphere to obtain a second mixed powder body.
  • the inventors summarized through a large amount of experimental data, when the sintering temperature is 1300°C ⁇ 1600°C, the pressure during sintering is 20MPa ⁇ 180MPa, and the sintering time is 0.5h ⁇ 4h, it can maximize the benefit of the first mixed powder body.
  • the sintering combination of various powders in the powder to produce fluorescent ceramics that meet the requirements.
  • the protective gas may be inert gas such as helium, neon, argon, or other chemically inactive gases, which are not limited here.
  • the ceramic matrix raw material powder particles in contact with each other gradually change from point contact to surface contact during the sintering process to form a sintering neck.
  • the agglomerates of the first powder body are crushed, and then sintered together with the untreated second powder body, the phosphor powder body and a small amount of sintering aid.
  • the sintering aid is located on the surface of the large-particle first powder, the untreated second powder and the phosphor powder formed by the pretreatment.
  • the sintering aid will accelerate the sintering between the first powder and the second powder, and the pretreated large-particle first powder 31 is easy to form pores 32, and the pores 32 will remain because it is difficult to eliminate Inside the crystal grains, a fluorescent ceramic with pores in the crystal grains is obtained, as shown in Figure 5.
  • the second powder of small particles can be filled between the crystal grains of the first powder, so that the ceramic matrix formed by the first powder and the second powder is a continuous phase, ensuring that it has good thermal conductivity.
  • the second mixed powder body needs to be annealed to obtain fluorescent ceramics.
  • the second mixed powder body is placed in an air atmosphere for annealing treatment.
  • the temperature of the annealing treatment is 1200°C ⁇ 1400°C, and the duration is 5h ⁇ 20h.
  • the fluorescent ceramic needs to be post-processed so that the fluorescent ceramic meets the requirements of the product size and surface properties.
  • the post-processing performed on the fluorescent ceramic includes at least one of cutting processing, grinding processing, polishing processing, and the like.
  • the cutting process is to cut the rough blank of the fluorescent ceramic into the fluorescent ceramic of the size and shape required by the product; and the grinding treatment and polishing treatment are to make the surface flatness, smoothness and other surface properties of the fluorescent ceramic meet the product requirements.
  • the pretreated alumina powder (i.e. the first powder) and the untreated alumina powder (i.e. the second powder) are mixed with a small amount of absolute ethanol at a mass ratio of 6:4.
  • Alumina balls are selected. (Similar to the choice of alumina crucible) for ball milling and mixing, the ball milling time is 24h.
  • magnesium oxide is added as a sintering aid, which accounts for 0.5% of the total mass of the powder.
  • a certain amount of YAG:Ce phosphor is weighed, which accounts for 50% of the total powder, and after ball milling and mixing for 1 hour, the slurry is dried at 70° C., followed by grinding and sieving.
  • the mixed fluorescent ceramic powder into a graphite mold, pre-press the powder under low pressure, and then place the graphite mold in an SPS hot-pressing furnace.
  • an SPS hot-pressing furnace In a vacuum atmosphere, heat preservation and sintering at 1500°C for 1 hour, The pressure during sintering is 50MPa.
  • the fluorescent ceramics are annealed at 1200°C for 15 hours in an air atmosphere. Finally, the fluorescent ceramics are cut, ground and polished to obtain intracrystalline porous fluorescent ceramics.
  • the pretreated alumina powder (i.e. the first powder) and the untreated alumina powder (i.e. the second powder) are mixed with a small amount of absolute ethanol at a mass ratio of 1:1.
  • Alumina balls are selected.
  • the ball milling and mixing are carried out, and the ball milling time is 16h.
  • magnesium oxide and yttrium oxide are added as sintering aids, which respectively account for 04% and 0.5% of the total mass of the powder.
  • a certain amount of YAG:Ce phosphor is weighed, which accounts for 40% of the total powder, and after ball milling and mixing for 1 hour, the slurry is dried at 70° C., followed by grinding and sieving.
  • the mixed fluorescent ceramic powder into a graphite mold, pre-press the powder under low pressure, and then place the graphite mold in an SPS hot-pressing furnace.
  • heat preservation and sintering at 1550°C for 0.5h , The pressure during sintering is 60MPa.
