CN115322619A - White ink and preparation method thereof, LED ceramic packaging substrate and light source - Google Patents
White ink and preparation method thereof, LED ceramic packaging substrate and light source Download PDFInfo
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- CN115322619A CN115322619A CN202211113295.4A CN202211113295A CN115322619A CN 115322619 A CN115322619 A CN 115322619A CN 202211113295 A CN202211113295 A CN 202211113295A CN 115322619 A CN115322619 A CN 115322619A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
Abstract
The application belongs to the technical field of materials, and particularly relates to white ink and a preparation method thereof, an LED packaging ceramic substrate and a light source. The white ink comprises 100 parts of a main agent of raw material components, wherein the main agent comprises 50-75 parts of an acrylic resin system, 25-48 parts of nano pigment particles, 0-2 parts of an initiator, 1-5 parts of an auxiliary agent, 0.1-20 parts of an accelerator and 10-100 parts of a solvent. According to the white ink, through the matching effect of the raw material components, the white ink has high wettability and adhesiveness to the ceramic substrate, and is beneficial to stable and firm combination of a white ink coating on the surface of the ceramic substrate to form an aging-resistant and high-low temperature cycle-resistant white ink coating; and the formed white ink coating has high reflectivity, and has small loss on the light emitting efficiency of the LED chip after being applied to a device, thereby being beneficial to improving the light efficiency of the device.
Description
Technical Field
The application belongs to the technical field of materials, and particularly relates to white ink and a preparation method thereof, an LED ceramic packaging substrate and a light source.
Background
Because the ceramic substrate has good heat resistance, thermal conductivity and stability, a ceramic package LED (Light Emitting Diode) is a good solution for a high power density Light source. But because pottery itself has certain absorbance, there is the extinction area also on the circuit layer of surface covering simultaneously, can reduce the luminous efficiency of LED lamp pearl to lead to the heat to gather, restricted ceramic package LED's light efficiency and further promoted, reduced the reliability. The reflectivity of the ceramic substrate is improved mainly by covering the surface of the substrate with a white light-reflecting material.
At present, a common method is to coat a substrate with a white ink material dedicated to a photosensitive developing type LED. The method is widely applied to the circuit board for the LED, and can improve the light emitting efficiency of the LED lamp. However, such inks are often used on conventional organometallic substrates, and for applications on ceramic substrates, it is desirable to overcome the drawbacks of wettability and adhesion. In addition, it is desirable to have good aging resistance and high and low temperature cycle performance. Meanwhile, the reflectivity needs to be improved, and the light efficiency of the device is improved.
Therefore, the problems of poor wettability and cohesiveness, low reflectivity and poor aging performance of the existing white ink material need to be overcome, and a novel white reflective material special for the ceramic substrate LED and an implementation mode thereof need to be developed.
Disclosure of Invention
The application aims to provide white ink and a preparation method thereof, an LED ceramic packaging substrate and a light source, and aims to solve the problems of poor wettability and cohesiveness, low reflectivity and poor aging performance of the conventional white ink on the ceramic substrate to a certain extent.
In order to achieve the purpose of the application, the technical scheme adopted by the application is as follows:
in a first aspect, the application provides a white ink, which comprises the following raw material components in parts by weight:
wherein the main agent comprises 50-75 parts of acrylic resin system, 25-48 parts of nano pigment particles and 0-2 parts of initiator.
In a second aspect, the present application provides a method for preparing a white ink, comprising the steps of:
the white ink is obtained by mixing the main agent, the auxiliary agent, the accelerant and the solvent in the formula amount.
In a third aspect, the present application provides an LED ceramic package substrate, which includes a ceramic substrate and a white ink coating bonded on the surface of the ceramic substrate, wherein the white ink coating is made of the above white ink or the white ink prepared by the above method.
In a fourth aspect, the present application provides a light source, the light source includes an LED chip and a ceramic package substrate for encapsulating the LED chip, the ceramic package substrate employs the above LED ceramic package substrate.
