CN109987932B - Complex phase fluorescent ceramic for white light illumination, preparation method and light source device - Google Patents

Complex phase fluorescent ceramic for white light illumination, preparation method and light source device Download PDF

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CN109987932B
CN109987932B CN201810002746.4A CN201810002746A CN109987932B CN 109987932 B CN109987932 B CN 109987932B CN 201810002746 A CN201810002746 A CN 201810002746A CN 109987932 B CN109987932 B CN 109987932B
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sintering
fluorescent
ceramic
light
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CN109987932A (en
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朱宁
叶勇
王红
胡恒庆
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Shanghai Aviation Electric Co Ltd
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Abstract

The invention discloses a complex phase fluorescent ceramic for white light illumination. The complex phase fluorescent ceramic has a fluorescent phase with lutetium aluminum garnet structure and an oxide dispersed phase such as Y 2 O 3 The light scattering phase is uniformly distributed and surrounds the lutetium aluminum garnet fluorescent phase, the grain size is in a nanometer or submicron level, and scattering mainly based on Mie scattering and Releigh scattering is realized on blue light excitation light entering a network structure and fluorescent light emitted by the fluorescent phase. The size of the prepared ceramic grains is less than 5 mu m, and the thermal shock resistance of the fluorescent ceramic can be further improved. The invention has the beneficial effects that: the problems that the white light of the fluorescent material is not uniform and the thermal shock resistance of the fluorescent material is weak in the current white light laser illumination are effectively solved.

Description

Complex phase fluorescent ceramic for white light illumination, preparation method and light source device
Technical Field
The invention relates to the field of laser illumination, in particular to a complex phase fluorescent ceramic for white light illumination, a preparation method and a light source device.
Background
The laser diode has the characteristics of high photoelectric efficiency, high brightness, high collimation, long irradiation distance, small size and the like. Compared with the LED light source product which is only suitable for the field of middle and low brightness, the laser light source can be suitable for the requirements of all brightness, and has incomparable advantages particularly in the fields of high brightness, high luminous efficiency, strong directivity and the like.
The fluorescent material of the white light LED light source can bear the blue light optical power density of 1W/mm in most parts during working 2 Below, not more than 5W/mm at maximum 2 Whereas a single laser diode (e.g., Nichia-4.5W bare spot size of about 1.5mm by 0.5mm) has an average optical power density of about 1.5W/mm 2 In practical application, multiple lasers are usually adopted to converge on the surface of the fluorescent material, that is, the power density of the blue light irradiation required to be borne by the fluorescent material for laser illumination is ten times or even more than one hundred times of that of the white light LED illumination. This allows fluorescence for laser illuminationThe optical material needs to have excellent blue light irradiation resistance, excellent high-temperature fluorescence characteristic and excellent thermal shock resistance.
Due to the technical limitation of the laser, the laser beam has uneven energy density distribution although the laser has strong directivity, and therefore the laser illumination system structure needs to be equipped with an efficient dodging technique. The inventor proposes to introduce scattered light into the high-efficiency fluorescent phase to improve the uniformity of light mixing, thereby simplifying the light path design and the optical-mechanical structure of the laser illumination light source device.
Scattering of light by a material can be divided into rayleigh scattering, Mie scattering, and geometric-optic catadioptric scattering according to the size of the scattering center and Fresnel's law. When the size of the scattering center is smaller than 1/3 of the wavelength of the incident light, rayleigh dominant scattering is formed, and the forward and backward scattering thereof are symmetrically distributed; when the size of the scattering center is larger than 1/3 incident light wavelength or close to the wavelength of light, Mie scattering is mainly used, the forward scattering is more concentrated, and the larger the particle is, the stronger the forward scattering is; when the size of the scattering center is larger than the wavelength of light, reflection and refraction are dominant.
Disclosure of Invention
The 1 st object of the present invention is to provide a fluorescent ceramic matrix lutetium aluminum garnet phase (LuAG) with excellent thermal conductivity, while introducing an oxide dispersed phase such as Y 2 O 3 . The oxide dispersed light has high refractive index>1.8 and the grain size is less than 1000nm, and can cause the scattering mainly based on the rayleigh scattering and the Mie scattering to the blue excitation light entering the fluorescent phase and the emission light of the fluorescent phase. The composite phases are uniformly distributed by three-dimensional mutual surrounding, so that the ceramic composite has uniform fluorescence and excellent heat resistance, and is suitable for being combined with a blue light-emitting element to form a high-efficiency light conversion member of a white light-emitting device.