  • the fluorescent ceramics are annealed at 1300°C for 8 hours in an air atmosphere. Finally, the fluorescent ceramics are cut, ground and polished to obtain intracrystalline porous fluorescent ceramics.
  • the third embodiment (the preprocessing step is omitted in this embodiment):
  • the ceramic green body is placed in a hot-pressing sintering furnace, and sintered at 1550°C for 1 hour under an argon atmosphere at a pressure of 40 MPa. After hot pressing and sintering, the fluorescent ceramics are annealed at 1350°C for 10 hours in an air atmosphere; finally, the ceramics are coarsely ground, finely ground and polished to obtain intracrystalline porous fluorescent ceramics.
  • the method for preparing fluorescent ceramics provides a first powder and a second powder with different particle sizes but the same material, and the two are mixed and sintered with the phosphor to make the phosphor
  • the body is dispersed in the ceramic matrix formed by the first powder and the second powder, and pores are formed in the crystal grains of the ceramic matrix.
  • the blue incident laser will scatter through the pores inside the crystal grains of the ceramic matrix. The scattered blue laser can then excite more fluorescent powder nearby to emit light, thereby improving the fluorescent ceramic The luminous efficiency.
  • FIG. 6 is a schematic structural diagram of an embodiment of a light source device of the present invention.
  • the light source device 4 includes a fluorescent ceramic 41.
  • the fluorescent ceramic 41 may be the fluorescent ceramic described in the above-mentioned embodiment, which will not be repeated here.
