WO2021104399A1 - 荧光陶瓷及其制备方法、发光装置以及投影装置 - Google Patents

荧光陶瓷及其制备方法、发光装置以及投影装置 Download PDF

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WO2021104399A1
WO2021104399A1 PCT/CN2020/131911 CN2020131911W WO2021104399A1 WO 2021104399 A1 WO2021104399 A1 WO 2021104399A1 CN 2020131911 W CN2020131911 W CN 2020131911W WO 2021104399 A1 WO2021104399 A1 WO 2021104399A1
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scattering
fluorescent ceramic
refractive index
fluorescent
ceramic
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English (en)
French (fr)
Chinese (zh)
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李乾
简帅
王艳刚
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Shenzhen Lighting Institute
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Shenzhen Lighting Institute
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Priority to EP20892446.4A priority Critical patent/EP4015483A4/en
Priority to JP2022519736A priority patent/JP7730808B2/ja
Publication of WO2021104399A1 publication Critical patent/WO2021104399A1/zh
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Definitions

  • This application relates to the field of fluorescent ceramics, in particular to a fluorescent ceramic and a preparation method thereof, a light emitting device and a projection device.
  • YAG fluorescent ceramics are different from YAG pure phase ceramics. By doping cerium and other lanthanide elements in YAG, a small amount of this element replaces part of the position of yttrium, so that YAG fluorescent ceramics can obtain luminous performance and can convert incident light into Longer wavelength light.
  • the present application provides a fluorescent ceramic and a preparation method thereof, a light emitting device, and a projection device, which can improve the scattering performance of the fluorescent ceramic to fluorescence, thereby improving the light efficiency utilization rate in the light source system.
  • the present application provides a fluorescent ceramic, which at least includes: a matrix; a light emitting center, a first scattering unit, and a second scattering unit distributed in the matrix; the refractive index of the first scattering unit is greater than the refractive index of the light emitting center ; The refractive index of the second scattering unit is less than the refractive index of the light emitting center.
  • the preparation method includes: preparing a fluorescent ceramic matrix material, a scattering material, and phosphor particles in a predetermined ratio, wherein the scattering material at least includes a pore former and a first scattering material.
  • the matrix material and the scattering material are mixed and ball milled in the first solvent to obtain the first ball mill slurry; the phosphor particles are mixed and ball milled in the second solvent to obtain the second ball mill slurry;
  • the first ball mill slurry and the second ball mill slurry are dried, and after drying, they are ground and sieved to obtain the first powder and the second powder; the first powder and the second powder are mixed, and the mixed powder is compressed, Obtain a preform; subject the preform to high temperature debinding treatment to obtain a green body; subject the green body to cold isostatic pressing; perform high temperature sintering on the green body after cold isostatic pressing, and obtain fluorescent ceramics after polishing .
  • the present application provides a light-emitting device, including an excitation light source and the aforementioned fluorescent ceramic, and the excitation light source is an incident laser light source.
  • the present application provides a projection device, including the aforementioned light-emitting device.
  • the beneficial effect of the present application is: different from the prior art, the present application uniformly distributes luminescent centers with different refractive indices, the first scattering unit, and the second scattering unit in the matrix of the fluorescent ceramic, and the first scattering unit
  • the refractive index is greater than the refractive index of the light emitting center, and the refractive index of the second scattering unit is less than the refractive index of the light emitting center. Since the scattering ability of particles depends on the linearity and relative refractive index of the particles, the incident laser light will be scattered at the interface of each phase.
  • the refraction and scattering of the incident laser light and fluorescence inside the fluorescent ceramic can be strengthened to make the excitation light
  • the optical path in the ceramic becomes longer, which weakens the lateral conduction of the fluorescence inside the fluorescent ceramic, so that the fluorescence is finally scattered from a small area near the incident laser, that is, the fluorescent spot produced is smaller, and the fluorescent ceramics’ ability to fluorescence is improved. Scattering performance.
  • FIG. 1 is a schematic structural diagram of an embodiment of the fluorescent ceramic of the present application.
  • FIG. 2 is a schematic flow chart of an embodiment of a method for preparing fluorescent ceramics according to the present application
  • FIG. 3 is a photo of the microstructure of the fluorescent ceramic prepared in Example 2.
  • FIG. 1 is a schematic structural diagram of an embodiment of the fluorescent ceramic of the present application.