The invention aims to solve the problem 2 that rare earth doped ions such as Ce, Mn and the like are introduced into a fluorescent ceramic substrate LuAG to adjust the fluorescence peak wavelength to 530-560 nm, so that a light-emitting device containing the ceramic composite realizes white light output, namely, the yellow light emitted by the excitation of blue light of the ceramic is directly compounded with the residual blue light of a laser to form white light. The light emitting element group is suitable for a light conversion member constituting a high-efficiency white light emitting device.
In order to achieve the purpose, the technical scheme of the invention is as follows: the multiphase fluorescent ceramic for white light illumination comprises a lutetium aluminum garnet fluorescent phase and an oxide light dispersing phase, wherein the relative volume fraction content of the oxide light dispersing phase is 0.001-30%, and the oxide light dispersing phase is uniformly distributed in a grid structure of the lutetium aluminum garnet fluorescent phase.
As a preferable scheme of the complex phase fluorescent ceramic for white light illumination, the expression of the lutetium aluminum garnet fluorescent phase is (Lu) 1-x-y RE y Ce x ) 3 (Al 1-z Mn z ) 5 O 12 Wherein RE is one or more of Tb, Gd, Eu, Sm and Pr, x is more than or equal to 0.0001 and less than or equal to 0.1, preferably more than or equal to 0.0005 and less than or equal to 0.05, and more preferably more than or equal to 0.001 and less than or equal to 0.03; y is more than 0 and less than or equal to 0.5, preferably more than 0.001 and less than or equal to 0.05; z is more than 0 and less than or equal to 0.1, preferably more than 0.001 and less than or equal to 0.03.
As a preferable scheme of the complex phase fluorescent ceramic for white light illumination, the refractive index of the oxide dispersed phase is more than 1.8-2.7, and further, the dispersed phase is selected from Y 2 O 3 、La 2 O 3 Lanthanide series rare earth oxide, TeO 2 、ZrO 2 、TiO 2 、ZnO、Nb 2 O 5 、Ta 2 O 5 、HfO 2 One or more of the above (1), the grain size is less than or equal to 1000nm, preferably 50-800 nm, and the distance between adjacent oxide light scattering phase particles is less than 20 μm, preferably less than 5.0 μm.
The preparation method of the complex phase fluorescent ceramic for white light illumination comprises the following steps
Step S1, weighing raw materials and sintering aids;
step S2, ball milling and mixing;
step S3, drying and sieving;
step S4, tabletting and forming;
step S5, sintering into ceramic blocks; and the number of the first and second groups,
and step S6, annealing to obtain the complex phase transparent fluorescent ceramic.
As a preferable scheme of the preparation method of the complex phase fluorescent ceramic for white light illumination, in step S1, the raw material is (Lu, RE, Ce) 3 (Al,Mn) 5 O 12 Fluorescent powder or a fluorescent powder precursor and oxide light-scattering phase powder, wherein the particle size D50 of the fluorescent powder or the fluorescent powder precursor is 0.1-10 mu m, preferably 0.5-3 mu m; the primary particle diameter D50 of the oxide light-scattering powder is 0.01-2 μm, preferably 0.05-0.8 μm.
As a preferable scheme of the preparation method of the complex phase fluorescent ceramic for white light illumination, in step S1, the sintering aid is Li + 、Ca 2+ /Mg 2+ /Ba 2+ 、La 3+ /Y 3+ 、TEOS/SiO 2 The metal ions may be salts in the form of oxides, carbonates, fluorides, etc.; the content is 0.01 to 5.0 wt%, preferably 0.1 to 2.0 wt%.
As a preferable scheme of the preparation method of the complex phase fluorescent ceramic for white light illumination, in step S5, the sintering is performed in one step by atmosphere sintering: the sintering heat preservation temperature is 1650-1800 ℃, and the heat preservation time is 1-20 hours. The sintering heat preservation temperature is preferably 1750-1780 ℃, and the sintering heat preservation time is preferably 3-6 hours.
