CN110395977B - Preparation method of polycrystalline block material for optical wavelength conversion - Google Patents
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Abstract
A method of preparing a polycrystalline bulk material for light wavelength conversion, comprising: the method comprises the following steps: 1) weighing aluminum oxide, yttrium oxide and cerium oxide as raw materials according to the chemical proportion of a garnet structure, and mixing the raw materials: alcohol: ball-milling and uniformly mixing the balls according to the mass ratio of 1:1.5:5, and drying to obtain initial raw material powder; 2) sieving the initial raw material powder by using a screen to obtain powder with different particle sizes, and combining the powder with a fine particle size and the powder with a coarse particle size according to a certain proportion after sieving to obtain powder for molding; 3) the powder for molding is pressed into a block by dry pressing and then a cold isostatic pressing process to obtain a block biscuit; 4) and adding a sintering aid into the block biscuit in a vacuum atmosphere, and sintering at a low temperature to finally obtain the polycrystalline block material with submicron grains. The invention can improve the light extraction efficiency of the polycrystalline block material for optical wavelength conversion, has relatively simple process, effectively controls the cost and is beneficial to large-scale industrial production.
Description
Technical Field
The invention belongs to the field of preparation of polycrystalline block materials, and particularly relates to a preparation method of a polycrystalline block material for optical wavelength conversion.
Background
The high refractive index of the inside of so-called polycrystalline bulk materials, such as ceramics, glasses, causes a serious problem: when light enters the material from the air, the total reflection phenomenon occurs due to the change of the refractive index, the efficiency (escape rate) of the light from the material to the air is low, and more light escapes from the side surface after the total reflection, so that the optical waveguide phenomenon is caused. This phenomenon can be explained in the field of white light semiconductor lighting, for example: the blue light semiconductor light source is used to excite the fluorescent materials with different emission wave bands to be converted into green light, yellow light, red light and the like, and the blue light and the light are mixed according to a certain proportion to obtain the white light source. As mentioned above, if the fluorescent material is not a powder material but a block material, the excitation light is affected by the total reflection phenomenon in the block fluorescent material, the vertical light extraction efficiency of the front surface is low, and the phenomenon that the excitation light overflows from the side surface is serious, so that the spatial distribution of the white light color is extremely uneven, and the performance and the secondary optical light distribution of the white light source are seriously affected.
In order to improve the extraction efficiency of excitation light, research is currently focused mainly on surface treatment of light conversion materials in the field of bulk fluorescent materials.
One approach is to change the geometry of the exit face of the block material: the original plane is changed into a convex curved surface (spherical surface or ellipsoid surface, etc.). Although the method does not change the total reflection performance of the material, the method can reduce the exit angle of light and reduce the probability of total reflection of the light. For example, chinese patent publication nos. CN201766096U and CN202423281U disclose a light conversion bulk material.
The disadvantages of this solution are:
1: the method has limited improvement effect;
2: the curved surface is manufactured by the plane, the process is complex, the period is long, the material loss rate is high, the manufacturing cost is greatly improved, and the large-scale industrial production and application are not facilitated.
Patent CN101904020A applied by royal philips electronics ltd discloses a photonic crystal structure on the surface of a light conversion material, which improves the light escape efficiency by forming a periodic structure on the surface to form diffracted light. This method of changing the microstructure of the surface of the bulk material can better improve the light extraction efficiency.
The disadvantages of this solution are:
the biggest defects of the method for regulating and controlling the microstructure of the constructed photonic crystal are that the demand on equipment is high, the process is complex, the manufacturing cost is greatly improved, and the method is not beneficial to industrial production and application.
Disclosure of Invention
The invention provides a preparation method of a polycrystalline block material for optical wavelength conversion, aiming at solving the defects of the prior art, improving the light extraction efficiency, ensuring that the process is relatively simple, effectively controlling the cost and being beneficial to large-scale industrial production.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method of preparing a polycrystalline bulk material for light wavelength conversion, comprising: the method comprises the following steps:
1) weighing aluminum oxide, yttrium oxide and cerium oxide as raw materials according to the chemical proportion of a garnet structure, and mixing the raw materials: alcohol: the mass ratio of the balls is 1:1.5:5, the balls are uniformly mixed by ball milling, and the initial raw material powder is obtained by drying;
2) sieving the initial raw material powder by using a screen to obtain powder with different particle sizes, and combining the powder with a fine particle size and the powder with a coarse particle size according to a certain proportion after sieving to obtain powder for molding;
3) the powder for molding is pressed into a block by dry pressing and then a cold isostatic pressing process, the applied pressure is 200-300MPa, and the block biscuit is obtained by degreasing in oxygen atmosphere at 600-800 ℃;
4) and adding a sintering aid into the block biscuit in a vacuum atmosphere, and sintering at a low temperature to finally obtain the polycrystalline block material with submicron grains.