  • the fluorescent ceramic includes at least: a substrate 101, a light emitting center 102, a first scattering unit 103 and a second scattering unit 104.
  • the luminous center 102, the first scattering unit 103 and the second scattering unit 104 are distributed in the matrix 101.
  • the substrate 101 can be prepared from a ceramic raw material.
  • the ceramic raw material can include one of alumina, aluminum nitride, silicon carbide, silicon nitride, and zirconia. It is characterized by low refractive index, good thermal conductivity, and light transmittance. Good to withstand the temperature during subsequent sintering.
  • the substrate 101 may be a cubic crystal system transparent ceramic with a garnet structure, and the light-emitting center 102 may be a phosphor with a garnet structure. When the light-emitting center 102 and the substrate 101 both have a garnet structure, the fluorescent ceramic can be optimized. The luminous performance and mechanical properties.
  • the matrix 101 is an alumina matrix
  • the luminous center 102 is a phosphor.
  • the alumina belongs to the trigonal crystal system and has birefringence. Therefore, there is grain boundary birefringence in the alumina matrix.
  • the incident laser light is in the fluorescent ceramic. Scattering occurs due to the birefringence of the grain boundary, and the scattered incident laser light can excite more luminous centers near it, which in turn makes the luminous efficiency good.
  • the inventor of the present application found that the refractive index of the alumina matrix and the refractive index of the phosphor are both 1.7-1.8, which are very close, resulting in the refraction or refraction of the incident laser and fluorescence by the fluorescent ceramics.
  • the scattering effect is weak, and it is easy to be transmitted to the surroundings in the lateral direction of the ceramic, which ultimately leads to a larger fluorescent spot of the fluorescent ceramic.
  • the spot spread is large, the collection efficiency of the collecting lens is low, which affects the light efficiency utilization rate in the light source system.
  • the inventors of the present application are distributed in the matrix with at least the difference between the refractive index and the luminescent center.
  • the first scattering unit and the second scattering unit, and the refractive index of the first scattering unit is greater than the refractive index of the light emitting center, and the refractive index of the second scattering unit is smaller than the refractive index of the light emitting center.
  • the feature of large difference in refractive index of the first scattering unit, the luminous center, and the first scattering unit in the fluorescent ceramic (it can be understood that because the refractive index of the substrate and the luminous center are close, the first scattering unit and the second scattering unit are different from each other.
  • the refractive index difference between the substrates is also large), and the scattering of incident laser light at the interface of each phase is strengthened.
  • the optical path of the excitation light in the ceramic becomes longer, and the lateral transmission of the fluorescence inside the fluorescent ceramic is weakened, so that the fluorescence finally moves from the small area near the incident laser.
  • the scope area is scattered out, that is, the generated fluorescent spot is small, and the scattering performance of the fluorescent ceramic to the fluorescent light is improved, thereby improving the light efficiency utilization rate in the light source system.
  • the refractive index difference between the first scattering unit 103 and the light emitting center 102, the second scattering unit 104 and the light emitting center is different, and the specific is not limited.
  • the refractive index difference between the first scattering unit 103 and the light emitting center 102 can reach 0.01-2.0, for example, 0.01, 0.4, 0.6, 0.8 or 2.0.
  • the refractive index difference between the second scattering unit 104 and the luminous center 102 can reach 0.01-2.0, for example, 0.01, 0.4, 0.6, 0.8 or 2.0.
  • the present application uniformly distributes the luminescence centers with different refractive indexes, the first scattering unit, and the second scattering unit in the matrix of the fluorescent ceramic, and the refractive index of the first scattering unit is greater than the refraction of the luminescence center.
  • the refractive index of the second scattering unit is smaller than the refractive index of the light emitting center. Since the scattering ability of particles depends on the linearity and relative refractive index of the particles, the incident laser light will be scattered at the interface of each phase.
  • the refraction and scattering of the incident laser light and fluorescence inside the fluorescent ceramic can be strengthened to make the excitation light
  • the optical path in the ceramic becomes longer, which weakens the lateral conduction of the fluorescence inside the fluorescent ceramic, so that the fluorescence is finally scattered from a small area near the incident laser, that is, the fluorescent spot produced is smaller, and the fluorescent ceramics’ ability to fluorescence is improved. Scattering performance, thereby improving the light efficiency utilization rate in the light source system.