  • the specific application form of the light source device 4 may be a fixed light source, a micro-projection light source, a television, and other projection equipment, etc., which are not limited herein.

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Abstract

涉及激光照明显示技术领域，公开了一种荧光陶瓷及其制备方法、光源装置。该荧光陶瓷包括陶瓷基体（11）以及散布于陶瓷基体（11）内的荧光粉体（12），其中陶瓷基体（11）的晶粒内部形成有气孔（13）。通过上述方式，能够提高荧光陶瓷的发光效率。

Description

荧光陶瓷及其制备方法、光源装置 技术领域
本发明涉及激光照明显示技术领域，特别是涉及一种荧光陶瓷及其制备方法、光源装置。
背景技术
激光照明显示技术主要通过蓝色激光激发荧光材料来获取其他波段的荧光。随着激光照明和显示技术的不断发展，对荧光材料各个性能上的要求也不断提高。而目前荧光材料的光转换效率、发光亮度以及导热性较差，并且难以承载更高功率密度的蓝色激光等。
发明内容
有鉴于此，本发明主要解决的技术问题是提供一种荧光陶瓷及其制备方法、光源装置，能够提高荧光陶瓷的发光效率。
为解决上述技术问题，本发明采用的一个技术方案是：提供一种荧光陶瓷，该荧光陶瓷包括陶瓷基体以及散布于陶瓷基体内的荧光粉体，其中陶瓷基体的晶粒内部形成有气孔。
在本发明的一实施例中，陶瓷基体的晶粒内部形成有多个均匀分布的气孔。
在本发明的一实施例中，气孔的孔径为0.1μm～2μm。
在本发明的一实施例中，荧光粉体的粒径为5μm～30μm。
在本发明的一实施例中，陶瓷基体的晶粒粒径为5μm～20μm。
为解决上述技术问题，本发明采用的又一个技术方案是：提供一种荧光陶瓷的制备方法，该制备方法包括：提供陶瓷基质原料粉体；将陶 瓷基质原料粉体进行烧结，得到晶粒内部形成有气孔的第一粉体；将第一粉体和荧光粉体混合烧结，进而将气孔保留在陶瓷基体的晶粒内部。
在本发明的一实施例中，将陶瓷基质原料粉体进行烧结，得到晶粒内部形成有气孔的第一粉体的步骤包括：取部分的陶瓷基质原料粉体进行烧结，得到第一粉体坯；其中，剩余的陶瓷基质原料粉体为第二粉体；将第一粉体坯进行破碎、研磨，得到晶粒内部形成有气孔的第一粉体。
在本发明的一实施例中，取部分的陶瓷基质原料粉体进行烧结，得到第一粉体坯的步骤包括：将所取的部分陶瓷基质原料粉体置于一温度为1600℃～1800℃的氛围中烧结2h～6h，得到第一粉体坯。
在本发明的一实施例中，第一粉体的粒径大于第二粉体的粒径。
在本发明的一实施例中，将第一粉体和荧光粉体混合烧结的步骤包括：将第一粉体、第二粉体、荧光粉体以及烧结助剂混合烧结；其中，烧结助剂为氧化镁、氧化钇、氧化镧、氧化钛中的至少一种。
在本发明的一实施例中，烧结助剂至少包括氧化钛。
在本发明的一实施例中，将第一粉体、第二粉体、荧光粉体以及烧结助剂混合烧结的步骤包括：将第一粉体、第二粉体、荧光粉体以及烧结助剂进行球磨混合，以得到第一混合粉体坯；将第一混合粉体坯置于真空或保护气体氛围中进行保温烧结，以得到第二混合粉体坯；其中，烧结温度为1300℃～1600℃，烧结时的压力为20MPa～180MPa，烧结时长为0.5h～4h；将第二混合粉体坯置于空气氛围中进行退火处理，以得到荧光陶瓷；其中，退火处理的温度为1200℃～1400℃、时长为5h～20h。
在本发明的一实施例中，荧光粉体占第一混合粉体坯总质量的30％～70％，烧结助剂占第一混合粉体坯总质量的0.1％～1％，且第一粉体与第二粉体的质量比为4:6至7:3。
为解决上述技术问题，本发明采用的又一个技术方案是：提供一种光源装置，该光源装置包括如上述实施例所阐述的荧光陶瓷。