Further: the specification of the screen mesh for sieving and sieving the powder in the step 2) is 50-150 microns.
Further: the combined proportion of the fine particle size powder and the coarse particle size powder in the powder for forming in the step 2) is a mass ratio (70-100%): (0-30%).
Further: the sintering aid added in the step 4) is one or more of magnesium oxide, calcium oxide and tetraethoxysilane.
Further: in the step 4), performing ceramic densification on the block biscuit in a vacuum atmosphere by using one or a combination of methods of spark plasma sintering, scintillation sintering, vibration hot-pressing sintering or hot isostatic pressing sintering; the sintering temperature is 1450-1750 ℃, and the heat preservation time is 0.2-10 h.
Further: the density of the polycrystalline block material with submicron crystal grains obtained in the step 4) is 90-99%, and the size of the crystal grains is 0.05-1 μm.
The invention has the advantages that:
1. the phenomenon of side light overflow of exciting light converted by a fluorescent polycrystalline block material is solved, and the light emitting color is uniform;
2. the light intensity of the light source in the vertical direction is improved, the light source is a Lambert body light source, and the Lambert body light source is expressed as a radiation source which radiates by itself and has unchanged radiation brightness in all directions;
3. by controlling the grain size of the polycrystalline ceramic, the scattering effect of the exciting light of the polycrystalline ceramic is realized, and compared with the modification of the ceramic surface, the uniformity, the process simplification degree and the economic effect of the polycrystalline ceramic are greatly improved.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is an SEM image of a polycrystalline bulk material obtained by the present invention;
FIG. 2 is a graph of the spatial angular distribution of color temperature for a white light emitting diode device encapsulated with a polycrystalline bulk material that has been wavelength converted;
fig. 3 is a graph of the spatial angular distribution of color temperature for a white light emitting diode device encapsulated with a polycrystalline bulk material that has been wavelength converted.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the drawings used in the description will be briefly introduced, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other embodiments can be obtained according to the drawings without inventive labor.
Example 1:
the invention relates to a preparation method of a polycrystalline block material for optical wavelength conversion, which comprises the following steps:
1) weighing aluminum oxide, yttrium oxide and cerium oxide as raw materials according to the chemical proportion of a garnet structure, and mixing the raw materials: alcohol: the mass ratio of the balls is 1:1.5:5, the balls are uniformly mixed by ball milling, and the initial raw material powder is obtained by drying;
2) sieving the initial raw material powder by using a 50-micron sieve to obtain powder with different coarse and fine particle sizes, wherein the sieved powder is fine particle size powder, the powder remained in the sieve is coarse particle size powder, and the mass ratio of the fine particle size powder to the coarse particle size powder is 70% after sieving: 30 percent of the powder for molding is obtained;
3) the powder for molding is pressed into a block by dry pressing and then a cold isostatic pressing process, the applied pressure is 200MPa, and the block biscuit is obtained by degreasing in oxygen atmosphere at 600 ℃;
4) and adding magnesium oxide as a sintering aid into the block biscuit in a vacuum atmosphere, performing spark plasma sintering, and performing ceramic densification at the sintering temperature of 1450 ℃ for 0.2h to finally obtain the polycrystalline block material with submicron grains, wherein the density of the obtained polycrystalline block material with the submicron grains is 90-99%, and the grain size is 0.05-1 mu m.
Example 2:
the invention relates to a preparation method of a polycrystalline block material for optical wavelength conversion, which comprises the following steps:
1) weighing aluminum oxide, yttrium oxide and cerium oxide as raw materials according to the chemical proportion of a garnet structure, and mixing the raw materials: alcohol: the mass ratio of the balls is 1:1.5:5, the balls are uniformly mixed by ball milling, and the initial raw material powder is obtained by drying;
2) sieving the initial raw material powder by using an 80-micron sieve to obtain powder with different coarse and fine particle sizes, wherein the sieved powder is fine particle size powder, the powder remained in the sieve is coarse particle size powder, and the mass ratio of the fine particle size powder to the coarse particle size powder is 80% after sieving: 20 percent of the powder is combined to obtain powder for molding;
3) the powder for molding is pressed into a block by dry pressing and then a cold isostatic pressing process, the applied pressure is 250MPa, and the block biscuit is obtained by degreasing in the oxygen atmosphere at 700 ℃;
4) and adding calcium oxide as a sintering aid into the block biscuit in a vacuum atmosphere, carrying out flash sintering, and carrying out ceramic densification, wherein the sintering temperature is 1550 ℃, and the heat preservation time is 1h, so as to finally obtain the polycrystalline block material with submicron grains, wherein the density of the obtained polycrystalline block material with submicron grains is 90-99%, and the grain size is 0.05-1 mu m.