As a preferred embodiment of the preparation method of the complex phase fluorescent ceramic for white light illumination, in step S5, vacuum two-step sintering is adopted: in a vacuum furnace, the vacuum degree is 10 -2 ~10 -4 Pa, firstly, increasing the sintering temperature to 1780-1820 ℃, and keeping the sintering temperature for 0.5-5 h, and secondly, reducing the sintering temperature to 1680-1780 ℃, and keeping the sintering temperature for 1-30 h; further, the sintering heat preservation of the second step is 1700-1730 ℃, and the sintering heat preservation time is 5-15 h.
As a preferred embodiment of the preparation method of the complex phase fluorescent ceramic for white light illumination, in step S5, two-step sintering by vacuum and hot isostatic pressing is adopted: the first step is sintering in a vacuum furnace with a vacuum degree of 10 -2 ~10 -4 Pa, the heat preservation temperature is 1700-1800 ℃, preferably 1700-1750 ℃, the sintering heat preservation time is 3-6 h, and in the second step, the ceramic block obtained in the first step is placed into a hot isostatic pressing furnace for sintering, the pressure is 150-200 MPa, and the heat preservation temperature is 150-200 MPaThe temperature is 1600-1700 ℃, the heat preservation time is 1-10 h, further, the sintering is 1620-1680 ℃, and the heat preservation time is 3-6 h.
The invention also provides a light source device, comprising,
a blue light exciter with the wavelength of 380-520 nm; and the number of the first and second groups,
the ceramic composite described above.
Compared with the prior art, the invention has the beneficial effects that:
1) introducing high-refractive index microcrystalline oxide light-scattering phase such as Y into garnet fluorescent phase structure 2 O 3 The oxide scattering phase is uniformly distributed and three-dimensionally surrounds the fluorescent phase, and scatters the incident blue light excitation light and the ceramic emission light to enable the emergent fluorescence of the ceramic composite to be uniform;
2) a lutetium aluminium garnet fluorescent phase ((Lu, RE, Ce) with excellent thermal conductivity is provided 3 (Al,Mn) 5 O 12 ) Due to Lu 3+ Ion radius ratio Y 3+ The ion radius is large, so that the LuAG matrix has better thermal shock resistance than the YAG matrix, and the spectrum of LuAG: Ce is red-shifted by doping Mn, RE and the like, so that white light can be emitted by mixing with blue light;
3) the grain size of the ceramic grains is relatively small by regulating and controlling the granularity of the raw material and the sintering method, so that the thermal shock resistance of the ceramic can be further improved;
4) the problems that the white light of the fluorescent material is not uniform and the thermal shock resistance of the fluorescent material is weak in the current white light laser illumination are effectively solved.
In addition to the technical problems addressed by the present invention, the technical features constituting the technical solutions, and the advantageous effects brought by the technical features of the technical solutions described above, other technical problems solved by the present invention, other technical features included in the technical solutions, and advantageous effects brought by the technical features will be described in further detail with reference to the accompanying drawings.
Drawings
Fig. 1 is a schematic diagram of a device for testing uniformity of light output.
FIG. 2 is a microscopic structural view of the ceramic composite body of the present invention.
FIG. 3 shows the excitation spectrum of the complex phase ceramic of the present invention.
FIG. 4 is an emission spectrum of the complex phase ceramic of the present invention.
FIG. 5 is a schematic view (transmissive type) of a light-emitting device comprising the complex phase ceramic of the present invention.
FIG. 6 is a schematic view of a light-emitting device (reflective type) comprising the complex phase ceramic of the present invention.