本发明的有益效果是：区别于现有技术，本发明提供一种荧光陶瓷，该荧光陶瓷的陶瓷基体的晶粒内部形成有气孔，当荧光陶瓷受激光(例如蓝色激光)照射时，入射激光经过陶瓷基体的晶粒内部的气孔会产生 散射，被散射的激光进而可以激发其附近更多的荧光粉体发光，从而提高荧光陶瓷的发光效率。
附图说明
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。其中：
图1是本发明荧光陶瓷一实施例的结构示意图；
图2是本发明荧光陶瓷一实施例的显微结构示意图；
图3是本发明荧光陶瓷的制备方法一实施例的流程示意图；
图4是本发明荧光陶瓷的制备方法另一实施例的流程示意图；
图5是本发明荧光陶瓷的烧结过程一实施例的结构示意图；
图6是本发明光源装置一实施例的结构示意图。
具体实施方式
为使本发明的上述目的、特征和优点能够更为明显易懂，下面结合附图，对本发明的具体实施方式做详细的说明。可以理解的是，此处所描述的具体实施例仅用于解释本发明，而非对本发明的限定。另外还需要说明的是，为了便于描述，附图中仅示出了与本发明相关的部分而非全部结构。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
本发明中的术语“第一”、“第二”等是用于区别不同对象，而不是用于描述特定顺序。此外，术语“包括”和“具有”以及它们任何变形，意图在于覆盖不排他的包含。例如包含了一系列步骤或单元的过程、方法、系统、产品或设备没有限定于已列出的步骤或单元，而是可选地还包括没有列出的步骤或单元，或可选地还包括对于这些过程、方法、产品或设备固有的其它步骤或单元。
在本文中提及“实施例”意味着，结合实施例描述的特定特征、结构或特性可以包含在本发明的至少一个实施例中。在说明书中的各个位置出现该短语并不一定均是指相同的实施例，也不是与其它实施例互斥的独立的或备选的实施例。本领域技术人员显式地和隐式地理解的是，本文所描述的实施例可以与其它实施例相结合。
用于激光照明和显示技术中的荧光材料大致可分为三类。一、通过有机硅胶/有机树脂等有机聚合物对荧光粉体进行封装。当随着蓝色激光功率的增加，有机基质所封装的荧光粉体在进行光转换时，所产生热量也急剧增加，致使其自身温度大幅上升，进而导致封装的硅胶/有机树脂等有机基质老化泛黄，进而引发光效损失、寿命减少等问题；二、荧光玻璃材料，其主要是将荧光粉体封装在SiO2基/硼硅酸盐基的玻璃中。荧光玻璃较有机树脂而言，在耐热性、高热稳定性、低色偏移等上有很大改善，但是其在导热性能上较有机树脂并无显著性的提高；三、荧光陶瓷。荧光陶瓷较有机基质和无机玻璃基质所封装的荧光材料，在无论是在耐热性能还是热导率上均有显著的优势。荧光陶瓷因其优异的性能而成为激光照明显示技术的一个重要发展方向。
荧光陶瓷分为两种，一种是通过在YAG(Y 3Al 5O 12，钇铝石榴石)等透明陶瓷中掺杂稀土元素制备而成，其为纯相陶瓷。另外一种是通过将荧光粉体封装在高导热系数的透明陶瓷中，形成复相的PIA陶瓷。
对于荧光陶瓷而言，如何提高其发光效率至关重要。荧光陶瓷中纯相陶瓷(例如上述第一种荧光陶瓷)由于自身结构原因，难以对激发光有较高的利用率；在其受激发时，其发光中心相对较少而导致其发光效率较差。相比而言，将荧光粉封装在透明陶瓷中所形成的荧光陶瓷，能对激发光有着很好的利用率。因此，复相结构的荧光陶瓷更具优势。
有鉴于此，本发明的一实施例提供一种荧光陶瓷，能够提高荧光陶瓷的发光效率。该荧光陶瓷包括陶瓷基体以及散布于陶瓷基体内的荧光粉体，其中陶瓷基体的晶粒内部形成有气孔。以下进行详细阐述。
请参阅图1，图1是本发明荧光陶瓷一实施例的结构示意图。
在一实施例中，荧光陶瓷包括陶瓷基体11以及散布于陶瓷基体11 内的荧光粉体12。可见，荧光粉体12封装于陶瓷基体11中，荧光陶瓷为复相结构，其具有较高的激发光利用率，有利于提高荧光陶瓷的发光效率。
