CN108695422B - Light emitting device and method for manufacturing the same - Google Patents
Light emitting device and method for manufacturing the same Download PDFInfo
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- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
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- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
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- H—ELECTRICITY
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- H01L33/50—Wavelength conversion elements
- H01L33/507—Wavelength conversion elements the elements being in intimate contact with parts other than the semiconductor body or integrated with parts other than the semiconductor body
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Abstract
The invention provides a light-emitting device and a preparation method thereof, wherein the components comprise fluorescent powder and a binder for binding, and the light-emitting device is an integral sintered body comprising a light-emitting layer and a functional layer laminated on the light-emitting layer; the luminescent layer comprises a first luminescent layer, the mass fraction of fluorescent powder in the first luminescent layer is 50-99%, and the thickness of the first luminescent layer is 150-200 mu m; the functional layer comprises a first functional layer, the mass fraction of fluorescent powder in the first functional layer is 5% -50%, and the thickness of the first functional layer is 5-50 μm; a continuous compact transition layer is arranged between the luminous layer and the functional layer; the phosphor has a different Mohs hardness than the binder. The invention solves the problem that the polishing flatness of the complex phase material light-emitting device is inconsistent and the coating is difficult, and simultaneously, the porosity between layers is low, thereby further avoiding the sintering separation phenomenon and improving the reliability and the finished product yield of the light-emitting device.
Description
Technical Field
The invention belongs to the technical field of optics, and particularly relates to a light-emitting device and a preparation method thereof.
Background
In recent years, with the rapid development of high-quality green lighting and high-end display technologies, the application of high-energy-density excitation methods such as Laser Semiconductors (LDs), high-power white LEDs, etc. has made higher requirements on the radiation resistance and structural stability of fluorescent materials, and Light wavelength conversion materials using fluorescent powder and silica gel as main raw materials have been widely applied to laser Light sources and LED (Light Emitting Diode) Light sources. With the increasing requirements of people on brightness, the optical power of the exciting light is higher and higher, and the optical wavelength conversion sheet prepared from the fluorescent powder and the silica gel is difficult to meet the application requirements in the aspects of high temperature resistance and heat conduction.
Currently, light wavelength conversion materials, such as luminescent glass, prepared from glass powder (or alumina powder) and YAG phase phosphor as main raw materials, wherein the glass powder is used as a transparent bonding medium and the YAG phase phosphor is used as a light emitter, have been gradually applied to high-power LEDs and laser light sources. However, the prepared complex phase phosphor needs to be ground, polished and the like during application. Because the Mohs hardness of the glass powder (or alumina powder) is different from that of the YAG-phase fluorescent powder, and the abrasion rates of the glass powder (or alumina powder) and the YAG-phase fluorescent powder are different under the same grinding condition, after grinding and polishing, the surface of the light-emitting device has a 'relief' phenomenon, so that a plurality of process problems exist in a later coating process.
In addition, in the related art, a method for preparing luminescent ceramics with gradient concentration is adopted, namely, one end face of porous ceramics is immersed in a fluorescent substance solution, the fluorescent substance solution enters the ceramics under the action of capillary siphon, and then the luminescent ceramics with different concentration gradients are prepared by heat treatment.
Or, the paste printing method is adopted to manufacture the light-emitting device with the gradient concentration structure, a great amount of organic carriers (such as resin, auxiliary agent, solvent and the like) are added into the fluorescent powder with different concentrations and the sintering binding material together to prepare printable paste, and then the layer-by-layer printing is carried out, so that when the next layer is printed between each layer, the operation can be carried out after the previous layer is required to be pre-baked, dried and cured, in order to remove small molecular organic matters (the solvent with low boiling point and the auxiliary agent), the surface of the interface between the two concentrations is uneven due to the printing of the particle paste, and the combination of the two is that the organic carrier in the second concentration layer flows into or permeates into the dry surface of the first concentration layer, so that the liquid organic carrier and the solid material with small particles are mainly enriched at the interface; after entering a sintering process, when reaching a certain temperature section, organic matter macromolecules begin to be decomposed into micromolecules and volatilize, and each concentration layer begins to shrink; with the further increase of the temperature, the resin starts to decompose and gasify, and at this time, defects such as holes and pore canals are formed in the position space occupied by the organic resin originally; as the temperature continues to rise, the material of the bonding medium begins to melt and gradually changes into a liquid phase, flows between the holes and the pore channels formed before, and then the volume of each concentration layer begins to further shrink, the liquid phase of the bonding medium fills most of the holes and the pore channels; the pore channels which cannot be filled form open pores, and the pores are the same as the outside, have the greatest harm to the polishing processing of ceramics and cannot be completely removed by processing. The phenomenon is more obvious and cracking is seriously caused because the organic carrier medium is gathered in the first concentration plane and the second concentration plane; the disadvantages of this process are high porosity and low density.
Therefore, there is a need to provide a new light emitting device and a method for manufacturing the same to solve the above problems.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the light-emitting device with gradient concentration, and the low-concentration layer is designed by controlling the mass fraction and distribution of the fluorescent material in each layer, so that the problem of difficult increase of a coating process caused by a coating interface 'relief' structure generated by different hardness of the luminescent material and a bonding medium in the prior art is solved; on the other hand, the porosity among the interfaces of each concentration layer of the structure is low, the condition of overlarge concentration difference does not exist, and the quality problems of cracking, stripping, falling and the like caused by large expansion coefficient difference in the sintering process are avoided;
the invention provides a light-emitting device, which comprises fluorescent powder and a binder for binding, wherein the light-emitting device is an integral sintered body comprising a light-emitting layer and a functional layer laminated on the light-emitting layer; the light-emitting layer comprises a first light-emitting layer, the mass fraction of fluorescent powder in the first light-emitting layer is 50% -99%, and the thickness of the first light-emitting layer is 150-200 mu m; the functional layer comprises a first functional layer, the mass fraction of fluorescent powder in the first functional layer is 5% -50%, and the thickness of the first functional layer is 5-50 μm; a continuous compact transition layer is arranged between the luminous layer and the functional layer; the phosphor and the binder have different Mohs hardness.
