CN112047758A - Preparation method for preparing large-size ultrathin fluorescent ceramic wafer through one-step forming - Google Patents
Preparation method for preparing large-size ultrathin fluorescent ceramic wafer through one-step forming Download PDFInfo
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Abstract
The invention discloses a preparation method for preparing a large-size ultrathin fluorescent ceramic wafer by one-step forming, and particularly relates to the field of preparation of fluorescent ceramic wafers, wherein the preparation method comprises the following steps: s1: preparing a ceramic wafer template, wherein the substrate template is made of fluorescent transparent ceramic with a YAG (yttrium aluminum garnet)/Ce/(Gd, Y) AG and Ce double-layer composite structure, a layer of metal nano-shell template is paved on the upper surface and the lower surface of the substrate, the metal nano-shell template is synthesized by a metal particle film, the metal nano-particle film is prepared by adopting an electroless chemical deposition method or a wet coating technology, and a group of electro-optical memory ceramic wafers are additionally arranged on the upper layer and the lower layer of the substrate; s2: and forming, namely bonding the substrate template and the electro-optical memory ceramic wafer by adopting a multi-template combined gel injection forming technology. The invention improves the brightness of the laser light source and the service life of the device to the utmost extent, meets the requirements of high color rendering index and low color temperature of white light emission required by indoor illumination, and can realize red light spectrum enhancement, red shift and widening.
Description
Technical Field
The invention relates to the field of preparation of fluorescent ceramic sheets, in particular to a preparation method for preparing a large-size ultrathin fluorescent ceramic sheet through one-step forming.
Background
Under the current large background that the world energy is increasingly tense and the environmental problem is outstanding, all countries in the world develop the technology of strengthening energy-saving and efficient green energy, and because the solid-state lighting light source has the advantages of energy conservation, environmental protection, high potential lighting effect, long service life, small volume and the like, the solid-state lighting light source is the green light source with the greatest development potential, the fluorescent ceramic has higher absorption coefficient and refractive index than the traditional fluorescent powder, and the fluorescent ceramic has the advantages of good transparency, high hardness, corrosion resistance, high temperature resistance, simple manufacturing process and low production cost, and can be produced in large batch.
The existing fluorescent ceramic sheet has single composition, and a multilayer composite structure ceramic material cannot be obtained by adopting a fluorescent ceramic system doped with rare earth-rare earth ions and rare earth-transition metal group ions, so that the red light spectrum enhancement, red shift and broadening are difficult to realize through the crystal structure and the crystal field environment regulation and control.
The above information disclosed in this background section is only for enhancement of understanding of the background of the disclosure and therefore it may contain information that does not constitute prior art that is already known to a person of ordinary skill in the art.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide a method for preparing a large-sized ultrathin fluorescent ceramic sheet by one-step molding, and the technical problem to be solved by the present invention is: how to realize red light spectrum enhancement, red shift and broadening through crystal structure and crystal field environment regulation and control.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method for preparing a large-size ultrathin fluorescent ceramic wafer in one-step forming comprises the following steps:
s1: preparing a ceramic wafer template, wherein the substrate template is made of fluorescent transparent ceramic with a YAG (yttrium aluminum garnet)/Ce/(Gd, Y) AG and Ce double-layer composite structure, a layer of metal nano-shell template is paved on the upper surface and the lower surface of the substrate, the metal nano-shell template is synthesized by a metal particle film, the metal nano-particle film is prepared by adopting an electroless chemical deposition method or a wet coating technology, and a group of electro-optical memory ceramic wafers are additionally arranged on the upper layer and the lower layer of the substrate;
s2: forming, namely bonding and forming the substrate template and the electro-optical memory ceramic wafer by adopting a multi-template combined gel injection forming technology, and then combining a medium-temperature heating sintering stage and a high-temperature heat preservation completion sintering stage of a sintering process to prepare a large-size fluorescent ceramic wafer;
s3: and cutting, namely cutting the large-size fluorescent ceramic wafer into the required size and shape by adopting a high-precision ceramic cutting machine.