举例而言，陶瓷基体11的材质可以是氧化铝等，荧光粉体12封装在陶瓷基体11中，陶瓷基体11呈透明状，不会阻碍荧光粉体12发光。基于氧化铝陶瓷的荧光陶瓷，其显微组织结构如图2所示，荧光粉体21均匀分布在连续介质氧化铝物相22(即陶瓷基体)中。由于氧化铝属于三方晶系，其存在双折射现象。激光在荧光陶瓷中会因双折射而发生散射，荧光陶瓷中被散射的激光进而可以激发其附近更多的荧光粉，其表现为发光效率更高。这也是复相陶瓷(例如PIA陶瓷)发光效率优于纯相陶瓷(例如YAG陶瓷)的原因所在，这点在荧光陶瓷厚度较薄时尤为显著。
本实施例在此基础上在陶瓷基体11的晶粒内部形成气孔13，激光到达气孔13时会进一步发生散射，从而进一步增加入射激光的散射，被散射的激光进而可以激发其附近更多的荧光粉体12发光，从而提高荧光陶瓷的发光效率。
需要说明的是，本实施例所阐述的荧光陶瓷其晶粒内部的气孔13并非位于晶粒交界处，而是位于晶粒靠近中部的区域。气孔13位于晶粒交界处，容易使陶瓷产生沿晶断裂，使陶瓷强度极大降低。而本实施例中气孔13位于晶粒靠近中部的区域，能够有效避免陶瓷强度降低。
可选地，陶瓷基体11的晶粒粒径优选为5μm～20μm，例如10μm等。发明人通过大量实验发现晶粒粒径为5μm～20μm的陶瓷基体11，有利于形成连续物相，保证荧光陶瓷具有良好的导热能力，同时使得荧光陶瓷的结构强度得到保证。
进一步地，陶瓷基体11的晶粒内部形成有多个均匀分布的气孔13。陶瓷基体11的晶粒内部的气孔13均匀分布，使得入射的激光更能够到达气孔13而发生散射，从而进一步增加入射激光的散射，进而提高荧光陶瓷的发光效率。
可选地，气孔13的孔径优选为0.1μm～2μm，例如1μm等。发明人 通过大量实验发现孔径为0.1μm～2μm的气孔13能够最大限度地增加入射激光的散射，同时使得荧光陶瓷各方面的性能能够得到保证。
进一步地，荧光粉体12可以为Ce:YAG黄色荧光粉或Ce:LuAG绿色荧光粉等，其粒径优选为5μm～30μm，例如15μm等。发明人通过大量实验发现粒径为5μm～30μm的荧光粉体12，其受激光激发而发光，能够使得荧光陶瓷具有良好的出光效果。
以上可以看出，本发明所提供的荧光陶瓷其内的荧光粉体受激光(例如蓝色激光)激发而发光。并且陶瓷基体的晶粒内部形成有气孔，当荧光陶瓷受激光照射时，入射激光经过陶瓷基体的晶粒内部的气孔会产生散射，被散射的激光进而可以激发其附近更多的荧光粉体发光，从而提高荧光陶瓷的发光效率。
以下对上述实施例所阐述的荧光陶瓷的制备方法进行阐述：
请参阅图3，图3是本发明荧光陶瓷的制备方法一实施例的流程示意图。需要说明的是，本实施例所阐述的荧光陶瓷的制备方法并不局限于以下步骤：
S101：提供陶瓷基质原料粉体；
在本实施例中，提供陶瓷基质原料粉体用于制备荧光陶瓷。其中，陶瓷基质原料粉体用于形成荧光陶瓷的陶瓷基体。
S102：将陶瓷基质原料粉体进行烧结，得到内部形成有气孔的第一粉体；
在本实施例中，将陶瓷基质原料粉体进行烧结，以得到第一粉体，第一粉体用于后续荧光陶瓷的制备工艺中用以形成荧光陶瓷的陶瓷基体。其中，第一粉体的晶粒内部形成有气孔，用于增加入射激光的散射，以提高荧光陶瓷的发光效率。
S103：将第一粉体和荧光粉体混合烧结，进而将气孔保留在陶瓷基体的晶粒内部；
在本实施例中，将上述步骤所得的第一粉体和荧光粉体混合烧结，即进行二次烧结，以得到陶瓷基体以及散布于陶瓷基体内的荧光粉体。荧光粉体接受激光激发而发光，实现荧光陶瓷的发光功能。同时，经过 二次烧结，一次烧结所得的气孔会保留在陶瓷基体的晶粒内部，进而制得晶粒内存在气孔的荧光陶瓷。
请参阅图4，图4是本发明荧光陶瓷的制备方法另一实施例的流程示意图。需要说明的是，本实施例所阐述的荧光陶瓷的制备方法并不局限于以下步骤：
S201：对陶瓷基质原料粉体进行预处理；