  • the first scattering unit 103 is at least one of pores or first scattering particles.
  • the scattering effect on the excitation light source is better.
  • the particle size of the pores may be 0.2 ⁇ m, 0.8 ⁇ m, 1.0 ⁇ m, or 2.0 ⁇ m.
  • the particle size of the pores in this embodiment refers to the diameter of the pores when the pores are spherical; when the pores are non-spherical, the particle size of the pores is the diameter of the smallest circumscribed sphere of the pores.
  • the volume fraction of the pores in the fluorescent ceramic in this embodiment is 0.01%-10%, such as 0.01%, 0.1%, 1%, 5% or 10% .
  • the refractive index of the first scattering particles is 1.2-3.5, such as 1.2, 1.7, 2.1, 2.5, or 3.5.
  • the first scattering particles account for 0.1% to 1% of the total mass of the fluorescent ceramic, for example, 0.1%, 0.5%, 0.8%, or 1%.
  • the above-mentioned first scattering particles may be at least one of titanium dioxide, zirconium oxide, yttrium oxide, calcium fluoride or magnesium fluoride.
  • the second scattering unit 104 is at least one of pores or second scattering particles.
  • the scattering effect on the excitation light source is better.
  • the particle size of the pores may be 0.2 ⁇ m, 0.8 ⁇ m, 1.0 ⁇ m, or 2.0 ⁇ m.
  • the particle size of the pores in this embodiment refers to the diameter of the pores when the pores are spherical; when the pores are non-spherical, the particle size of the pores is the diameter of the smallest circumscribed sphere of the pores.
  • the volume fraction of the pores in the fluorescent ceramic in this embodiment is 0.01%-10%, such as 0.01%, 0.1%, 1%, 5% or 10% .
  • the refractive index of the second scattering particles is 1.2-2.5, such as 1.2, 1.4, 1.6, 1.8 or 2.5.
  • the second scattering particles account for 0.1% to 1% of the total mass of the fluorescent ceramic, such as 0.1%, 0.5%, 0.8%, or 1%.
  • the above-mentioned second scattering particles are at least one of calcium fluoride, magnesium fluoride, yttrium oxide or zirconium oxide.
  • the fluorescent ceramic further includes: third scattering units (not shown in the figure) distributed in the matrix 101,
  • the refractive index of the third scattering unit is between the first scattering unit 103 and the second scattering unit 104.
  • the refractive index difference between the first scattering unit 103 and the third scattering unit, the second The refractive index difference between the scattering unit 104 and the third scattering unit, and the refractive index difference between the light-emitting center and the third scattering unit are different, which are not specifically limited.
  • the absolute difference between the refractive index of the third scattering unit and the refractive index of the first scattering unit 103 is 0.6 to 1.5, for example, 0.6, 0.8, 1.0, or 1.5.
  • the absolute difference between the refractive index of the third scattering unit and the refractive index of the second scattering unit 104 is 0.6 to 1.5, for example, 0.6, 0.8, 1.0, or 1.5.
  • the third scattering unit is at least one of pores or third scattering particles.
  • the refractive index of the aforementioned third scattering particles is 1.2-2.5, such as 1.2, 1.4, 1.6, 1.8 or 2.5.
  • the third scattering particles account for 0.1% to 1% of the total mass of the fluorescent ceramic, such as 0.1%, 0.5%, 0.8%, or 1%.
  • the aforementioned light emitting center 102 is a lanthanide-doped YAG phosphor particle with a particle size of 5 ⁇ m-30 ⁇ m, for example, 5 ⁇ m, 10 ⁇ m, 20 ⁇ m, or 30 ⁇ m.
  • the doping amount is 1% to 5%, for example, 1%, 2%, 3%, or 5%.
  • the lanthanide-doped YAG phosphor particles account for 40%-50% of the total mass of the fluorescent ceramic, for example, 40%, 42%, 45% or 50%.
  • the phosphor as the luminous center 102 must have a sufficient amount to ensure the luminous intensity of the fluorescent ceramic.
  • the lanthanide-doped YAG phosphor particles account for 40% to 50% of the total mass of the fluorescent ceramic, the luminous efficiency is improved due to the luminescent center 102 with a large grain size, and there is no impurity phase, and the grain boundary is pure and uniform.