Preferably, the first functional layer is formed by laminating at least two first sub-functional layers, a continuous and compact transition layer is arranged between each first sub-functional layer, the mass fraction of the phosphor in each first sub-functional layer increases progressively with a specific gradient along the direction extending from the first functional layer to the first light-emitting layer, and the specific gradient ranges from 5% to 10%; and the fluorescent powder in each first sub-functional layer is uniformly distributed.
Preferably, the first light-emitting layer is formed by laminating at least two first sub-light-emitting layers, a continuous and compact transition layer is arranged between each first sub-light-emitting layer, the mass fraction of the phosphor in each first sub-light-emitting layer increases progressively with a specific gradient along the direction extending from the first functional layer to the first light-emitting layer, and the specific gradient ranges from 5% to 10%; and the fluorescent powder in each first sub-luminous layer is uniformly distributed.
Preferably, the first functional layer is formed by laminating at least two first sub-functional layers, a continuous and compact transition layer is arranged between each first sub-functional layer, the mass fraction of the phosphor in each first sub-functional layer increases progressively with a specific gradient along the direction extending from the first functional layer to the first light-emitting layer, and the specific gradient ranges from 5% to 10%; the fluorescent powder in each first sub-functional layer is uniformly distributed; the first light-emitting layer is formed by laminating at least two first sub light-emitting layers, a continuous and compact transition layer exists between every two first sub light-emitting layers, the mass fraction of fluorescent powder in each first sub light-emitting layer in the first light-emitting layers is increased progressively by the same specific gradient, and the fluorescent powder in each first sub light-emitting layer is uniformly distributed; the mass fraction difference of the fluorescent powder in the adjacent first sub-luminous layer and the first sub-functional layer is 0 or the specific gradient.
Preferably, the porosity of the transition layer is 2% to 6.4%.
Preferably, an optical coating is disposed on the first functional layer at a side away from the first light emitting layer, and the optical coating includes a reflective film and an antireflection film.
Preferably, the functional layer further comprises a second functional layer, the second functional layer is laminated on the first functional layer and far away from the first light-emitting layer, and forms an integral sintered body with the first functional layer, the mass fraction of fluorescent powder in the second functional layer is 0, the thickness of the second functional layer is 0.1-5 μm, and a continuous and compact transition layer is arranged between the second functional layer and the first functional layer.
Preferably, the functional layer further comprises a third functional layer stacked on the first light-emitting layer and away from the first functional layer and a fourth functional layer stacked on the third functional layer and away from the first light-emitting layer, the mass fraction of the phosphor in the third functional layer is 5-50%, and the thickness of the third functional layer is 5-50 μm; the mass fraction of the fluorescent powder in the fourth functional layer is 0, and the thickness of the fourth functional layer is 0.1-5 μm; a continuous and compact transition layer is arranged between the first light-emitting layer and the third functional layer; and the continuous and compact transition layer is arranged between the fourth functional layer and the third functional layer.
Preferably, the fluorescent powder is Y3Al5O12:Ce3+Phosphor or Lu3Al5O12:Ce3+Fluorescent powder; the binder is glass powder or alumina powder or Y3Al5O12Powder or Lu3Al5O12And (3) pulverizing.
The invention also provides a preparation method of the light-emitting device, which comprises the following steps:
step S1: mixing materials; ball-milling the binder to obtain a ball-milled blank; adding fluorescent powder into the ball-milling blank, and continuously performing ball milling to obtain a mixed primary material;
step S2: charging; filling the mixed initial material into a mould;
step S3: pre-pressing; pre-pressing the mixed initial material in the die to obtain a pre-formed blank body;
step S4: sintering; carrying out cold isostatic pressing treatment on the pre-formed blank to obtain a biscuit, and sintering the biscuit to obtain the light-emitting device;
the step S1 further includes dividing the mixed blank into at least two parts including a first part and a second part, wherein the mass ratio of the binder added to the first part is 1:1 or 99:1, adding the fluorescent powder into the second part, wherein the mass ratio of the fluorescent powder to the binder in the second part is 1:19, and respectively continuing ball milling to obtain a first mixed initial material and a second mixed initial material; the step S2 is specifically to sequentially load the first mixed starting material and the second mixed starting material into the mold; the biscuit obtained in the step S4 includes a luminescent biscuit layer containing 50% or 99% by mass of phosphor and a functional biscuit layer containing 5% by mass of phosphor, and the thickness of the luminescent biscuit layer is greater than that of the functional biscuit layer.
Compared with the prior art, the light-emitting device and the preparation method thereof have different concentrations, even gradient different concentrations, and form a low-concentration layer on which a coating is polished. Because the hardness of the phosphor and the bonding medium are different, different wear states occur during polishing of the high-concentration layer, and 'emboss' is formed. And the low-concentration layer has less or no fluorescent powder, and the polished surface is relatively flat, thereby being convenient for coating. The invention solves the problem that the surface of the light-emitting device of the complex phase material is seriously uneven after being polished due to the hardness difference of two-phase media by adjusting the content of the fluorescent powder of the low-concentration layer, and the processing is simple and convenient; because the content of the fluorescent powder in the light-emitting device directly influences the light-emitting efficiency of the light-emitting device, the light-emitting device ensures the fluorescence efficiency of a main body and adjusts the proper gradient concentration on a shallow surface layer, so that the polished surface is close to a pure phase, and the polishing defect of the surface is reduced; meanwhile, the concentration of the fluorescent powder of each layer is controllable, so that the separation phenomenon of different concentration layers caused by inconsistent volume shrinkage during sintering is avoided.