在本实施例中，提供具有第二粒径的陶瓷基质原料粉体，并对陶瓷基质原料粉体进行预处理，以得到具有第一粒径的第一粉体。具体可以包括：取部分的陶瓷基质原料粉体进行烧结，得到第一粉体坯，而剩余的陶瓷基质原料粉体即为第二粉体。将第一粉体坯进行破碎、研磨，得到晶粒内部形成有气孔的第一粉体。其中，陶瓷基质原料粉体、第一粉体以及第二粉体为同种材质。
具体地，将所取的部分陶瓷基质原料粉体置于坩埚(坩埚的材质与陶瓷基质原料粉体、第一粉体相同，能够避免陶瓷基质原料粉体、第一粉体与坩埚产生化学反应，有利于维持陶瓷基质原料粉体、第一粉体的成分稳定)中，振实并压实处理；随即在马弗炉中烧结2h～6h，烧结温度为1600℃～1800℃；待烧结完冷却后，将第一粉体坯中的烧结块体进行破碎并球磨粉碎至粒径为第一粒径，即得到第一粉体，装瓶待用，完成对陶瓷基质原料粉体的预处理。
S202：将第一粉体、第二粉体、荧光粉体以及烧结助剂进行球磨混合，以得到第一混合粉体坯；
在本实施例中，将预处理所得的第一粉体、第二粉体、荧光粉体以及烧结助剂进行球磨混合(球磨属于本领域技术人员的理解范畴，在此就不再赘述)，以得到第一混合粉体坯，用于后续的烧结环节。其中，第一粉体与第二粉体的质量比为4:6至7:3，荧光粉体占第一混合粉体坯总质量的30％～70％，烧结助剂占所述第一混合粉体坯总质量的0.1％～1％。发明人通过大量实验数据总结得到，当第一粉体、第二粉体、荧光粉体以及烧结助剂的添加量如上述所示时，制得的荧光陶瓷在各方面均能表现出良好的性能。
需要说明的是，第一粉体的粒径大于第二粉体的粒径，即第一粒径大于第二粒径。晶粒粒径较小的第二粉体与晶粒粒径较大的第一粉体混合烧结，第二粉体可以在二次烧结的过程中更好地与第一粉体融合，将第一粉体的各晶粒连接成连续相，以使最终制得的荧光陶瓷的陶瓷基体为连续物相，使得荧光陶瓷具有良好的导热能力，有利于其散热，同时具有良好的结构强度。
可选地，第一粒径可以为5μm～10μm，第二粒径可以为0.05μm～0.5μm。发明人通过大量实验数据总结得到第一粉体和第二粉体的上述最优粒径范围，能够最大限度地利于荧光陶瓷中气孔的形成以及使得陶瓷基体能够形成连续物相。
可选地，烧结助剂可以为氧化镁、氧化钇、氧化镧、氧化钛中的至少一种。并且，烧结助剂优选为氧化钛，添加氧化钛作为烧结助剂会促使陶瓷基体更易形成晶内孔。晶内孔的形成主要是由于变价钛离子使基于陶瓷基体(例如氧化铝材质的陶瓷基体)出现大量晶格缺陷，还与陶瓷基体形成固溶体，促进晶界迁移从而形成晶内孔。气孔由界面扩散转变为体扩散，其扩散过程所需能量更高而难以排出，进而更易于形成晶内孔。
S203：对第一混合粉体坯进行烧结，以得到第二混合粉体坯；
在本实施例中，将混合得到的第一混合粉体坯充填至石墨磨具中，对第一混合粉体在较小压力下进行预压处理，随后将充填有第一混合粉体坯的石墨磨具置于SPS热压炉中，在真空或保护气体的氛围中进行保温烧结，以得到第二混合粉体坯。
其中，发明人通过大量实验数据总结得到，当烧结温度为1300℃～1600℃，烧结时的压力为20MPa～180MPa，烧结时长为0.5h～4h时，能够最大限度地利于第一混合粉体坯中各种粉体之间的烧结结合，以制得满足要求的荧光陶瓷。
可选地，保护气体可以为氦气、氖气、氩气等惰性气体，或是其他化学性质不活泼的气体，在此不做限定。
需要说明的是，通过对陶瓷基质原料粉体进行预烧结，相互接触的 陶瓷基质原料粉体颗粒在烧结过程中，逐渐由点接触到面接触，形成烧结颈。随后将第一粉体坯的团聚块进行粉碎，再同未处理的第二粉体、荧光粉体以及少量的烧结助剂一同烧结。烧结助剂位于预先处理形成的大颗粒第一粉体和未处理的第二粉体以及荧光粉体表面。在烧结过程中，烧结助剂会加快第一粉体和第二粉体间的烧结，而预处理过的大颗粒第一粉体31内容易形成气孔32，并且气孔32会因难以排除而存留在晶粒内部，进而获得晶粒内存在气孔的荧光陶瓷，如图5所示。小颗粒的第二粉体能够填充于第一粉体的晶粒之间，使得第一粉体和第二粉体所形成的陶瓷基体为连续相，保证其具备良好的导热性能。
S204：对第二混合粉体坯进行退火处理，以得到荧光陶瓷；