  • the light performance is good, which can meet the needs of high-power light sources such as incident laser; at the same time, due to the addition of scattering particles, when the incident laser irradiates the scattering particles, the excitation light source is scattered; after the excitation light source is scattered, the excitation light is in the ceramic
  • the optical path length of the light is longer, thereby improving the light conversion efficiency.
  • the material of the matrix 101 is alumina with a particle size of 0.05 ⁇ m to 1 ⁇ m, for example, 0.05 ⁇ m, 0.1 ⁇ m, 0.5 ⁇ m, or 1.0 ⁇ m.
  • Alumina accounts for 40%-60% of the total mass of the fluorescent ceramic, for example, 40%, 50%, 55% or 60%.
  • the lanthanide-doped YAG phosphor particles are Ce or Lu-doped YAG phosphor particles.
  • the preparation scheme adopted in this embodiment doped the YAG substrate 101 with Ce at a percentage of 1% to 5%.
  • Lu can be doped so that the YAG substrate 101 can also emit light, which is used as a fluorescent ceramic.
  • the YAG matrix 101 is used as the bonding medium to bond YAG phosphor particles with large grain sizes.
  • the fluorescent ceramic can be achieved within a certain range.
  • the color coordinate is adjustable; the doping content of YAG matrix 101 and YAG phosphor particles with large grain size are different, and the fluorescence spectrum range is different. The two complement each other and improve the color rendering of incident laser light.
  • the scattering particles with high refractive index are uniformly distributed in the fluorescent ceramics.
  • the incident laser is irradiated on the scattering particles, the excitation light source is scattered; after the excitation light source is scattered, the optical path of the excitation light in the ceramic becomes longer, thereby increasing the light Conversion efficiency.
  • FIG. 2 is a schematic flowchart of an embodiment of a method for preparing fluorescent ceramics according to the present application. This application also provides a method for preparing fluorescent ceramics, which includes:
  • the matrix material can be alumina with a purity of 99.0% and a particle size of 0.05 ⁇ m to 1 ⁇ m.
  • the phosphor particles can be selected from YAG phosphor particles doped with lanthanides with a purity of 99.0% and a particle size of 5 ⁇ m-30 ⁇ m.
  • the scattering material includes at least a pore former and first and second scattering particles.
  • the pore former is starch (particle size 0.1 ⁇ m-10 ⁇ m, such as 0.1 ⁇ m, 1 ⁇ m, 10 ⁇ m) or PMMA microspheres (particle diameter 0.1 ⁇ m-10 ⁇ m, such as 0.1 ⁇ m, 1 ⁇ m, 10 ⁇ m).
  • the first scattering particles can be selected from at least one of titanium dioxide, zirconium oxide, yttrium oxide, calcium fluoride or magnesium fluoride with a purity of 99.0%.
  • the second scattering particles can be at least one of calcium fluoride, magnesium fluoride, yttrium oxide or zirconium oxide with a purity of 99.0%.
  • the matrix material and the scattering material are mixed according to a preset ratio, and the first solvent is used as the liquid phase medium, and placed in a ball mill tank for ball milling and mixing.
  • the ball milling speed is 120r/min ⁇ 300r/min, and the ball milling is 1h ⁇ After 4h, the first ball mill slurry was obtained.
  • the first solvent can be silicone oil, ethanol, ethylene glycol, xylene, ethyl cellulose, terpineol, butyl carbitol, PVA, PVB, PAA, PEG in various systems including phenyl, methyl, etc.
  • One or more mixtures can be silicone oil, ethanol, ethylene glycol, xylene, ethyl cellulose, terpineol, butyl carbitol, PVA, PVB, PAA, PEG in various systems including phenyl, methyl, etc.
  • One or more mixtures are possible.
  • the first solvent is used as the liquid phase medium
  • the phosphor particles are put into a ball milling tank, and the ball milling is carried out, and the ball milling speed is 120r/min ⁇ 300r/min.
  • the second ball grinding slurry is obtained.
  • the second solvent can be silicone oil, ethanol, ethylene glycol, xylene, ethyl cellulose, terpineol, butyl carbitol, PVA, PVB, PAA, PEG in various systems including phenyl, methyl, etc. One or more mixtures.
  • the first ball mill slurry and the second ball mill slurry can be vacuum defoamed to obtain a low or even bubble-free first ball mill slurry and a second ball mill slurry suitable for casting.