Drawings
The present invention will be described in detail below with reference to the accompanying drawings. The foregoing and other aspects of the invention will become more apparent and more readily appreciated from the following detailed description, taken in conjunction with the accompanying drawings. In the drawings:
FIG. 1 is a schematic structural diagram of a light-emitting device according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a second light-emitting device according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of a light-emitting device according to a third embodiment of the present invention;
FIG. 4 is a schematic diagram of a fourth structure of a light-emitting device according to an embodiment of the present invention;
FIG. 5 is a schematic structural diagram of a light-emitting device according to a fifth embodiment of the present invention;
FIG. 6 is a schematic diagram of a sixth structure of a light-emitting device according to an embodiment of the present invention;
FIG. 7 is a block flow diagram of a method of making a light emitting device according to the present invention;
fig. 8 is a flow chart of the material mixing step in fig. 7.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
The embodiments/examples described herein are specific embodiments of the present invention, are intended to be illustrative of the concepts of the present invention, are intended to be illustrative and exemplary, and should not be construed as limiting the embodiments and scope of the invention. In addition to the embodiments described herein, those skilled in the art will be able to employ other technical solutions which are obvious based on the disclosure of the claims and the specification of the present application, and these technical solutions include those which make any obvious replacement or modification of the embodiments described herein, and all of which are within the scope of the present invention.
Example one
Referring to fig. 1, the present invention provides a light emitting device 10, which comprises phosphor and a binder for binding.
In this embodiment, the phosphor is commercially available Y3Al5O12:Ce3+Fluorescent powder; the binder is glass powder or alumina powder or Y3Al5O12The powder mainly plays a role in binding other components. The hardness of the binder is different from that of the fluorescent powder, such as: the Mohs hardness of the glass powder is 5.5-6, the Mohs hardness of the fluorescent powder is 8-8.5, and the Mohs hardness of the alumina powder is 9. The light-emitting device of the present invention is designed with a low concentration layer on which a plating film can be polished. Because the hardness of the phosphor and the bonding medium are different, different wear states occur during polishing of the high-concentration layer, and 'emboss' is formed. And the low-concentration layer has less or no fluorescent powder, and the polished surface is relatively flat, thereby being convenient for coating.
The light emitting device 10 is designed by adopting a differential concentration ratio method to perform tablet sintering, and is an integral sintered body comprising a light emitting layer 11 and a functional layer 12 laminated on the light emitting layer 11.
The light-emitting layer 11 comprises a first light-emitting layer 111, and the mass fraction of the fluorescent powder in the first light-emitting layer 111 is 50-99%. Since the first light emitting layer 111 generally serves as a main wavelength conversion layer, the inventor experimentally found that the luminous efficacy increases with the increase of the thickness of the first light emitting layer 111 when the concentration of the fluorescent material is the same, the slope of the curve at this point approaches 0 when the thickness of the first light emitting layer 111 increases to 150 μm, which indicates that the luminous efficacy approaches the maximum, and the slope of the curve is 0 when the thickness increases to more than 200 μm, so that the luminous efficacy reaches the maximum. Therefore, in order to ensure the light efficiency characteristics, in the present embodiment, the thickness of the first light emitting layer 111 is 150 to 200 μm.
The functional layer 12 comprises a first functional layer 121, the mass fraction of the fluorescent powder in the first functional layer 121 is 5% -50%, and the thickness of the first functional layer 121 is 5-50 μm. A continuous and dense transition layer (not shown) is present between the light-emitting layer 11 and the functional layer 12.
Since the first functional layer 121 is mainly used as a film coating layer, the processing precision and the light efficiency loss need to be considered. Due to the difference of expansion coefficients, the sintering process after the high-concentration layer and the low-concentration layer are filled and assembled can generate the condition of different shrinkage rates, the processing is uncontrollable when the thickness is too small, and the cracking phenomenon can be generated when the thickness is too large. On the other hand, because the first light emitting layer 111 is used as a main wavelength conversion layer, a light source enters from the side of the first light emitting layer 111 far away from the first functional layer 121, excitation light firstly enters the first light emitting layer 111, is absorbed by the fluorescent powder of the first light emitting layer 111 to emit first received laser light, and the first received laser light enters the first functional layer 121 and is emitted through the layer; in addition, a part of the excitation light which is not completely absorbed by the phosphor in the first light emitting layer 111 also penetrates through the first light emitting layer 111 to enter the first functional layer 121 and is absorbed by the phosphor in the first functional layer 121 to emit second stimulated light, and the second stimulated light is emitted through the layer; if the first functional layer 121 is too thick, the first received laser light may laterally propagate when passing through the layer to cause light loss; if the first functional layer 121 is too thin, excitation light that is not completely absorbed by the phosphor in the first light emitting layer 111 easily penetrates the first functional layer 121, causing light loss. In this embodiment, the inventor found out through experiments that the thickness of the first functional layer 121 is optimally controlled to be 5 to 50 μm, in view of the processing accuracy and the light loss.
The specific thickness setting of the first functional layer 121 and the first light-emitting layer 111 needs to be determined according to the proportion of volume shrinkage after sintering, and only needs to satisfy that the thickness of the light-emitting layer of the light-emitting device obtained by sintering satisfies 150-200 μm and the thickness of the functional layer satisfies 5-50 μm.
In addition, in the present embodiment, since the tablet sintering method is adopted, the transition layer is continuously dense, and the porosity is detected to be 2% to 6.4%.
In this embodiment, specifically, the phosphor may be Lu3Al5O12:Ce3+Fluorescent powder; correspondingly, the binder is glass powder or alumina powder or Lu3Al5O12And (3) pulverizing.
Example two
Referring to fig. 2, the present invention provides a light emitting device 20, which comprises phosphor and a binder for binding.
In this embodiment, the phosphor is commercially available Y3Al5O12:Ce3+Fluorescent powder; the binder is glass powder or alumina powder or Y3Al5O12The powder mainly plays a role in binding other components. The hardness of the binder is different from that of the fluorescent powder, such as: the Mohs hardness of the glass powder is 5.5-6, the Mohs hardness of the fluorescent powder is 8-8.5, and the Mohs hardness of the alumina powder is 9.
The light emitting device 20 is designed to be tablet-sintered by a gradient differential concentration ratio method, and includes a light emitting layer 21 and an integral sintered body of a functional layer 22 laminated on the light emitting layer 21.