In the white ink provided by the first aspect of the application, the acrylic resin system enables the white ink to have good adhesion performance with a ceramic substrate, the accelerant improves the wettability and adhesion of the white ink on the surface of the ceramic substrate, the ceramic substrate is pretreated by the accelerant to form a functional active surface, and the interaction between the raw material components in the white ink and the functionally activated surface realizes stronger wettability and adhesion on the ceramic substrate. The nano pigment particles can improve the dispersion characteristic of the white ink, so that the white ink and the ceramic substrate have stronger interaction; the reflectivity of the white ink coating can be improved, and the white ink is applied to a device, so that the light efficiency of the device is improved. The auxiliary agent can improve the dispersibility, stability, leveling property, film forming property and other properties of the white ink.
According to the preparation method of the white ink provided by the second aspect of the application, the main agent, the auxiliary agent, the accelerator and the solvent in the formula amount in the white ink are mixed, so that the raw material components are uniformly mixed, and the white ink can be obtained. Through the matching effect of the raw material components, the white ink has higher wettability and adhesiveness to the ceramic substrate, and is favorable for stably and firmly combining the white ink coating on the surface of the ceramic substrate to form an aging-resistant and high-low temperature cycle-resistant white ink coating; and the formed white ink coating has high reflectivity, and the loss of the light-emitting efficiency of the LED chip is small after the white ink coating is applied to a device, so that the light efficiency of the device is improved.
The utility model provides a LED ceramic packaging substrate, because ceramic substrate surface combines the white printing ink coating that above-mentioned white printing ink made, this white printing ink coating combines stably and firmly with ceramic substrate, has characteristics such as ageing-resistant, resistant high low temperature cycle, reflectivity height, has improved LED ceramic packaging substrate to the packaging effect of LED chip, and the light-emitting efficiency to the LED chip subtracts the loss for a short time simultaneously, is favorable to improving the light efficiency of device.
The light source that this application fourth aspect provided, because the ceramic packaging substrate that the LED chip adopted above-mentioned LED chip encapsulates, not only improved the stability of LED chip, this LED chip's ceramic packaging substrate has characteristics such as reflectivity height, ageing-resistant, resistant high low temperature cycle moreover, improves the light efficiency and the life of light source.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a schematic flow chart of a preparation method of a white ink provided in an embodiment of the present application.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application more clearly apparent, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
In this application, the term "and/or" describes an association relationship of associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a alone, A and B together, and B alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In the present application, "at least one" means one or more, "a plurality" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items. For example, "at least one (one) of a, b, or c," or "at least one (one) of a, b, and c," may each represent: a, b, c, a-b (i.e. a and b), a-c, b-c, or a-b-c, wherein a, b, and c can be single or multiple respectively.
It should be understood that, in various embodiments of the present application, the sequence number of each process does not mean the execution sequence, some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its function and inherent logic, and should not constitute any limitation to the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the examples of this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weight of the related components mentioned in the examples of the present application may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components according to the examples of the present application is scaled up or down within the scope disclosed in the examples of the present application. Specifically, the mass in the examples of the present application may be in units of mass known in the chemical field such as μ g, mg, g, kg, etc.
The terms "first" and "second" are used for descriptive purposes only and are used for distinguishing purposes such as substances from one another and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. For example, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX, without departing from the scope of embodiments of the present application. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
The first aspect of the embodiments of the present application provides a white ink, which comprises the following raw material components in parts by weight:
wherein the main agent comprises 50-75 parts of acrylic resin system, 25-48 parts of nano pigment particles and 0-2 parts of initiator.