In one embodiment, a ceramic sheet mold is preparedThe plate and the substrate template are made of YAG Ce/(Gd, Y) AG Ce double-layer composite structure fluorescent transparent ceramics, when the substrate template is manufactured, the YAG Ce/(Gd, Y) AG Ce double-layer composite structure fluorescent transparent ceramics are manufactured by adopting the components and the structure design of a garnet structure phosphor, and Gd is changed3+The doping concentration of the substrate is controlled within the range of 3100k-3600k, the luminous efficiency reaches 109.9lm/w, a layer of metal nano-shell template is paved on the upper surface and the lower surface of the substrate, the metal nano-shell template is synthesized by a metal particle film, the metal nano-particle film is manufactured by adopting an electroless chemical deposition method or a wet plating technology, the metal nano-particle film material adopts metal nano-particles with the diameter of 40nm, the metal particles are selected from gold, platinum, silver or copper materials, the same metal particles are selected, the substrate template and the metal nano-shell template form a substrate, the plasmon resonance effect can be extended to an infrared band by changing the composition of the substrate, the plasmon resonance frequency can be adjusted to the infrared region by changing the core-shell ratio of the metal nano-shell template, a group of electro-optical memory ceramic sheets are respectively arranged on the upper layer and the lower layer of the substrate, the electro-optical memory ceramic sheets adopt lead lanthanum titanate composite ceramics obtained by adding rare earth lanthanum into lead titanate ceramics, the method comprises the steps of adopting a multi-template combined gel injection molding technology to bond and mold a substrate template and an electro-optic memory ceramic chip, then combining a medium-temperature heating sintering stage and a high-temperature heat preservation completion sintering stage of a sintering process to prepare the large-size fluorescent ceramic chip, wherein in the high-temperature heat preservation completion sintering stage, the fluorescent ceramic chip forms a large number of closed pores and continues to be reduced, so that the pore size and the total pore number are reduced, the sintered body density is obviously increased, and a high-precision ceramic cutting machine is adopted to cut the large-size fluorescent ceramic chip into the required size and shape.
In a preferred embodiment, in S1, the Gd is changed during the fabrication of the substrate template3+The doping concentration of the organic electroluminescent material enables the color temperature to be controllable in the range of 3100k-3600k, and the luminous efficiency reaches 109.9 lm/w.
In a preferred embodiment, the metal nanoparticle thin film material in S1 adopts metal nanoparticles with a diameter of 40nm, and the metal particles are selected from gold, platinum, silver or copper materials.
In a preferred embodiment, the electro-optic memory ceramic sheet in S1 is a lead lanthanum zirconate titanate composite ceramic obtained by adding rare earth lanthanum to lead zirconate titanate ceramic.
In a preferred embodiment, in the sintering stage of completing the high-temperature heat preservation in S2, the fluorescent ceramic sheet forms a large number of closed pores and continues to shrink, so that the pore size and the total number of pores are reduced, and the density of the sintered body is obviously increased.
In a preferred embodiment, the fluorescent transparent ceramic with YAG: Ce/(Gd, Y) AG: Ce double-layer composite structure in S1 is prepared by adopting the components and the structural design of a garnet-structure phosphor.
In a preferred embodiment, the substrate template and the metal nanoshell template in S1 constitute a base, and the plasmon resonance effect can be extended to the infrared band by changing the constitution of the base.
In a preferred embodiment, the plasmon resonance frequency can be adjusted to the infrared region by changing the core-shell ratio of the metal nanoshell template in S1.
The invention has the technical effects and advantages that:
1. according to the invention, a fluorescent ceramic system doped with rare earth-rare earth ions and rare earth-transition metal group ions is adopted to obtain a multilayer composite structure ceramic material, so that the requirements of high color rendering index and low color temperature white light emission required by indoor illumination are met, red light spectrum enhancement can be realized, and red shift and spectrum broadening of a spectrum are realized through crystal structure and crystal field environment regulation;
2. aiming at the display requirement of wide color gamut, the fluorescent ceramic sheet obtained according to the energy level characteristics of rare earth and transition metal group ions has the properties of high heat conduction and stable luminescence heat, can completely replace fluorescent powder, and fundamentally solves the problems of fluorescent functional layer damage, luminescence heat quenching, luminescent layer aging and the like caused by thermal shock and thermal aggregation, thereby improving the brightness of a laser light source and prolonging the service life of devices to the maximum extent.