The light-emitting layer 21 comprises a first light-emitting layer 211, and the mass fraction of the fluorescent powder in the first light-emitting layer 211 is 50-99%. Since the first light emitting layer 211 is usually used as a main wavelength conversion layer, the inventor experimentally found that the luminous efficacy increases with the increase of the thickness of the first light emitting layer 211 when the concentration of the fluorescent material is the same, and the slope of the curve at this point approaches 0 when the thickness of the first light emitting layer 211 increases to 150 μm, which indicates that the luminous efficacy approaches the maximum, and the slope of the curve is 0 when the thickness increases to more than 200 μm, so that the luminous efficacy reaches the maximum. Therefore, in order to ensure the light efficiency characteristics, in the present embodiment, the thickness of the first light emitting layer 211 is 150 to 200 μm.
The functional layer 22 comprises a first functional layer 221, the mass fraction of the fluorescent powder in the first functional layer 221 is 5% -50%, and the thickness of the first functional layer 221 is 5-50 μm. A continuous and dense transition layer (not shown) is present between the light-emitting layer and the functional layer.
Since the first functional layer 221 is mainly used as a film coating layer, the processing precision and the light efficiency loss need to be considered. Due to the difference of expansion coefficients, the sintering process after the high-concentration layer and the low-concentration layer are filled and assembled can generate the condition of different shrinkage rates, the processing is uncontrollable when the thickness is too small, and the cracking phenomenon can be generated when the thickness is too large. On the other hand, since the first light emitting layer 211 is used as a main wavelength conversion layer, a light source enters from a side of the first light emitting layer 211 away from the first functional layer 221, excitation light firstly enters the first light emitting layer 211, is absorbed by phosphor of the first light emitting layer 211 to emit first received laser light, and the first received laser light enters the first functional layer 221 and exits through the layer; in addition, a part of the excitation light which is not completely absorbed by the phosphor in the first light emitting layer 211 also penetrates through the first light emitting layer 211 to enter the first functional layer 221 and be absorbed by the phosphor of the first functional layer 221 to emit second received laser light, and the second received laser light is emitted through the layer; if the first functional layer 221 is too thick, the first received laser light may laterally propagate when passing through the layer to cause light loss; if the first functional layer 221 is too thin, excitation light that is not completely absorbed by the phosphor in the first light emitting layer 211 easily penetrates the first functional layer 221, causing light loss. In this embodiment, the inventors have found through experiments that the thickness of the first functional layer 221 is optimally controlled to be 5 to 50 μm, in view of the processing accuracy and the light loss.
The difference from the first embodiment is that: the first functional layer 221 is formed by stacking at least two first sub-functional layers 2211, a continuous and dense transition layer (not shown) is arranged between each first sub-functional layer 2211, the mass fraction of the phosphor in each first sub-functional layer 2211 increases by a specific gradient along the direction extending from the first functional layer 221 to the first light-emitting layer 211, and the specific gradient ranges from 5% to 10%; the phosphor in each of the first sub-functional layers 2211 is uniformly distributed.
In this embodiment, an optical coating 23 may be disposed on the first functional layer 221 on a side away from the first light emitting layer 211, where the optical coating 23 includes a reflective film and an antireflection film, and the coating manner includes, but is not limited to, magnetron sputtering and vacuum evaporation.
Because the hardness of the fluorescent powder and the adhesive is different, the abrasion state is different when the high-concentration layer is polished, and embossing is formed; however, the light emitting efficiency is affected by directly reducing the concentration of the phosphor in the light emitting layer, so the first functional layer 221 is designed and coated with a film on the first functional layer 221, and it needs to be considered that if the concentration of the first functional layer 221 is too low, the first light emitting layer 211 and the first functional layer 221 are broken due to too large difference of shrinkage coefficients in the subsequent sintering process.
Therefore, unlike the first embodiment, in this embodiment, the first functional layer 221 is formed by stacking at least two first sub-functional layers 2211, a continuous and dense transition layer is present between each first sub-functional layer 2211, the phosphor content of each first sub-functional layer 2211 is different, and increases in a specific gradient along the direction extending from the first functional layer 221 to the first light-emitting layer 211, and this structure has an advantage that the phosphor concentration in the first sub-functional layer 2211 close to the first light-emitting layer 211 is higher and is smaller than or equal to the phosphor concentration in the first light-emitting layer 211; while the concentration of the phosphor in the first sub-functional layer 2211 far away from the first light emitting layer 211 is low, close to pure phase, even 0. It is much easier to plate the optical film 23 on the first sub-functional layer 2211 remote from the first light-emitting layer 211. Such a change in gradient concentration does not cause a crack in a certain portion due to an excessively large difference in shrinkage coefficient, and the light-emitting efficiency of the first light-emitting layer 211 is ensured. In the present embodiment, the transition layer porosity is 2% to 6.4%.
Similarly, in this embodiment, the phosphor may be Lu3Al5O12:Ce3+Fluorescent powder; the binder is glass powder or alumina powder or Lu3Al5O12And (3) pulverizing.
The specific thickness setting of the first functional layer 221 and the first light-emitting layer 211 is determined according to the proportion of volume shrinkage after sintering, and only needs to satisfy that the thickness of the light-emitting layer of the light-emitting device obtained by sintering satisfies 150-200 μm and the thickness of the functional layer satisfies 5-50 μm. Of course, the specific thickness of each of the first sub-functional layers 2211 may also be determined with reference to the above conditions.
EXAMPLE III
Referring to fig. 3, the present invention provides a light emitting device 30, which comprises phosphor and a binder for binding.
In this embodiment, the phosphor is commercially available Y3Al5O12:Ce3+Fluorescent powder; the binder isGlass powder or alumina powder or Y3Al5O12The powder mainly plays a role in binding other components. The hardness of the binder is different from that of the fluorescent powder, such as: the Mohs hardness of the glass powder is 5.5-6, the Mohs hardness of the fluorescent powder is 8-8.5, and the Mohs hardness of the alumina powder is 9. The light emitting device of the present invention is designed to have a gradient concentration to form a low concentration layer on which a plating film is polished. Because the hardness of the phosphor and the bonding medium are different, different wear states occur during polishing of the high-concentration layer, and 'emboss' is formed. And the low-concentration layer has less or no fluorescent powder, and the polished surface is relatively flat, thereby being convenient for coating.