The white ink provided by the first aspect of the embodiment of the application comprises 100 parts of raw material components of a main agent, wherein the main agent comprises 50-75 parts of an acrylic resin system, 25-48 parts of nano pigment particles, 0-2 parts of an initiator, 1-5 parts of an auxiliary agent, 0.1-20 parts of an accelerator and 10-100 parts of a solvent. The acrylic resin system enables the white ink and the ceramic substrate to have good bonding performance, the accelerant improves the wettability and the bonding performance of the white ink on the surface of the ceramic substrate, the ceramic substrate is pretreated through the accelerant to form a functional active surface, and the interaction between the raw material components in the white ink and the functionally activated surface realizes stronger wettability and bonding performance on the ceramic substrate. The nano pigment particles can improve the dispersion characteristic of the white ink, so that the white ink and the ceramic substrate have stronger interaction; the reflectivity of the white ink coating can be improved, and the white ink is applied to a device, so that the light efficiency of the device is improved. The auxiliary agent can improve the performances of the white ink such as dispersibility, stability, leveling property, film forming property and the like. According to the white ink provided by the embodiment of the application, through the matching effect of the raw material components, the white ink has high wettability and adhesiveness to the ceramic substrate, and is beneficial to stably and firmly bonding the white ink coating on the surface of the ceramic substrate to form the aging-resistant and high-low temperature cycle-resistant white ink coating; and the formed white ink coating has high reflectivity, and has small loss on the light emitting efficiency of the LED chip after being applied to a device, thereby being beneficial to improving the light efficiency of the device.
According to the embodiment of the application, the proportion of the raw material components in the white ink ensures the wettability and the adhesiveness of the white ink to the ceramic substrate, and the aging resistance, the high and low temperature cycle resistance, the light reflectivity and other comprehensive properties of a coating formed by the white ink. If the content of the resin system in the base material is too high, the content of the nanopigment particles is reduced, thereby reducing the reflectance of the white ink coating layer, and if the content of the nanopigment particles is too high, the dispersibility of the white ink is affected, thereby affecting the moldability of the white ink. If the content of the auxiliary is too small, it is not preferable to improve the dispersion stability, leveling property, film forming property and the like of the white ink, and it is also not preferable to improve the adhesion between the white ink and the substrate. If the content of the additive is too large, the mechanical properties of the white ink coating are reduced, thereby reducing the aging properties of the white ink coating. If the solvent content is too large or too small, the workability such as film forming property of the white ink and the dispersibility of each component are affected. If the content of the accelerant is too small, the functional activation treatment of the white ink on the surface of the ceramic substrate is influenced, so that the bonding performance of the white ink coating and the ceramic substrate is influenced; if the content of the accelerator is too large, the accelerator can cause self interaction, so that the surface of the ceramic substrate is abnormally functionalized, and the white ink coating is not favorably combined on the surface of the ceramic substrate.
In some embodiments, the acrylic resin system comprises: at least one of organosilicon modified acrylic resin and acrylic resin; the acrylic resin is a polymer formed by modifying chemical components such as methyl methacrylate, ethyl methacrylate, butyl methacrylate and the like through hydroxyl, carboxyl and the like. Due to the unsaturated double bond 'C = C', this unsaturation, under uv irradiation, activates the initiator to initiate the chain reaction, polymerizing into a solid resin. The organic silicon modified acrylic resin is a modified resin prepared by reacting polyacrylic phenol resin containing active groups with organic silicon oligomer containing active hydroxyl (or alkoxy), and has the characteristics of no foaming, no falling off, no color change, high heat resistance, high weather resistance and the like after soaking.
In some embodiments, the nanopigment particles comprise silane-modified nanopitanium dioxide; the silane-modified nano titanium dioxide has better dispersion performance in a solvent, and can be stably and uniformly dispersed in the white ink, so that the stability and the film forming uniformity of the white ink are improved, and a coating formed by the white ink has a better reflection effect on the luminescence of an LED chip.
In some embodiments, the nanopigment particles have a particle size of 200 to 400nm; the excessively small particle size causes diffraction of light due to the nano-size effect, and the reflectance with respect to visible light is reduced to enhance the shielding effect with respect to ultraviolet rays. Too large a particle size may reduce the stability and distribution of the ink, and may also reduce the reflectance.
In some embodiments, the initiator includes a photosensitizer and a thermal decomposition initiator. According to the embodiment of the application, the initiator in the white ink simultaneously comprises the photosensitizer and the thermal decomposition initiator, wherein the photosensitizer mainly plays a role in realizing pre-curing after the white ink is deposited on the ceramic substrate, the thermal decomposition initiator plays a role in temperature control curing, and the photosensitizer and the thermal decomposition initiator are synergistic to ensure that the white ink has better curing film-forming performance.