在本实施例中，对第一混合粉体坯进行烧结得到第二混合粉体坯后，需要对第二混合粉体坯进行退火处理，以得到荧光陶瓷。具体地，将第二混合粉体坯置于空气氛围中进行退火处理。退火处理的温度为1200℃～1400℃，时长为5h～20h。
S205：对荧光陶瓷进行后处理；
在本实施例中，经过退火处理得到荧光陶瓷的粗坯后，需要对荧光陶瓷进行后处理，使得荧光陶瓷满足产品的尺寸规格以及表面性质的要求。具体地，对荧光陶瓷所进行的后处理包括切割处理、研磨处理以及抛光处理等中的至少一种。其中，切割处理旨在将荧光陶瓷的粗坯裁切出产品要求的大小、形状的荧光陶瓷；而研磨处理以及抛光处理旨在使得荧光陶瓷的表面平整度、光滑度等表面性质满足产品要求。
结合上文所述的荧光陶瓷的制备方法，以下举例说明几种具体的荧光陶瓷制备过程：
第一实施例：
将粒径在0.1μm的纳米氧化铝粉置于氧化铝坩埚中，振实并压实处理，所用氧化铝的纯度在99％以上；随即在马弗炉中并在1700℃的温度下预烧结4h。待烧结完冷却后，将氧化铝烧结块体进行破碎并球磨粉碎至粒径在5～10μm的第一粉体，装瓶待用。
将预处理后的氧化铝粉(即第一粉体)同未处理的氧化铝粉(即第 二粉体)按质量比6：4，同少量的无水乙醇进行球磨混合，选用氧化铝球(与选用氧化铝坩埚同理)进行球磨混料，球磨时间为24h。同时添加氧化镁做烧结助剂，其占粉体总质量的0.5％。称取一定量的YAG:Ce荧光粉，其占总粉体的50％，球磨混合1h后，将浆料于70℃下干燥，随后进行研磨，过筛处理。
将混合后的荧光陶瓷粉体充填至石墨模具中，对粉体在小压力下进行预压处理，随后将石墨模具置于SPS热压炉中，在真空气氛中，1500℃下保温烧结1h，烧结时压力在50MPa。待烧结完成后将荧光陶瓷在空气气氛下1200℃退火15h。最后对荧光陶瓷进行切割，研磨抛光处理，即可获得晶内多孔的荧光陶瓷。
第二实施例：
将粒径在0.05μm的纳米氧化铝粉置于氧化铝坩埚中，振实并压实处理，所用氧化铝的纯度在99％以上；随即在马弗炉中并在1650℃的温度下预烧结5h。待烧结完冷却后，将氧化铝烧结块体进行破碎并球磨粉碎至粒径在5～10μm的第一粉体，装瓶待用。
将预处理后的氧化铝粉(即第一粉体)同未处理的氧化铝粉(即第二粉体)按质量比1：1，同少量的无水乙醇进行球磨混合，选用氧化铝球进行球磨混料，球磨时间为16h。同时添加氧化镁和氧化钇做烧结助剂，其分别占粉体总质量的04％和0.5％。称取一定量的YAG:Ce荧光粉，其占总粉体的40％，球磨混合1h后，将浆料于70℃下干燥，随后进行研磨，过筛处理。
将混合后的荧光陶瓷粉体充填至石墨模具中，对粉体在小压力下进行预压处理，随后将石墨模具置于SPS热压炉中，在真空气氛中，1550℃下保温烧结0.5h，烧结时压力在60MPa。待烧结完成后将荧光陶瓷在空气气氛下1300℃退火8h。最后对荧光陶瓷进行切割，研磨抛光处理，即可获得晶内多孔的荧光陶瓷。
第三实施例(本实施例中省略预处理环节)：
选取高纯度纳米级别的氧化铝粉和氧化钛粉(作为烧结助剂)，二者纯度均在99％以上；将二者同少量的无水乙醇一同倒入球磨罐中，氟 化钛占粉体总质量的1％，选取高纯度的氧化铝球进行球磨，球磨时间为20h。
称取一定的YAG:Ce荧光粉，其占总粉体质量的60％；球磨1h后，在60℃下进行真空干燥，随即进行研磨、过筛处理，待用。
将陶瓷素坯置于热压烧结炉中，在氩气气氛下，压力为40MPa，1550℃下烧结1h。待热压烧结后，将荧光陶瓷在空气气氛下，1350℃退火处理10h；最后对陶瓷进行粗磨、细磨以及抛光处理得到晶内多孔的荧光陶瓷。
综上所述，本发明所提供的荧光陶瓷的制备方法提供粒径大小不同但为同种材质的第一粉体、第二粉体，并将二者与荧光粉体混合烧结，使得荧光粉体散布于第一粉体和第二粉体所形成的陶瓷基体内，且在陶瓷基体的晶粒内部形成气孔。当荧光陶瓷受蓝色激光照射时，蓝色入射激光经过陶瓷基体的晶粒内部的气孔会产生散射，被散射的蓝色激光进而可以激发其附近更多的荧光粉体发光，从而提高荧光陶瓷的发光效率。