  • the first ball mill slurry and the second ball mill slurry are dried in vacuum at a constant temperature to obtain dry powder, and the dry powder is calcined in a muffle furnace to remove organic components in the dry powder, and then the powder is sieved and granulated to obtain the first powder And the second powder.
  • the pressing method is not particularly limited, and conventional pressing methods such as cold isostatic pressing and the like can be used.
  • the pressing pressure is usually 5 MPa to 200 MPa, preferably 15 MPa to 100 MPa. If the pressure is too small, there will be more and larger pores, which will affect the density of the final sintered product.
  • the crucible loaded with the preform is placed in the muffle furnace near the thermocouple to start the debinding process.
  • the debinding process can be as follows: at a heating rate of 0.3°C/min to 0.6°C/min, heating to 200°C for 0h to 2h to remove free water, crystal water and other moisture in the body. Then, the temperature is increased to 500°C at a heating rate of 0.4°C/min-0.7°C/min for 0h to 3h to decompose and volatilize the organic matter in the green body. Then increase to the densification temperature at a heating rate of 0.4°C/min ⁇ 0.7°C/min for 2h ⁇ 6h.
  • the densification temperature is generally lower than the sintering temperature of the ceramic by 300°C to 1000°C to avoid the sintering process of the raw material powder and the ceramic body, and facilitate the removal of the raw material powder.
  • the cooling method is furnace cooling, and the atmosphere is atmospheric. Through the debinding process, not only the moisture and organic matter in the green body are removed, but also the green body obtains uniform shrinkage and achieves a certain degree of densification, with a volume shrinkage of 4%-30% and a weight loss of 20%-50%.
  • the fluorescent ceramic green body is subjected to cold isostatic pressing under a pressure of 150 MPa to 200 MPa to increase the density of the ceramic green body.
  • S80 Carry out high-temperature sintering treatment on the blank after cold isostatic pressing, and obtain fluorescent ceramics after polishing.
  • the fluorescent ceramic obtained after the heat treatment further includes a reduction treatment step for the fluorescent ceramic.
  • This step is carried out in a reducing atmosphere (such as a nitrogen/hydrogen mixed gas).
  • the reduction treatment is carried out at a temperature slightly lower than the sintering temperature of the heat treatment. It is 1200°C ⁇ 1650°C.
  • the reduction treatment process can remove impurities attached to the fluorescent ceramic in the heat treatment step, and prevent the impurities from becoming the heat generating center of the fluorescent ceramic in the working environment and affecting the use of the fluorescent ceramic.
  • the matrix of the fluorescent ceramic may be an alumina matrix
  • the luminescent center is a fluorescent powder. Since alumina belongs to the trigonal crystal system, there is birefringence phenomenon, so there is grain boundary birefringence in the alumina matrix fluorescent ceramic, and the incident laser light Fluorescent ceramics will scatter due to the birefringence of the grain boundaries, and the scattered incident laser light can excite more luminous centers in the vicinity, thereby making the luminous efficiency good.
  • the inventor of the present application found that the refractive index of the alumina matrix and the refractive index of the phosphor are both 1.7-1.8, which are very close, resulting in the refraction or refraction of the incident laser and fluorescence by the fluorescent ceramics.
  • the scattering effect is weak, and it is easy to be transmitted to the surroundings in the lateral direction of the ceramic, which ultimately leads to a larger fluorescent spot of the fluorescent ceramic.
  • the spot spread is large, the collection efficiency of the collecting lens is low, which affects the light efficiency utilization rate in the light source system.
  • the inventors of the present application are distributed in the matrix with at least the difference between the refractive index and the luminescent center.
  • the first scattering unit and the second scattering unit, and the refractive index of the first scattering unit is greater than the refractive index of the light emitting center, and the refractive index of the second scattering unit is smaller than the refractive index of the light emitting center.
  • the feature of large difference in refractive index of the first scattering unit, the luminous center, and the first scattering unit in the fluorescent ceramic (it can be understood that because the refractive index of the substrate and the luminous center are close, the first scattering unit and the second scattering unit are different from each other.
  • the refractive index difference between the substrates is also large), and the scattering of incident laser light at the interface of each phase is strengthened.
  • the optical path of the excitation light in the ceramic becomes longer, and the lateral transmission of the fluorescence inside the fluorescent ceramic is weakened, so that the fluorescence finally moves from the small area near the incident laser.