Detailed Description
Example embodiments will now be described more fully hereinafter with reference to examples of the invention. Example embodiments may, however, be embodied in many different forms and should not be construed as limited to the examples set forth herein; rather, these example embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Furthermore, the described features, structures, or characteristics may be combined in any suitable manner in one or more example embodiments. In the following description, numerous specific details are provided to give a thorough understanding of example embodiments of the disclosure. One skilled in the relevant art will recognize, however, that the subject matter of the present disclosure can be practiced without one or more of the specific details, or with other methods, components, steps, and so forth. In other instances, well-known structures, methods, implementations, or operations are not shown or described in detail to avoid obscuring aspects of the disclosure.
The invention provides a preparation method for preparing a large-size ultrathin fluorescent ceramic wafer by one-step forming, which comprises the following steps:
s1: preparing a ceramic wafer template, wherein the substrate template is made of fluorescent transparent ceramic with a YAG (yttrium aluminum garnet)/Ce/(Gd, Y) AG and Ce double-layer composite structure, a layer of metal nano-shell template is paved on the upper surface and the lower surface of the substrate, the metal nano-shell template is synthesized by a metal particle film, the metal nano-particle film is prepared by adopting an electroless chemical deposition method or a wet coating technology, and a group of electro-optical memory ceramic wafers are additionally arranged on the upper layer and the lower layer of the substrate;
s2: forming, namely bonding and forming the substrate template and the electro-optical memory ceramic wafer by adopting a multi-template combined gel injection forming technology, and then combining a medium-temperature heating sintering stage and a high-temperature heat preservation completion sintering stage of a sintering process to prepare a large-size fluorescent ceramic wafer;
s3: and cutting, namely cutting the large-size fluorescent ceramic wafer into the required size and shape by adopting a high-precision ceramic cutting machine.
In the step S1, Gd is changed during the fabrication of the substrate template3+The doping concentration of the organic electroluminescent material enables the color temperature to be controllable in the range of 3100k-3600k, and the luminous efficiency reaches 109.9 lm/w.
The metal nanoparticle film material in S1 adopts metal nanoparticles with the diameter of 40nm, and the metal particles are selected from gold, platinum, silver or copper materials.
The electro-optical memory ceramic sheet in S1 is a lead lanthanum zirconate titanate composite ceramic obtained by adding rare earth lanthanum into lead zirconate titanate ceramic.
In the sintering stage of finishing high-temperature heat preservation in the S2, the fluorescent ceramic sheet forms a large number of closed pores and is continuously reduced, so that the size and the total number of the pores are reduced, and the density of a sintered body is obviously increased.
The fluorescent transparent ceramic with the YAG: Ce/(Gd, Y) AG: Ce double-layer composite structure in the S1 is prepared by adopting the components and the structural design of a garnet-structured phosphor.
In the step S1, the substrate template and the metal nano-shell template form a substrate, and the plasmon resonance effect can be extended to an infrared band by changing the composition of the substrate.
In the step S1, the plasmon resonance frequency can be adjusted to the infrared region by changing the core-shell ratio of the metal nanoshell template.