In some embodiments, the mass ratio of photosensitizer to thermal decomposition initiator in the initiator is 1: (3-5); the photosensitizer plays a role in pre-curing, the thermal decomposition initiator plays a role in temperature control curing, and the two synergistically control the formability and reliability of the ink layer.
In some embodiments, the photosensitizer comprises at least one of TPO (2, 4, 6-trimethylbenzoyl-diphenylphosphine oxide), 184 (1-hydroxy-cyclohexyl-phenyl-methanone).
In some embodiments, the thermal decomposition initiator comprises at least one of TAPO (cleavage type free radical photoinitiator), TBPA (tetrabromophthalic anhydride), TAPA (tris (4-aminophenyl) amine).
In some embodiments, the accelerator comprises a silane coupling agent. In some embodiments, the silane coupling agent includes, but is not limited to, at least one of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, glycidoxypropyltrimethoxysilane, methacryloxypropyltrimethoxysilane, mercaptopropyltrimethoxysilane, and aminoethylaminopropyltrimethoxysilane. The silane coupling agent accelerator adopted in the embodiment of the application is used for preprocessing a ceramic substrate in the process of the ceramic substrate by a white ink material, a functional active surface is formed by preprocessing the ceramic substrate by the accelerator, and the interaction between the raw material components in the white ink and the functionally activated surface realizes stronger wettability and adhesiveness on the ceramic substrate.
In some embodiments, the adjuvant comprises at least one of a defoamer, a leveling agent, a plasticizer, a thickener, a toughener, a filler, a surfactant, an emulsifier, a dispersant, an antistatic agent, a mold inhibitor, an antiskinning agent, a matting agent, a light stabilizer, an antioxidant. In some embodiments, defoamers include, but are not limited to, BYK-019 defoamers; leveling agents include, but are not limited to, polyether modified silicones, polyester modified silicones, polyacrylates, acrylic urethane resins, polydimethylsiloxanes, polymethylphenylsiloxanes, organo-modified polysiloxanes, and the like; plasticizers include, but are not limited to, at least one of bisphenol a, tetrabromobisphenol a, alkyl phthalates; thickeners include, but are not limited to, alginic acid esters of benzene glycols; the toughening agent comprises but is not limited to one or more of trimethylolpropane triglycidyl ether, glycerol triglycidyl ether, polypropylene glycol diglycidyl ether or resorcinol diglycidyl ether; fillers include, but are not limited to, titanium dioxide and the like; surfactants include, but are not limited to, sodium dodecylbenzene sulfonate and the like. Emulsifiers include, but are not limited to, one or more of tall oil fatty acids, dimerized fatty acids, white petrolatum, hydrogenated polyisobutene; antistatic agents include, but are not limited to, fatty acid amides; light stabilizers include, but are not limited to, carbon black and hindered amine light stabilizers; the antioxidant includes but is not limited to any one or a mixture of more than one of 2, 6-di-tert-butyl-p-cresol, tetra [ B- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and B- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester.
In some embodiments, the adjuvant comprises at least one dispersant of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, glycidyloxypropyltrimethoxysilane, methacryloxypropyltrimethoxysilane, mercaptopropyltrimethoxysilane, aminoethylaminopropyltrimethoxysilane, monoalkoxy titanate coupling agents, monoalkoxy phosphate titanate coupling agents, monoalkoxy unsaturated fatty acid titanates, oxoacetate bis (dioctylphosphate) titanate. The dispersing agents are beneficial to improving the dispersion stability of each raw material component in the white ink.
In some embodiments, the solvent includes at least one of toluene, xylene, methanol, ethanol, n-propanol, n-hexane, cyclohexane, propylene glycol methyl ether, dipropylene glycol methyl ether, and ethylene glycol butyl ether, and these solvents have a good dissolving/dispersing effect on raw material components such as resin, nano pigment particles, promoters, and additives in the white ink, so that the white ink can form a slurry with stable dispersion, which is beneficial for the white ink to deposit a film to form a coating with uniform thickness, flat film layer, and firm bonding with the ceramic substrate.