  • the scope area is scattered out, that is, the generated fluorescent spot is small, and the scattering performance of the fluorescent ceramic to the fluorescent light is improved, thereby improving the light efficiency utilization rate in the light source system.
  • the present application uniformly distributes the luminescence centers with different refractive indexes, the first scattering unit, and the second scattering unit in the matrix of the fluorescent ceramic, and the refractive index of the first scattering unit is greater than the refraction of the luminescence center.
  • the refractive index of the second scattering unit is smaller than the refractive index of the luminescent center. Since the scattering ability of the particles depends on the linearity and relative refractive index of the particles, the incident laser will be scattered at the interface of each phase. Therefore, the fluorescent ceramics can be strengthened.
  • the refraction and scattering effects of the incident laser light and the fluorescence inside it make the optical path of the excitation light in the ceramic become longer, thereby weakening the lateral conduction of the fluorescence inside the fluorescent ceramic, so that the fluorescence is finally scattered from a small area near the incident laser. That is, the generated fluorescent spot is smaller, and the scattering performance of the fluorescent ceramic to the fluorescent light is improved, thereby improving the light efficiency utilization rate in the light source system.
  • alumina powder, zirconia powder and magnesium fluoride powder with a purity of 99.0% or more, weigh 99.0% alumina powder, 0.5% zirconia powder and 0.5% magnesium fluoride powder according to mass percentages, and then use wet ball milling Method: Use absolute ethanol as a medium to grind the mixed powder raw materials, and the ball milling time is 24 hours to obtain the first ball mill slurry.
  • the mass percentage of PVB in the PVB ethanol solution is 0.5%-2%.
  • the mass percentage refers to the percentage of the mass of a certain substance to the total mass, here refers to the mass of PVB to the total percentage of the solution composed of PVB and ethanol.
  • the mixed fluorescent ceramic powder is pressed into a block under a pressure of 80 MPa. Then the molded ceramic blank is debinding in a muffle furnace. The debinding process is 500°C for 2 hours and 900°C for 4 hours. After debinding, the fluorescent ceramic green body is subjected to cold isostatic pressing under a pressure of 200 MPa to increase the density of the ceramic green body.
  • the ceramic green body is placed in a vacuum furnace with a vacuum degree of 10-3 Pa and sintered at 1650°C for 4 hours. After vacuum sintering, the fluorescent ceramics are annealed at 1300°C for 10 hours in an air atmosphere; then the fluorescent ceramics are thinned and polished, and finally usable fluorescent ceramics are obtained.
  • alumina powder with a purity of 99.9% or more, titanium oxide with a purity of 99%, and a pore former and weigh 98.0% of the alumina powder, 1.0% of the titanium oxide powder and 1.0% of the pore former according to mass percentages, and anhydrous Ethanol is used as the medium to grind the mixed powder raw materials, and the ball milling time is 24 hours to obtain the first ball mill slurry.
  • the mass percentage of PVB in the PVB ethanol solution is 0.5%-2%.
  • the mass percentage refers to the percentage of the mass of a certain substance to the total mass, here refers to the mass of PVB to the total percentage of the solution composed of PVB and ethanol.
  • Vacuum drying is carried out at 60°C, then grinding and sieving are carried out, and the powder is filled for later use.
  • the mixed fluorescent ceramic powder is pressed into a block under a pressure of 50 MPa. Then the formed ceramic green body is debinding in a muffle furnace. The debinding process is 600°C for 2 hours and 1000°C for 6 hours. After debinding, the fluorescent ceramic green body is subjected to cold isostatic pressing under a pressure of 180 MPa to increase the density of the ceramic green body.
  • the ceramic green body is placed in a vacuum furnace with a vacuum degree of 10Pa-3Pa and sintered at 1600°C for 4h. After vacuum sintering, the fluorescent ceramic is annealed at 1350°C for 10 hours in an air atmosphere; then the fluorescent ceramic is thinned and polished to finally obtain a usable fluorescent ceramic.
  • FIG. 3 is a photo of the microstructure of the fluorescent ceramic prepared in Example 2. It can be seen from the figure that after removing the uniformly dispersed phosphor particles in the alumina ceramic matrix, there are still a small amount of low refractive index phase (pores) and high refractive index phase (titanium oxide).