The light-emitting device 30 of the present embodiment includes a light-emitting layer 31, and a sintered body of a functional layer 32 laminated on the light-emitting layer 31, similarly to the light-emitting device described in the first embodiment.
The light-emitting layer 31 comprises a first light-emitting layer 311, and the mass fraction of the fluorescent powder in the first light-emitting layer 311 is 50-99%. In order to ensure the light-emitting characteristics, in this embodiment, the thickness of the first light-emitting layer 311 is 150 to 200 μm. The thickness of the first light-emitting layer 311 is set according to the description in the first embodiment, and is not described herein again.
The functional layer 32 comprises a first functional layer 321, the mass fraction of the fluorescent powder in the first functional layer 321 is 5% -50%, and the thickness of the first functional layer 321 is 5-50 μm. The thickness of the first functional layer 321 is set according to the description in the first embodiment, and is not described herein again. A continuous and dense transition layer (not shown) is present between the light-emitting layer 31 and the functional layer 32. The difference from the first embodiment is that: the first light emitting layer 311 is formed by stacking at least two first sub-light emitting layers 3111, a continuous and dense transition layer is arranged between each first sub-light emitting layer 3111, the mass fraction of the phosphor in each first sub-light emitting layer 3111 increases progressively with a specific gradient along the direction extending from the first functional layer 321 to the first light emitting layer 311, and the specific gradient ranges from 5% to 10%; the phosphor in each of the first sub-light emitting layers 3111 is uniformly distributed.
Due to the low thickness of the first functional layer 321, the design requirement for performing the gradient concentration on the first functional layer 321 as described in example two is high, and the cost is correspondingly high if the light-emitting device is used in some environments where the requirement for the light-emitting efficiency is not particularly high. Therefore, in the present embodiment, the gradient difference concentration is designed in the first light emitting layer 311, since the thickness of the first light emitting layer 311 is relatively high, it is easy to design a plurality of first sub light emitting layers 3111 with gradient concentration variation to form the first light emitting layer 311, and the difference between the concentration of the phosphor in the first sub light emitting layer 3111 close to the first functional layer 321 and the concentration of the phosphor in the first functional layer 321 is relatively small, even equal; the concentration of the phosphor in the first sub-emission layer 3111 away from the first functional layer 321 is designed to be higher, thus ensuring the light emission efficiency.
In the same manner as the second embodiment, an optical coating 33 may be disposed on a side of the first functional layer 321 away from the first light emitting layer 311, where the optical coating 33 includes a reflective film and an antireflection film, and the coating manner includes but is not limited to magnetron sputtering and vacuum evaporation.
The advantage of the light emitting device 30 in this embodiment is the same as that of the light emitting device in the second embodiment, that is, the concentration of the phosphor in the light emitting device 30 is changed in a gradient manner, and the phosphor is not broken during sintering, and meanwhile, the low concentration is designed on the first functional layer 321 to facilitate the film coating process due to the controllable concentration.
In the present embodiment, the transition layer porosity is 2% to 6.4%.
Similarly, the phosphor described in this embodiment may be Lu3Al5O12:Ce3+Fluorescent powder; the binder is glass powder or alumina powder or Lu3Al5O12And (3) pulverizing.
For determining the thickness of each layer, reference may be made to embodiment one or embodiment two, and details are not repeated here.
Example four
Referring to fig. 4, this embodiment is an extension of the second embodiment and the third embodiment, that is, the second embodiment and the third embodiment are combined to form a fourth embodiment:
that is, the first functional layer 421 of the light-emitting device 40 is formed by stacking at least two first sub-functional layers 4211, a continuous and dense transition layer (not shown) is present between each first sub-functional layer 4211, the mass fraction of the phosphor in each first sub-functional layer 4211 increases by a specific gradient along the direction extending from the first functional layer 421 to the first light-emitting layer 411, and the specific gradient ranges from 5% to 10%; the phosphor in each of the first sub-functional layers 4211 is uniformly distributed.
The first light-emitting layer 411 of the light-emitting layer 41 is formed by stacking at least two first sub-light-emitting layers 4111, a continuous and dense transition layer exists between each first sub-light-emitting layer 4111, the mass fraction of the phosphor in each first sub-light-emitting layer 4111 in the first light-emitting layer 411 increases by the same specific gradient, and it should be noted that the mass fraction increases by the same specific gradient, that is: when the mass fraction of the phosphor in each of the first sub-functional layers 4211 increases at a gradient of 6% in a direction extending from the first functional layer 421 to the first light-emitting layer 411, the mass fraction of the phosphor in each of the first sub-light-emitting layers 4111 in the first light-emitting layer 411 also increases at a gradient of 6%; the phosphor in each of the first sub-emission layers 4111 is uniformly distributed; the difference in mass fractions of the phosphors in the adjacent first sub light emitting layer 4111 and the first sub functional layer 4211 is 0 or the specific gradient.
Of course, in this embodiment, the specific gradient may be increased incrementally, that is, two different values are selected within a range of 5% to 10% of the specific gradient, and the increasing gradient of the first functional layer 421 is different from the increasing gradient of the first light-emitting layer 411, and is respectively changed by the respective specific gradients, for example: the mass fraction of the phosphor in each of the first sub-functional layers 4211 increases by a gradient of 6% in a direction extending from the first functional layer 421 to the first light-emitting layer 411, and the mass fraction of the phosphor in each of the first sub-light-emitting layers 4111 increases by a gradient of 7% in a direction extending from the first functional layer 421 to the first light-emitting layer 411. The phosphor in each of the first sub-emission layers 4111 is uniformly distributed; the difference in mass fractions of the phosphors in the adjacent first sub light emitting layer 4111 and the first sub functional layer 4211 may be 0.