Detailed Description
The present invention will be described in further detail below with reference to specific embodiments and drawings. Here, the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Comparative example 1
Using high purity yttrium oxide (Y) 2 O 3 ) Alumina (Al) 2 O 3 ) Cerium oxide (CeO) 2 ) As raw materials, magnesium oxide (MgO) and Tetraethoxysilane (TEOS) are used as sintering aids. The addition amount of magnesium oxide (MgO) is 0.1 percent by mass, and the addition amount of Tetraethoxysilane (TEOS) is 0.6 percent by mass. Preparing a powder raw material according to the composition formula, then taking absolute ethyl alcohol as a ball milling medium, putting the ball milling medium into an alumina ball milling tank for wet ball milling to prepare ceramic powder, and drying, sieving and tabletting the powder; then the ceramic blank is applied with 200MPa cold isostatic pressing to form a blank body, the ceramic blank body is pre-sintered after being preserved for 4 hours at 700 ℃, and then is put into a vacuum sintering furnace at 1750 ℃ and the vacuum degree of 10 - 3 Sintering for 8 hours under the condition of Pa, and finally annealing for 20 hours at 1450 ℃ in a muffle furnace to obtain (Y) 0.99 Ce 0.01 ) 3 Al 5 O 12 And the obtained ceramic material is subjected to cutting, grinding and polishing processing to obtain the 0.3mm thick complex-phase fluorescent ceramic for white light illumination.
Example 1
According to (Lu) 0.96 Tb 0.03 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 Chemical proportioning scaleTaking high-purity yttrium oxide (Lu) 2 O 3 ) Alumina (Al) 2 O 3 ) Cerium oxide (CeO) 2 ) Terbium oxide (Tb) 4 O 7 ) Manganese oxide (MnO) 2 ) Selecting oxide dispersed phase Y as raw material 2 O 3 The content by volume of (D50: 0.5 μm) was 25%. Magnesium oxide (MgO) and Tetraethoxysilane (TEOS) are used as sintering aids, the addition amount of the magnesium oxide (MgO) is 0.1 percent of the total mass of the composite phase, and the addition amount of the Tetraethoxysilane (TEOS) is the first phase (Lu) 0.96 Tb 0.03 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 0.6% of the mass. According to the ceramic preparation process flow and parameters in the comparative example 1, the complex phase fluorescent ceramic with the thickness of 0.3mm for white light illumination is obtained.
Example 2
In this example, a liquid-phase coprecipitation method is used to synthesize fluorescent phase precursor powder (Lu) 0.96 Tb 0.03 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 The preparation method comprises the following steps: selecting Lu (NO) with purity of more than 99.9% 3 ) 3 、A1(NO 3 ) 3 、Ce(NO 3 ) 3 、Tb(NO 3 ) 3 、Mn(NO 3 ) 2 As raw material, with H 2 C 2 O 4 As a precipitant, calcining the precipitate at 700 ℃ for 4h to obtain nano oxide powder with good dispersion and large sintering activity; then adding a second phase Y with the volume fraction of 15 percent into the oxide precursor 2 O 3 Powder (D50 is 0.3 μm), and sintering aids of magnesium oxide (MgO) and Tetraethoxysilane (TEOS) are introduced, wherein the addition amount of the magnesium oxide (MgO) is 0.1 percent of the total mass of the composite phase, and the addition amount of the Tetraethoxysilane (TEOS) is (Lu) 0.96 Tb 0.03 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 0.6% of the mass. Preparing a powder raw material according to the composition formula, then taking absolute ethyl alcohol as a ball milling medium, putting the ball milling medium into an alumina ball milling tank for wet ball milling to prepare ceramic powder, and drying, sieving and tabletting the powder; then the ceramic blank is applied with 200MPa cold isostatic pressing to form a blank, the ceramic blank is pre-sintered after being preserved for 4 hours at 700 ℃,placing into a vacuum sintering furnace at 1800 ℃ and a vacuum degree of 10 -3 Sintering under Pa for 2 hours, cooling to 1720 ℃, preserving heat for 8 hours, and finally annealing at 1450 ℃ for 20 hours in a muffle furnace to obtain (Lu) 0.96 Tb 0.03 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 And Y 2 O 3 And cutting, grinding and polishing the obtained ceramic material to obtain the 0.3mm thick complex phase fluorescent ceramic for white light illumination.