  • alumina powder, magnesium fluoride, titanium oxide and zirconia with a purity of more than 99.9%, and weigh 99.0% of alumina powder, 0.30% of magnesium fluoride, 0.30% of titanium oxide and 0.40% of zirconia according to mass percentages.
  • the wet ball milling method is used to grind the mixed powder raw materials with anhydrous ethanol as the medium, and the ball milling time is 36 hours to obtain the first ball mill slurry.
  • the mass percentage of PVB in the PVB ethanol solution is 0.5%-2%.
  • the mass percentage refers to the percentage of the mass of a certain substance to the total mass, here refers to the mass of PVB to the total percentage of the solution composed of PVB and ethanol.
  • the ceramic powder into the graphite mold, perform pre-pressing treatment under the pressure of 5-20MPa, then place the graphite mold in the SPS hot pressing furnace, in a vacuum/argon atmosphere, heat preservation and sintering at 1200°C-1600°C 0.5 h-4h, the pressure during sintering is 20MPa-150MPa.
  • the fluorescent ceramic is annealed at 1300°C for 10 hours in an air atmosphere; then the fluorescent ceramic is thinned and polished, and finally a usable fluorescent ceramic is obtained.
  • Vacuum drying is carried out at 70°C, then grinding and sieving are carried out, and the powder is filled for later use.
  • the ceramic powder into a graphite mold, and perform pre-pressing treatment at a pressure of 50MPa-20MPa, and then place the graphite mold in an SPS hot pressing furnace, in a vacuum/argon atmosphere, heat preservation and sintering at 1200°C-1600°C for 0.5 h-4h, the pressure during sintering is 200MPa-150MPa.
  • the fluorescent ceramic is annealed at 1300°C for 10 hours in an air atmosphere; then the fluorescent ceramic is thinned and polished, and finally a usable fluorescent ceramic is obtained.
  • Example 1 The fluorescent ceramics prepared in Example 1, Example 2, and Example 3 and the fluorescent ceramics that have not been optimized (ie comparative example) were processed into test samples, and placed in a test platform for test comparison.
  • the test results obtained are as follows As shown, the light effect in the table specifically refers to the conversion efficiency of the blue incident laser light power.
  • the luminescence centers with different refractive indices, the first scattering unit, and the second scattering unit are uniformly distributed in the matrix of the fluorescent ceramic in Examples 1-3, and the first scattering unit and the luminescence center in the matrix are uniformly distributed.
  • the feature that the refractive index difference of the first scattering unit is large (it can be understood that due to the close refractive index of the substrate and the luminous center, the refractive index difference between the first scattering unit and the second scattering unit and the substrate is also large) Since the scattering ability of particles depends on the linearity and relative refractive index of the particles, the incident laser will be scattered at the interface of each phase.
  • the fluorescent ceramic can strengthen the refraction and scattering of the incident laser and fluorescence inside the fluorescent ceramic, so that excitation
  • the optical path of light in the ceramic becomes longer, which weakens the lateral conduction of the fluorescence inside the fluorescent ceramic, so that the fluorescence is finally scattered from a small area near the incident laser, that is, the fluorescent spot produced is smaller, which improves the fluorescence of the fluorescent ceramic.
  • the scattering performance of the light source system improves the light efficiency utilization rate in the light source system.
  • the present application also provides a light-emitting device, including an excitation light source and the above-mentioned fluorescent ceramic, wherein the excitation light source is an incident laser light source, and the fluorescent ceramic is irradiated by the excitation light source to generate high-brightness light.
  • the light-emitting device can be applied to projection and display systems, such as liquid crystal displays (LCD, Liquid Crystal Display) or digital light processor (DLP, Digital Light Processor) projectors; it can also be applied to lighting systems, such as automotive lighting; or Used in the field of 3D display technology.
  • LCD liquid crystal displays
  • DLP Digital Light Processor
  • the above-mentioned fluorescent ceramic can also be made into a movable device, such as a color wheel, so that the excitation light source emitted by the excitation light source is incident on the rotating color wheel to generate incident laser light.
  • the application also provides a projection device.
  • the projection device may be an educational projector, an incident laser TV, a micro-projector or a cinema machine, etc.
  • the projection device includes the light-emitting device of the above-mentioned embodiment.
  • For the specific structure of the light-emitting device refer to the above-mentioned implementation. example.

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