In designing the thickness of each of the first sub-functional layers 4211 and/or each of the first sub-luminescent layers 4111, the following method may be referred to:
usually, the first light emitting layer 411 is used as a main wavelength conversion layer, the first functional layer 421 is used as a coating layer, because the performance optimization problem of the whole light emitting device is considered, the mass fraction of the fluorescent powder of the wavelength conversion layer is 50% -99%, the thickness is 150-200 μm, when the concentration gradient distribution of the wavelength conversion layer is carried out, the mass fraction (namely, specific gradient) difference (marked as concentration tolerance d1) between every two layers can be increased or decreased gradually according to 5% -10%, and the concentration gradient grading mainly considers the content of the fluorescent powder and influences the volume shrinkage after sintering, so the concentration difference between every two layers cannot be too large. Therefore, the number of phosphor gradient layers T1 of the first light emitting layer 411 (i.e., wavelength conversion layer) is (N)max-Nmin) D1, wherein NmaxIs the maximum value of the mass fraction of the phosphor in each of the first sub-emitting layers 4111, NminThe minimum value of the mass fraction of the phosphor in each first sub-functional layer 4211; the thickness H of each layer (i.e., each of the first sub-emitting layers 4111 of the first emitting layer 411) corresponds to the concentration of phosphor, wherein the thickness H1 is H1/T1, H1 is the thickness of the first emitting layer 411, and H1 is 150-200 μm. d1 can be 0, i.e. the phosphor in the first light emitting layer 411 is uniformly distributed as a whole.
Similarly, the thickness H2 of each of the first sub-functional layers 4211 of the first functional layer 421 of the functional layer 42 is H2/T2, T2 is the number of gradient concentration layers of the phosphor of the first functional layer 421 (i.e., the coating layer), and T2 is (M) Mmax-Mmin) D2, wherein MmaxIs the maximum value of the mass fraction of the phosphor in the first functional layer 421, MminIs the minimum value of the mass fraction of the phosphor in the first functional layer 421; d2 is the concentration tolerance of the first functional layer 421, d2 is any value of 5% to 10%; d2 may be 0, that is, the phosphor is uniformly distributed in the first functional layer 421. D1 and d2 may be the same or different as described above.
Similarly, in this embodiment, an optical coating 43 may also be disposed on the first functional layer 421 on a side away from the first light emitting layer 411, where the optical coating 43 includes a reflective film and an antireflection film, and the coating manner includes, but is not limited to, magnetron sputtering and vacuum evaporation.
In this embodiment, for the selection of the phosphor and the binder, reference may be made to the description of any one of the first to third embodiments, which is not repeated herein.
EXAMPLE five
Please refer to fig. 5, the fifth embodiment is another extension of the first to fourth embodiments. That is, in the light-emitting device according to any one of the first to fourth embodiments, the functional layer 52 of the light-emitting device 50 according to this embodiment further includes a second functional layer 522 (that is, including a first functional layer 521 and a second functional layer 522), and the second functional layer 522 is laminated on the first functional layer 521 and on the side of the first light-emitting layer 511 apart from the light-emitting layer 51, and forms an integral sintered body with the first functional layer 521. The mass fraction of the fluorescent powder in the second functional layer 522 is 0, the thickness of the second functional layer 522 is 0.1-5 μm, a continuous and compact transition layer (not shown) is arranged between the second functional layer 522 and the first functional layer 521, and the porosity of the transition layer is 2-6.4%. Otherwise, this embodiment is the same as any of the first to fourth embodiments, and is not repeated herein.
When the structure of this embodiment is selected, correspondingly, the optical coating 53 may be disposed on the second functional layer 522 away from the first light emitting layer 521, where the optical coating 53 includes a reflective film and an antireflection film, and the coating manner includes, but is not limited to, magnetron sputtering and vacuum evaporation.
EXAMPLE six
Referring to fig. 6, the present embodiment is expanded based on any one of the first to fifth embodiments.
Namely, the difference is that: in this embodiment, the functional layer 62 of the light-emitting device 60 further includes a third functional layer 623 laminated on the first light-emitting layer 611 of the light-emitting layer 61 on the side away from the first functional layer 621, and a fourth functional layer 624 laminated on the third functional layer 623 on the side away from the first light-emitting layer 611. I.e. comprising a first functional layer 621, a second functional layer 622, a third functional layer 623 and a fourth functional layer 624.
The mass fraction of the fluorescent powder in the third functional layer 623 is 5% -50%, and the thickness of the third functional layer 523 is 5-50 μm; the mass fraction of the fluorescent powder in the fourth functional layer 624 is 0, and the thickness of the fourth functional layer 624 is 0.1-5 μm; the transition layer (not shown) is continuously and densely present between the first light-emitting layer 611 and the third functional layer 623; the transition layer (not shown) is continuously and densely provided between the fourth functional layer 624 and the third functional layer 623, and the transition layer has a porosity of 2% to 6.4%.
In this embodiment, the third functional layer 623 may have a uniform phosphor concentration distribution as a whole, or may have a gradient concentration distribution by providing a plurality of sub-functional layers as in the second functional layer 622 described in the second embodiment, which will be easily understood by those skilled in the art and will not be described herein again.
Of course, in addition to this embodiment, it is also possible to laminate the optical coating film 63 on the side of the fourth functional layer 624 away from the first light-emitting layer 611.
It should be noted that: when the optical coating film 63 is laminated on both the side of the second functional layer 622 away from the first light-emitting layer 611 and the side of the fourth functional layer 624 away from the first light-emitting layer 611: the optical coating films on the two sides are both reflecting films or are both antireflection films; or one side of the film may be a reflective film and the other side may be an anti-reflective film, as will be apparent to those skilled in the art.