请参阅图6，图6是本发明光源装置一实施例的结构示意图。
在本实施例中，光源装置4包括荧光陶瓷41。荧光陶瓷41可以为上述实施例所阐述的荧光陶瓷，在此就不再赘述。光源装置4的具体应用形式可以为固定式光源、微投光源、电视以及其他投影设备等，在此不做限定。
以上所述仅为本发明的实施方式，并非因此限制本发明的专利范围，凡是利用本发明说明书及附图内容所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (14)

  1. 一种荧光陶瓷，其特征在于，所述荧光陶瓷包括陶瓷基体以及散布于所述陶瓷基体内的荧光粉体，其中所述陶瓷基体的晶粒内部形成有气孔。
  2. 根据权利要求1所述的荧光陶瓷，其特征在于，所述陶瓷基体的晶粒内部形成有多个均匀分布的所述气孔。
  3. 根据权利要求2所述的荧光陶瓷，其特征在于，所述气孔的孔径为0.1μm～2μm。
  4. 根据权利要求1所述的荧光陶瓷，其特征在于，所述荧光粉体的粒径为5μm～30μm。
  5. 根据权利要求1所述的荧光陶瓷，其特征在于，所述陶瓷基体的晶粒粒径为5μm～20μm。
  6. 一种荧光陶瓷的制备方法，其特征在于，所述制备方法包括：
    提供陶瓷基质原料粉体；
    将所述陶瓷基质原料粉体进行烧结，得到晶粒内部形成有气孔的第一粉体；
    将所述第一粉体和荧光粉体混合烧结，进而将所述气孔保留在所述陶瓷基体的晶粒内部。
  7. 根据权利要求6所述的制备方法，其特征在于，所述将所述陶瓷基质原料粉体进行烧结，得到晶粒内部形成有气孔的第一粉体的步骤包括：
    取部分的所述陶瓷基质原料粉体进行烧结，得到第一粉体坯；其中，剩余的所述陶瓷基质原料粉体为第二粉体；
    将所述第一粉体坯进行破碎、研磨，得到晶粒内部形成有所述气孔的所述第一粉体。
  8. 根据权利要求7所述的制备方法，其特征在于，所述取部分的所述陶瓷基质原料粉体进行烧结，得到第一粉体坯的步骤包括：
    将所取的部分所述陶瓷基质原料粉体置于一温度为1600℃～1800℃ 的氛围中烧结2h～6h，得到所述第一粉体坯。
  9. 根据权利要求7所述的制备方法，其特征在于，所述第一粉体的粒径大于所述第二粉体的粒径。
  10. 根据权利要求7所述的制备方法，其特征在于，所述将所述第一粉体和荧光粉体混合烧结的步骤包括：
    将所述第一粉体、所述第二粉体、所述荧光粉体以及烧结助剂混合烧结；其中，所述烧结助剂为氧化镁、氧化钇、氧化镧、氧化钛中的至少一种。
  11. 根据权利要求10所述的制备方法，其特征在于，所述烧结助剂至少包括氧化钛。
  12. 根据权利要求10所述的制备方法，其特征在于，所述将所述第一粉体、所述第二粉体、所述荧光粉体以及烧结助剂混合烧结的步骤包括：
    将所述第一粉体、所述第二粉体、所述荧光粉体以及所述烧结助剂进行球磨混合，以得到第一混合粉体坯；
    将所述第一混合粉体坯置于真空或保护气体氛围中进行保温烧结，以得到第二混合粉体坯；其中，烧结温度为1300℃～1600℃，烧结时的压力为20MPa～180MPa，烧结时长为0.5h～4h；
    将所述第二混合粉体坯置于空气氛围中进行退火处理，以得到所述荧光陶瓷；其中，所述退火处理的温度为1200℃～1400℃、时长为5h～20h。
  13. 根据权利要求12所述的制备方法，其特征在于，所述荧光粉体占所述第一混合粉体坯总质量的30％～70％，所述烧结助剂占所述第一混合粉体坯总质量的0.1％～1％，且所述第一粉体与所述第二粉体的质量比为4:6至7:3。
  14. 一种光源装置，其特征在于，所述光源装置包括如权利要求1至5任一项所述的荧光陶瓷。
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