Example 3
In this example, a liquid-phase coprecipitation method was used to synthesize fluorescent phase precursor powder (Lu) 0.84 Tb 0.15 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 The preparation method is the same as that of example 2; then adding a second phase Y with the volume fraction of 5 percent into the oxide precursor 2 O 3 Powder (D50 is 0.1 μm), and sintering aids of magnesium oxide (MgO) and Tetraethoxysilane (TEOS) are introduced, wherein the addition amount of the magnesium oxide (MgO) is 0.1 percent of the total mass of the composite phase, and the addition amount of the Tetraethoxysilane (TEOS) is the first phase (Lu) 0.84 Tb 0.15 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 0.4% of the mass. Preparing a powder raw material according to the composition formula, then taking absolute ethyl alcohol as a ball milling medium, putting the ball milling medium into an alumina ball milling tank for wet ball milling to prepare ceramic powder, and drying, sieving and tabletting the powder; then the ceramic blank is applied with 200MPa cold isostatic pressing to form a blank body, the ceramic blank body is pre-sintered after heat preservation for 4h at 700 ℃, and then is put into a vacuum sintering furnace at 1650 ℃ and the vacuum degree of 10 -3 Sintering for 5 hours under Pa, then sintering for 5 hours in a hot isostatic pressing furnace at 1550 ℃ and 200MPa, and finally annealing for 20 hours at 1450 ℃ in a muffle furnace to obtain (Lu) 0.84 Tb 0.15 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 And Y 2 O 3 And cutting, grinding and polishing the obtained ceramic material to obtain the 0.3mm thick complex phase fluorescent ceramic for white light illumination.
Example 4
This exampleSynthesizing fluorescent phase precursor powder (Lu) by liquid phase coprecipitation method 0.595 Tb 0.4 Ce 0.005 ) 3 (Al 0.992 Mn 0.008 ) 5 O 12 The preparation method is the same as example 2; then adding 10% volume fraction of a second phase Y to the oxide precursor 2 O 3 Powder (D50 is 0.1 μm), and sintering aids of magnesium oxide (MgO) and Tetraethoxysilane (TEOS) are introduced, wherein the addition amount of magnesium oxide (MgO) is 0.08% of the total mass of the composite phase and the addition amount of Tetraethoxysilane (TEOS) is the first phase (Lu) 0.595 Tb 0.4 Ce 0.005 ) 3 (Al 0.992 Mn 0.008 ) 5 O 12 0.4% of the mass. The powder raw materials are prepared according to the composition formula, the multiphase ceramic is prepared according to the same preparation process of the embodiment 3, and the obtained ceramic material is cut, ground and polished to obtain the multiphase fluorescent ceramic with the thickness of 0.3mm for white light illumination.
Example 5
In this example, a liquid-phase coprecipitation method is used to synthesize fluorescent phase precursor powder (Lu) 0.685 Tb 0.3 Ce 0.015 ) 3 (Al 0.988 Mn 0.012 ) 5 O 12 The preparation method is the same as example 2; then, a 20% volume fraction of the second phase Y is added to the oxide precursor 2 O 3 Powder (D50 is 0.3 μm), and sintering aids of magnesium oxide (MgO) and Tetraethoxysilane (TEOS) are introduced, wherein the addition amount of magnesium oxide (MgO) is 0.12% of the total mass of the composite phase, and the addition amount of Tetraethoxysilane (TEOS) is the first phase (Lu) 0.685 Tb 0.3 Ce 0.015 ) 3 (Al 0.988 Mn 0.012 ) 5 O 12 0.4% of the mass. The powder raw materials are prepared according to the composition formula, the multiphase ceramic is prepared according to the same preparation process of the embodiment 3, and the obtained ceramic material is cut, ground and polished to obtain the multiphase fluorescent ceramic with the thickness of 0.3mm for white light illumination.
Table 1 shows the composite ceramic components, preparation process parameters and luminous intensities thereof in comparative examples and examples 1 to 5
Figure BDA0001537519310000081
Figure BDA0001537519310000091
The main preparation process parameters and light extraction uniformity of the fluorescent ceramics of these examples are shown in Table 1. Compared with the comparative example, the light-emitting uniformity testing device and method shown in fig. 1 have the advantages that the illuminance variances of different areas in examples 1-5 are obviously improved, the light-emitting uniformity in example 5 is better, and the illuminance mean value in example 3 is improved by 6%. As can be seen from the electron scanning electron micrograph of FIG. 2, the fluorescent phase and the astigmatic phase are uniformly distributed, and the grain size is about 2 to 3 μm; as can be seen from FIGS. 3 to 4, the optimal excitation wavelength of the fluorescent ceramic is 450 to 465nm, the fluorescent ceramic has a broad emission peak at 568nm, and yellow-orange light emission is presented. Referring to fig. 5 to 6, the bottom surface of the ceramic composite is plated with silver and soldered in a copper heat dissipation base 5, so that white light illumination can be realized through a transmission-type or reflection-type light path. The method comprises the steps of utilizing a single or multiple lasers 1 as excitation light sources, collimating, bunching and homogenizing the light by a lens 2 and then irradiating the light on the surface of a ceramic composite body 4, converting the wavelength 6 of the excitation light sources into orange light by the ceramic composite body, and mixing the residual blue light with the emitted light of a ceramic chip to obtain uniform white light 7 with high brightness and the color rendering index Ra being more than 85.