In addition, when the functional layer 63 may include at least one of the first functional layer 621, the second functional layer 622, the third functional layer 623 and the fourth functional layer 624, the optical coating 63 is disposed on a side of the first functional layer 621, the second functional layer 622, the third functional layer 623 or the fourth functional layer 624 away from the light-emitting layer 61, for example:
when only the first functional layer 621 is included, the optical coating 63 is disposed on the side of the first functional layer 621 away from the light-emitting layer 61;
when the light-emitting layer 61 comprises the first functional layer 621 and the second functional layer 622 which are sequentially laminated on the same side of the light-emitting layer 61, the second functional layer 622 is positioned on the side of the first functional layer 621 far away from the light-emitting layer 61, and the optical coating 63 is positioned on the side of the second functional layer 622 far away from the light-emitting layer 61;
when the light-emitting device includes a first functional layer 621, a second functional layer 622 and a third functional layer 623 which are stacked on the light-emitting layer, the first functional layer 621 and the second functional layer 622 are located on the same side of the light-emitting layer 61, the second functional layer 622 is located on the side of the first functional layer 621 away from the light-emitting layer 61, and the third functional layer 623 is located on the side of the light-emitting layer 61 away from the first functional layer 621, the optical coating 63 may be disposed on the side of the second functional layer 622 away from the light-emitting layer 61 or/and on the side of the third functional layer 623 away from the light-emitting layer 61.
By analogy, this is possible, as are the principles, and will be readily apparent to those skilled in the art from the foregoing description.
Referring to fig. 7-8, the present invention further provides a method for manufacturing a light emitting device, the method comprising the steps of:
step S1, mixing materials:
mixing and ball-milling an organic carrier and a binder to obtain a ball-milling blank; and adding fluorescent powder into the ball-milling blank, and continuously performing ball milling to obtain a mixed initial material.
Specifically, step S1 includes step S11 of adding alumina powder (or glass powder or Y)3Al5O12Powder or Lu3Al5O12Powder) is added with absolute ethyl alcohol as a liquid phase medium, PVA or PVB with the concentration of 1-5% is added as a binder, and mixed to obtain a mixed raw material.
And step S12, putting the mixed raw materials into a ball milling tank for ball milling and mixing, and carrying out nodular graphite treatment for 4-8 hours to form ball milling blanks.
Step S13, dividing the ball milling blank into at least two parts including a first part and a second part, adding fluorescent powder into the first part, wherein the mass ratio of the fluorescent powder to the binder in the first part is 1-99: 1, adding fluorescent powder into the second part, wherein the mass ratio of the fluorescent powder to the binder in the second part is 1: 1-19, respectively continuing to perform ball milling, setting the ball milling time to be 30-60 minutes, drying at 80 ℃ to remove the absolute ethyl alcohol, respectively separating, grinding and sieving to obtain the mixed primary material, including the first mixed primary material and the second mixed primary material.
Of course, the number of parts of the mixed stock is not limited thereto, and may be divided into more parts (portions). In this step, preferably, the mixed blank further includes a divided third portion; the first part is added with fluorescent powder with the component content of 50% -75%, and the second part is added with fluorescent powder with the component content of 5% -15%; the third portion is free of added phosphor.
Step S2, charging:
and filling the mixed initial material into a mold.
Specifically, the first mixed initial material and the second mixed initial material are sequentially filled in the die.
Step S3, pre-compression:
paving the mixed primary material in the die, and applying 80-100 kg/cm2Pre-pressing under pressure to obtain a pre-formed blank.
Step S4, heat treatment, molding:
and (3) degreasing and degumming the preformed blank body in a high-temperature furnace, regulating the temperature to be the decomposition temperature of the binder, keeping for 5-10 hours, placing the preformed blank body in a hydraulic cavity of cold isostatic pressing, keeping the pressure for 1 minute at the pressure of 250-300 Mpa, and performing cold isostatic pressing treatment to form a biscuit.
In the step, the obtained biscuit comprises a luminescent biscuit layer containing 50-99% of fluorescent powder by mass and a functional biscuit layer containing 5-50% of fluorescent powder by mass, and the thickness of the luminescent biscuit layer is larger than that of the functional biscuit layer.
Of course, the specific time for protection in the high temperature furnace may depend on the volume of the preform body.
Step S5, sintering:
putting the biscuit into a vacuum tungsten filament furnace, wherein the vacuum degree is 10-4And (3) keeping the temperature within the range of Pa and at the temperature of 1500-1800 ℃ for 4-10 hours, and performing vacuum sintering to obtain the light-emitting device.
The preparation method adopts a tabletting and sintering process, the particles of the powder are stacked together after being mixed, are subjected to prepressing forming, are subjected to high-temperature binder removal to remove organic matters, and then although some holes can be formed, cold isostatic pressing is carried out, high pressure is applied to the sample again to ensure that the powder is more compact, the holes are eliminated to a certain extent, and after the sintering process is carried out, the liquid-phase binding material is further filled, so that the porosity is higher than that of the printing mode;
of course, the preparation method can also adopt hot-pressing sintering, and the glass powder (or alumina powder or Y) is directly used without adding organic components in the powder material, removing glue and other processes3Al5O12Powder or Lu3Al5O12Powder) as a binder, i.e., the mixing process of step S1 described in the above preparation method does not add an organic vehicle, and the binder is directly ball-milled to obtain a ball-milled raw material, so that the heat treatment step of step S4 can be omitted. Because the method does not have a glue discharging process and can not increase the porosity, powder is directly filled according to the gradient concentration, and then the sintering process is carried out while sintering and pressurizing; the density of the material is further improved, and the porosity can be further reduced.
Compared with the prior art, the light-emitting device and the preparation method thereof have different concentrations, even gradient different concentrations, and form a low-concentration layer on which a coating can be polished. Because of the different hardness of the phosphor and binder, polishing at high concentration layers can exhibit different wear states, forming "embossments". And the low-concentration layer has less or no fluorescent powder, and the polished surface is relatively flat, thereby being convenient for coating. The invention solves the problem that the surface of the light-emitting device of the complex phase material is seriously uneven after being polished due to the hardness difference of two-phase media by adjusting the content of the fluorescent powder of the low-concentration layer, and the processing is simple and convenient; because the content of the fluorescent powder in the light-emitting device directly influences the light-emitting efficiency of the light-emitting device, the light-emitting device ensures the fluorescence efficiency of a main body and adjusts the proper gradient concentration on a shallow surface layer, so that the polished surface is close to a pure phase, and the polishing defect of the surface is reduced; meanwhile, the concentration of the fluorescent powder of each layer is controllable, so that the separation phenomenon of different concentration layers caused by inconsistent volume shrinkage during sintering is avoided.