The implementation mode is specifically as follows: preparing a ceramic wafer template, wherein the substrate template is fluorescent transparent ceramic with a YAG (yttrium aluminum garnet)/Ce/(Gd, Y) AG and Ce double-layer composite structure, and when the substrate template is prepared, the fluorescent transparent ceramic with the YAG/Ce/(Gd, Y) AG and Ce double-layer composite structure is prepared by adopting the components and the structural design of a garnet-structure phosphor and changing Gd3+The doping concentration of the metal nano-shell template is controlled within the range of 3100k-3600k, the luminous efficiency reaches 109.9lm/w, a layer of metal nano-shell template is paved on the upper surface and the lower surface of the substrate, the metal nano-shell template is synthesized by a metal particle film, the metal nano-particle film is prepared by adopting an electroless chemical deposition method or a wet plating technology, the metal nano-particle film material adopts metal nano-particles with the diameter of 40nm, and the metal particles are selected from gold, platinum, silver or copper materialsWherein, the substrate template and the metal nanometer shell template form a substrate, the plasmon resonance effect can be extended to an infrared band by changing the structure of the substrate, the plasmon resonance frequency can be adjusted to an infrared region by changing the core-shell ratio of the metal nanometer shell template, a group of electro-optic memory ceramic sheets are respectively arranged on the upper layer and the lower layer of the substrate, the electro-optic memory ceramic sheets adopt lead lanthanum zirconate titanate composite ceramics obtained by adding rare earth lanthanum into lead zirconate titanate ceramics, the substrate template and the electro-optic memory ceramic sheets are bonded and formed by adopting a multi-template combined gel injection molding technology, and then the medium temperature heating sintering stage and the high temperature heat preservation completion sintering stage of the sintering process are combined to prepare large-size fluorescent ceramic sheets, in the high temperature heat preservation completion sintering stage, the fluorescent ceramic sheets form a large amount of closed pores and are continuously reduced, so that the pore size and the total number of pores are reduced, the density of a sintered body is obviously increased, a high-precision ceramic cutting machine is adopted to cut a large-size fluorescent ceramic piece into required size and shape, aiming at the display requirement of wide color gamut, according to the energy level characteristics of rare earth and transition metal group ions, the obtained fluorescent ceramic piece has the performances of high heat conduction and stable luminous heat, can completely replace fluorescent powder, and fundamentally solves the problems of damage of a fluorescent function layer, quenching of luminous heat, aging of a luminous layer and the like caused by thermal shock and thermal aggregation, thereby furthest improving the brightness of a laser light source and the service life of devices, meeting the white light emission requirements of high color rendering index and low color temperature required by indoor illumination, a fluorescent ceramic system co-doped with rare earth-rare earth ions and rare earth-transition metal group ions is adopted to obtain a multilayer composite structure ceramic material, the red light spectrum enhancement can be realized, and the crystal structure and, realizing the red shift of the spectrum and the spectrum broadening.
The working principle of the invention is as follows:
preparing a ceramic wafer template, wherein the substrate template is fluorescent transparent ceramic with a YAG (yttrium aluminum garnet)/Ce/(Gd, Y) AG and Ce double-layer composite structure, and when the substrate template is prepared, the fluorescent transparent ceramic with the YAG/Ce/(Gd, Y) AG and Ce double-layer composite structure is prepared by adopting the components and the structural design of a garnet-structure phosphor and changing Gd3+The doping concentration of the organic electroluminescent material enables the color temperature to be controllable within the range of 3100k-3600k, the luminous efficiency reaches 109.9lm/w, and the organic electroluminescent material is in the baseThe upper surface and the lower surface of the substrate are paved with a layer of metal nano-shell template, the metal nano-shell template is synthesized by a metal particle film, the metal nano-particle film is prepared by an electroless chemical deposition method or a wet coating technology, the metal nano-particle film material adopts metal nano-particles with the diameter of 40nm, the metal particles are selected from gold, platinum, silver or copper materials, the substrate template and the metal nano-shell template form a substrate, the plasmon resonance effect can be extended to an infrared light wave band by changing the composition of the substrate, the plasmon resonance frequency can be adjusted to an infrared region by changing the core-shell ratio of the metal nano-shell template, a group of electro-optic memory ceramic pieces are respectively arranged on the upper layer and the lower layer of the substrate, the electro-optic memory ceramic pieces adopt lead zirconate titanate lanthanum composite ceramic obtained by adding rare earth lanthanum into lead zirconate titanate ceramic, and a multi-template combined gel injection molding technology is adopted, bonding and molding the substrate template and the electro-optical memory ceramic wafer, and combining a medium-temperature heating sintering stage and a high-temperature heat preservation completion sintering stage of a sintering process to prepare the large-size fluorescent ceramic wafer, wherein in the high-temperature heat preservation completion sintering stage, the fluorescent ceramic wafer forms a large number of closed pores and is continuously reduced, so that the pore size and the pore total number are reduced, the sintered body density is obviously increased, and a high-precision ceramic cutting machine is adopted to cut the large-size fluorescent ceramic wafer into the required size and shape.