The foregoing merely represents embodiments of the present invention, which are described in some detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (6)

1. The complex phase fluorescent ceramic for white light illumination is characterized by comprising a lutetium aluminum garnet fluorescent phase and an oxide dispersed phase, wherein the relative volume fraction content of the oxide dispersed phase is 0.001-30%, and the oxide dispersed phase is uniformly distributed in a grid structure of the lutetium aluminum garnet fluorescent phase;
the lutetium aluminum garnet fluorescent phase is (Lu) 0.96 Tb 0.03 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 、(Lu 0.84 Tb 0.15 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 、(Lu 0.595 Tb 0.4 Ce 0.005 ) 3 (Al 0.992 Mn 0.008 ) 5 O 12 Or (Lu) 0.685 Tb 0.3 Ce 0.015 ) 3 (Al 0.988 Mn 0.012 ) 5 O 12 (ii) a The oxide light-dispersing phase is Y 2 O 3
2. The preparation method of the complex phase fluorescent ceramic for white light illumination is characterized by comprising the following steps,
step S1, weighing raw materials and sintering aids: the raw materials are phosphor powder precursor and oxide light-dispersing phase powder, the phosphor powder precursor is (Lu) 0.96 Tb 0.03 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 、(Lu 0.84 Tb 0.15 Ce 0.01 ) 3 (Al 0.99 Mn 0.01 ) 5 O 12 、(Lu 0.595 Tb 0.4 Ce 0.005 ) 3 (Al 0.992 Mn 0.008 ) 5 O 12 Or (Lu) 0.685 Tb 0.3 Ce 0.015 ) 3 (Al 0.988 Mn 0.012 ) 5 O 12 (ii) a The oxide light-dispersing powder is Y 2 O 3 (ii) a The sintering aid is magnesium oxide MgO and tetraethoxysilane TEOS;
step S2, ball milling and mixing;
step S3, drying and sieving;
step S4, tabletting and forming;
step S5, sintering into ceramic blocks;
and step S6, annealing to obtain the complex phase fluorescent ceramic.
3. The method for preparing a complex phase fluorescent ceramic for white light illumination as claimed in claim 2, wherein in step S5, the complex phase fluorescent ceramic is sintered in one step by atmosphere sintering: the sintering heat preservation temperature is 1650-1800 ℃, and the heat preservation time is 1-20 hours.
4. The method of claim 2, wherein in step S5, the ceramic is prepared by vacuum two-step sintering: in a vacuum furnace, the vacuum degree is 10 -2 ~10 -4 Pa, firstly, the sintering temperature is increased to 1780-1820 ℃ in the first step, the sintering heat preservation time is 0.5-5 h, and secondly, the sintering temperature is decreased to 1680-1780 ℃, and the sintering heat preservation time is 1-30 h.
5. The method of claim 2, wherein in step S5, the sintering is performed by two steps of vacuum and hot isostatic pressing: the first step is sintering in a vacuum furnace with a vacuum degree of 10 -2 ~10 -4 Pa, the heat preservation temperature is 1700-1800 ℃, the sintering heat preservation time is 3-6 h, and in the second step, the ceramic block body obtained in the first step is placed into a hot isostatic pressing furnace for sintering, the pressure is 150-200 MPa, the heat preservation temperature is 1600-1700 ℃, and the heat preservation time is 1-10 h.
6. The light source device is characterized by comprising,
a blue light exciter; and the number of the first and second groups,
the complex phase fluorescent ceramic of claim 1.
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