Example 3:
the invention relates to a preparation method of a polycrystalline block material for optical wavelength conversion, which comprises the following steps:
1) weighing aluminum oxide, yttrium oxide and cerium oxide as raw materials according to the chemical proportion of a garnet structure, and mixing the raw materials: alcohol: the mass ratio of the balls is 1:1.5:5, the balls are uniformly mixed by ball milling, and the initial raw material powder is obtained by drying;
2) sieving the initial raw material powder by using a 100-micron sieve to obtain powder with different coarse and fine particle sizes, wherein the sieved powder is fine particle size powder, the powder remained in the sieve is coarse particle size powder, and the mass ratio of the fine particle size powder to the coarse particle size powder is 90%: 10 percent of the mixture is combined to obtain powder for molding;
3) the powder for molding is pressed into a block by dry pressing and then a cold isostatic pressing process, the applied pressure is 250MPa, and the block biscuit is obtained by degreasing in the oxygen atmosphere at 700 ℃;
4) and adding tetraethoxysilane as a sintering aid into the block biscuit in a vacuum atmosphere, vibrating, hot-pressing and sintering to perform ceramic densification, wherein the sintering temperature is 1600 ℃, and the heat preservation time is 2 hours, so that the polycrystalline block material with submicron grains is finally obtained, the density of the obtained polycrystalline block material with submicron grains is 90-99%, and the grain size is 0.05-1 mu m.
Example 4:
the invention relates to a preparation method of a polycrystalline block material for optical wavelength conversion, which comprises the following steps:
1) weighing aluminum oxide, yttrium oxide and cerium oxide as raw materials according to the chemical proportion of a garnet structure, and mixing the raw materials: alcohol: the mass ratio of the balls is 1:1.5:5, the balls are uniformly mixed by ball milling, and the initial raw material powder is obtained by drying;
2) sieving the initial raw material powder by using a 100-micron sieve to obtain powder with different coarse and fine particle sizes, wherein the sieved powder is fine particle size powder, the powder remained in the sieve is coarse particle size powder, and the mass ratio of the fine particle size powder to the coarse particle size powder is 100% after sieving: 0 percent of the mixture is combined to obtain powder for molding;
3) the powder for molding is pressed into a block by dry pressing and then a cold isostatic pressing process, the applied pressure is 300MPa, and the block biscuit is obtained by degreasing in an oxygen atmosphere at 800 ℃;
4) adding magnesium oxide and calcium oxide as sintering aids into the block biscuit in a vacuum atmosphere, carrying out hot isostatic pressing sintering, and carrying out ceramic densification, wherein the sintering temperature is 1700 ℃, and the heat preservation time is 4 hours, so as to finally obtain the polycrystalline block material with submicron grains, wherein the density of the obtained polycrystalline block material with submicron grains is 90-99%, and the grain size is 0.05-1 μm.
Example 5:
the invention relates to a preparation method of a polycrystalline block material for optical wavelength conversion, which comprises the following steps:
1) weighing aluminum oxide, yttrium oxide and cerium oxide as raw materials according to the chemical proportion of a garnet structure, and mixing the raw materials: alcohol: the mass ratio of the balls is 1:1.5:5, the balls are uniformly mixed by ball milling, and the initial raw material powder is obtained by drying;
2) sieving the initial raw material powder by using a 100-micron sieve to obtain powder with different coarse and fine particle sizes, wherein the sieved powder is fine particle size powder, the powder remained in the sieve is coarse particle size powder, and the mass ratio of the fine particle size powder to the coarse particle size powder is 70% after sieving: 30 percent of the powder for molding is obtained;
3) the powder for molding is pressed into a block by dry pressing and then a cold isostatic pressing process, the applied pressure is 250MPa, and the block biscuit is obtained by degreasing in the oxygen atmosphere at 700 ℃;
4) and adding calcium oxide and tetraethoxysilane as sintering aids into the block biscuit in a vacuum atmosphere, performing spark plasma sintering, performing ceramic densification, wherein the sintering temperature is 1750 ℃, and the heat preservation time is 10 hours, so as to finally obtain the polycrystalline block material with submicron grains, wherein the density of the obtained polycrystalline block material with the submicron grains is 90-99%, and the grain size is 0.05-1 mu m.