Finally, it should be noted that: first, the present invention has been described in detail by the general description and the specific embodiments, but on the basis of the present invention, the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention;
secondly, the method comprises the following steps: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (8)
1. A preparation method for preparing a large-size ultrathin fluorescent ceramic wafer by one-step forming is characterized by comprising the following steps: the preparation method comprises the following steps:
s1: preparing a ceramic wafer template, wherein the substrate template is made of fluorescent transparent ceramic with a YAG (yttrium aluminum garnet)/Ce/(Gd, Y) AG and Ce double-layer composite structure, a layer of metal nano-shell template is paved on the upper surface and the lower surface of the substrate, the metal nano-shell template is synthesized by a metal particle film, the metal nano-particle film is prepared by adopting an electroless chemical deposition method or a wet coating technology, and a group of electro-optical memory ceramic wafers are additionally arranged on the upper layer and the lower layer of the substrate;
s2: forming, namely bonding and forming the substrate template and the electro-optical memory ceramic wafer by adopting a multi-template combined gel injection forming technology, and then combining a medium-temperature heating sintering stage and a high-temperature heat preservation completion sintering stage of a sintering process to prepare a large-size fluorescent ceramic wafer;
s3: and cutting, namely cutting the large-size fluorescent ceramic wafer into the required size and shape by adopting a high-precision ceramic cutting machine.
2. The method for preparing the large-size ultrathin fluorescent ceramic sheet by one-step molding according to claim 1, characterized in that: in the step S1, Gd is changed during the fabrication of the substrate template3+The doping concentration of the organic electroluminescent material enables the color temperature to be controllable in the range of 3100k-3600k, and the luminous efficiency reaches 109.9 lm/w.
3. The method for preparing the large-size ultrathin fluorescent ceramic sheet by one-step molding according to claim 1, characterized in that: the metal nanoparticle film material in S1 adopts metal nanoparticles with the diameter of 40nm, and the metal particles are selected from gold, platinum, silver or copper materials.
4. The method for preparing the large-size ultrathin fluorescent ceramic sheet by one-step molding according to claim 1, characterized in that: the electro-optical memory ceramic sheet in S1 is a lead lanthanum zirconate titanate composite ceramic obtained by adding rare earth lanthanum into lead zirconate titanate ceramic.
5. The method for preparing the large-size ultrathin fluorescent ceramic sheet by one-step molding according to claim 1, characterized in that: in the sintering stage of finishing high-temperature heat preservation in the S2, the fluorescent ceramic sheet forms a large number of closed pores and is continuously reduced, so that the size and the total number of the pores are reduced, and the density of a sintered body is obviously increased.
6. The method for preparing the large-size ultrathin fluorescent ceramic sheet by one-step molding according to claim 1, characterized in that: the fluorescent transparent ceramic with the YAG: Ce/(Gd, Y) AG: Ce double-layer composite structure in the S1 is prepared by adopting the components and the structural design of a garnet-structured phosphor.
7. The method for preparing the large-size ultrathin fluorescent ceramic sheet by one-step molding according to claim 1, characterized in that: in the step S1, the substrate template and the metal nano-shell template form a substrate, and the plasmon resonance effect can be extended to an infrared band by changing the composition of the substrate.
8. The method for preparing the large-size ultrathin fluorescent ceramic sheet by one-step molding according to claim 1, characterized in that: in the step S1, the plasmon resonance frequency can be adjusted to the infrared region by changing the core-shell ratio of the metal nanoshell template.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI829330B (en) * | 2021-09-10 | 2024-01-11 | 美商賀利氏科納米北美有限責任公司 | Uv-activated red ceramic bodies comprising yag for use in semiconductor processing chambers |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI829330B (en) * | 2021-09-10 | 2024-01-11 | 美商賀利氏科納米北美有限責任公司 | Uv-activated red ceramic bodies comprising yag for use in semiconductor processing chambers |
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