Claims (10)
1. A light-emitting device, its component includes phosphor powder and binder used for playing the function of adhesion, characterized by that: the light-emitting device is an integral sintered body including a light-emitting layer and a functional layer laminated on the light-emitting layer;
the light-emitting layer comprises a first light-emitting layer, the mass fraction of fluorescent powder in the first light-emitting layer is 50% -99%, and the thickness of the first light-emitting layer is 150-200 mu m;
the functional layer comprises a first functional layer, the mass fraction of fluorescent powder in the first functional layer is 5% -50%, and the thickness of the first functional layer is 5-50 μm;
a continuous compact transition layer is arranged between the luminous layer and the functional layer;
the phosphor and the binder have different Mohs hardness.
2. The light-emitting device according to claim 1, wherein the first functional layer is formed by stacking at least two first sub-functional layers, a continuous and dense transition layer is present between each first sub-functional layer, the mass fraction of the phosphor in each first sub-functional layer increases with a specific gradient in a direction extending from the first functional layer to the first light-emitting layer, and the specific gradient ranges from 5% to 10%; and the fluorescent powder in each first sub-functional layer is uniformly distributed.
3. The light-emitting device according to claim 1, wherein the first light-emitting layer is formed by stacking at least two first sub-light-emitting layers, a continuous and dense transition layer is present between each first sub-light-emitting layer, and the mass fraction of the phosphor in each first sub-light-emitting layer increases with a specific gradient in a direction extending from the first functional layer to the first light-emitting layer, and the specific gradient is in a range of 5% to 10%; and the fluorescent powder in each first sub-luminous layer is uniformly distributed.
4. The light-emitting device according to claim 1, wherein the first functional layer is formed by stacking at least two first sub-functional layers, a continuous and dense transition layer is present between each first sub-functional layer, the mass fraction of the phosphor in each first sub-functional layer increases with a specific gradient in a direction extending from the first functional layer to the first light-emitting layer, and the specific gradient ranges from 5% to 10%; the fluorescent powder in each first sub-functional layer is uniformly distributed; the first light-emitting layer is formed by laminating at least two first sub light-emitting layers, a continuous and compact transition layer exists between every two first sub light-emitting layers, the mass fraction of fluorescent powder in each first sub light-emitting layer in the first light-emitting layers is increased progressively by the same specific gradient, and the fluorescent powder in each first sub light-emitting layer is uniformly distributed; the mass fraction difference of the fluorescent powder in the adjacent first sub-luminous layer and the first sub-functional layer is 0 or the specific gradient.
5. The light-emitting device according to any one of claims 1 to 4, wherein the transition layer has a porosity of 2% to 6.4%.
6. The light-emitting device according to claim 5, wherein an optical coating film is provided on the first functional layer on a side away from the first light-emitting layer, and the optical coating film includes a reflective film and an antireflection film.
7. The light-emitting device according to claim 5, wherein the functional layer further comprises a second functional layer laminated on the first functional layer on a side away from the first light-emitting layer, the second functional layer forming an integral sintered body with the first functional layer, the second functional layer has a phosphor mass fraction of 0, the second functional layer has a thickness of 0.1 to 5 μm, and a continuous and dense transition layer is present between the second functional layer and the first functional layer.
8. The light-emitting device according to claim 6 or 7, wherein the functional layers further include a third functional layer stacked on the first light-emitting layer and away from the first functional layer, and a fourth functional layer stacked on the third functional layer and away from the first light-emitting layer, the mass fraction of the phosphor in the third functional layer is 5% to 50%, and the thickness of the third functional layer is 5 μm to 50 μm; the mass fraction of the fluorescent powder in the fourth functional layer is 0, and the thickness of the fourth functional layer is 0.1-5 μm; a continuous and compact transition layer is arranged between the first light-emitting layer and the third functional layer; and the continuous and compact transition layer is arranged between the fourth functional layer and the third functional layer.
9. The light-emitting device according to any one of claims 1 to 4, 6 or 7, wherein the phosphor is Y3Al5O12:Ce3+Phosphor or Lu3Al5O12:Ce3+Fluorescent powder; the binder is glass powder or alumina powder or Y3Al5O12Powder or Lu3Al5O12And (3) pulverizing.
10. A method of making a light emitting device comprising the steps of:
step S1: mixing materials; ball-milling the binder to obtain a ball-milled blank; adding fluorescent powder into the ball-milling blank, and continuously performing ball milling to obtain a mixed primary material;
step S2: charging; filling the mixed initial material into a mould;
step S3: pre-pressing; pre-pressing the mixed initial material in the die to obtain a pre-formed blank body;
step S4: sintering; carrying out cold isostatic pressing treatment on the pre-formed blank to obtain a biscuit, and sintering the biscuit to obtain the light-emitting device;
the method is characterized in that:
step S1 further includes dividing the ball mill blank into at least two parts including a first part and a second part, where the mass ratio of the binder added to the first part is 1:1 or 99:1, adding fluorescent powder into the second part, wherein the mass ratio of the fluorescent powder to the binder in the second part is 1:19, and respectively continuing ball milling to obtain a first mixed initial material and a second mixed initial material;
the step S2 is specifically to sequentially load the first mixed starting material and the second mixed starting material into the mold;
the biscuit obtained in the step S4 includes a luminescent biscuit layer containing 50% or 99% by mass of phosphor and a functional biscuit layer containing 5% by mass of phosphor, and the thickness of the luminescent biscuit layer is greater than that of the functional biscuit layer.
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| PCT/CN2017/109313 WO2018188326A1 (en) | 2017-04-10 | 2017-11-03 | Light emitting device and manufacturing method therefor |
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| CN115846899B (en) * | 2022-11-30 | 2023-07-18 | 广州星熠新材料科技有限公司 | Processing technology of CVD diamond piece |
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| WO2018188326A1 (en) | 2018-10-18 |
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