As shown in fig. 1:
SEM of polycrystalline bulk material shows a honeycomb structure, i.e. a polycrystalline structure composed of a combination of single crystal grains of different orientations. The grain size is the proper size mentioned in the invention, namely the grain size is 0.05-1 μm, and the self-scattering property is provided.
As shown in fig. 2:
As shown in fig. 3:
curves 3 and 4 show the spatial angular distribution of color temperature of white light emitting diode devices packaged with the polycrystalline bulk material using light wavelength conversion. The grain size of the optical wavelength-converted polycrystalline bulk material used in curve 3 is 1 μm or more, and the grain size of the optical wavelength-converted polycrystalline bulk material used in curve 4 is 0.05 to 1 μm, which is the solution disclosed in this patent. As is apparent from FIG. 3, the light intensity in the vertical direction of the light source is improved, and the light source is a Lambertian light source which is expressed as a radiation source which radiates by itself and has constant radiation brightness in all directions.
The idea of the invention is to modify the material itself from a block material and to eliminate the total reflection phenomenon from the interior of the material.
Polycrystalline material means that the interior of the material is composed of single crystal tiny grains which are randomly arranged in different directions, when the size of the grains is equal to the size of light wavelength, the Mie scattering condition is satisfied, and light generates strong scattering characteristics at the grain boundary.
The self-scattering performance is generated by regulating and controlling the microscopic grain size of the polycrystalline block conversion material, light is scattered in the conversion material and is emitted into the air, the light is uniformly distributed in space, and the emission efficiency is high. The method does not perform complex processing treatment on the surface of the conversion material, but generates self-scattering characteristics in the material by changing the internal microstructure of the material, so that the light extraction efficiency is improved to the maximum extent fundamentally, the process is relatively simple, the cost is effectively controlled, and the method is favorable for large-scale industrial production.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (1)
1. A method of preparing a polycrystalline bulk material for light wavelength conversion, comprising: the method comprises the following steps:
1) weighing aluminum oxide, yttrium oxide and cerium oxide as raw materials according to the chemical proportion of a garnet structure, and mixing the raw materials: alcohol: the mass ratio of the balls is 1:1.5:5, the balls are uniformly mixed by ball milling, and the initial raw material powder is obtained by drying;
2) sieving the initial raw material powder by using a screen to obtain powder with different particle sizes, and combining the powder with a fine particle size and the powder with a coarse particle size according to a certain proportion after sieving to obtain powder for molding; the specification of a screen mesh for sieving and sieving the powder is 50-150 microns; the combined proportion of the fine particle size powder and the coarse particle size powder in the powder for molding is 70-100 percent by mass: (0-30%);
3) the powder for molding is pressed into a block by dry pressing and then a cold isostatic pressing process, the applied pressure is 200-300MPa, and the block biscuit is obtained by degreasing in oxygen atmosphere at 600-800 ℃;
4) adding a sintering aid into the block biscuit in a vacuum atmosphere, and sintering at a low temperature to finally obtain a polycrystalline block material with submicron crystal grains; the added sintering aid is one or more of magnesium oxide, calcium oxide and tetraethoxysilane; performing ceramic densification on the block biscuit in a vacuum atmosphere by using one or a combination of methods of spark plasma sintering, flash sintering, vibration hot pressing sintering or hot isostatic pressing sintering; the sintering temperature is 1450-1750 ℃, and the heat preservation time is 0.2-10 h; the density of the obtained submicron-grain polycrystalline block material is 90-99%, and the grain size is 0.05-1 μm.
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| CN102924073A (en) * | 2012-11-16 | 2013-02-13 | 北京雷生强式科技有限责任公司 | Method for preparing rare earth ion-doped yttrium aluminum garnet (Re: YAG) transparent laser ceramic by using hot-pressing post treatment |
| CN104685024A (en) * | 2012-12-06 | 2015-06-03 | 常耀辉 | Luminescent material for solid-state sources of white light |
| CN104177079A (en) * | 2014-07-17 | 2014-12-03 | 江苏诚赢照明电器有限公司 | Ce:YAG based transparent ceramic being used for fluorescence conversion of white LED and containing Sr and preparation method thereof |
| CN107129293A (en) * | 2017-06-08 | 2017-09-05 | 江苏师范大学 | A kind of preparation method of Mg adjuvant systems YAG base transparent ceramics |
| CN107915481A (en) * | 2017-11-22 | 2018-04-17 | 中国科学院过程工程研究所 | A kind of nanostructured Yt aluminum garnet-base transparent ceramic material, preparation method and the usage |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024019940A3 (en) * | 2022-07-21 | 2024-02-29 | Heraeus Conamic North America Llc | Process for sintering yag layers |
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