In some embodiments, the composition comprises the following raw material components in parts by weight:
wherein the main agent comprises 50-75 parts of acrylic resin system, 25-48 parts of nano pigment particles and 0.1-2 parts of initiator. According to the white ink, the white ink has better wettability and adhesiveness to a ceramic substrate, and a coating formed by the white ink has better aging resistance, high and low temperature cycle resistance, light reflectivity and other comprehensive properties.
As shown in fig. 1, a second aspect of the embodiments of the present application provides a method for preparing a white ink, including the following steps:
in S10, the main agent, the auxiliary agent, the accelerator and the solvent in the formula amount in the white ink are obtained and mixed to obtain the white ink.
In the method for preparing the white ink according to the second aspect of the embodiments of the present application, the white ink can be obtained by mixing the main agent, the auxiliary agent, the accelerator, and the solvent in the formula amounts to uniformly mix the raw material components. Through the matching effect of the raw material components, the white ink has higher wettability and adhesiveness to the ceramic substrate, and is favorable for stably and firmly combining the white ink coating on the surface of the ceramic substrate to form an aging-resistant and high-low temperature cycle-resistant white ink coating; and the formed white ink coating has high reflectivity, and has small loss on the light emitting efficiency of the LED chip after being applied to a device, thereby being beneficial to improving the light efficiency of the device.
In some embodiments, the white ink comprises the following raw material components in parts by weight: 100 parts of main agent, 1-5 parts of auxiliary agent, 0.1-20 parts of accelerant and 10-100 parts of solvent, wherein the main agent comprises 50-75 parts of acrylic resin system, 25-48 parts of nano pigment particles and 0-2 parts of initiator. Further, the white ink comprises the following raw material components in parts by weight: 100 parts of main agent, 1-5 parts of auxiliary agent, 5-20 parts of accelerant and 10-100 parts of solvent, wherein the main agent comprises 50-75 parts of acrylic resin system, 25-48 parts of nano pigment particles and 0.1-2 parts of initiator.
In some embodiments, the acrylic resin system comprises: at least one of organosilicon modified acrylic resin and acrylic resin;
in some embodiments, the nanopigment particles comprise silane-modified nanopitanium dioxide. In some embodiments, the nanopigment particles have a particle size of 200 to 400nm.
In some embodiments, the initiator includes a photosensitizer and a thermal decomposition initiator. In some embodiments, the mass ratio of photosensitizer to thermal decomposition initiator in the initiator is 1: (3-5); wherein the photosensitizer comprises at least one of TPO (2, 4, 6-trimethylbenzoyl-diphenylphosphine oxide) and 184 (1-hydroxy-cyclohexyl-phenyl ketone), and the thermal decomposition initiator comprises at least one of TAPO (cleavage type radical photoinitiator), TBPA (tetrabromophthalic anhydride), TAPA (tris (4-aminophenyl) amine).
In some embodiments, the accelerator comprises a silane coupling agent. In some embodiments, the adjuvant comprises at least one dispersant of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, glycidoxypropyltrimethoxysilane, methacryloxypropyltrimethoxysilane, mercaptopropyltrimethoxysilane, aminoethylaminopropyltrimethoxysilane, monoalkoxy titanate coupling agent, monoalkoxy phosphate titanate coupling agent, monoalkoxy unsaturated fatty acid titanate, oxyacetate bis (dioctylphosphate) titanate.
In some embodiments, the adjuvant comprises at least one of a defoamer, a leveling agent, a plasticizer, a thickener, a toughener, a filler, a surfactant, an emulsifier, a dispersant, an antistatic agent, a mildewcide, an antiskinning agent, a matting agent, a light stabilizer, an antioxidant. In some embodiments, the silane coupling agent includes, but is not limited to, at least one of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, glycidoxypropyltrimethoxysilane, methacryloxypropyltrimethoxysilane, mercaptopropyltrimethoxysilane, and aminoethylaminopropyltrimethoxysilane.
In some embodiments, the solvent comprises at least one of toluene, xylene, methanol, ethanol, n-propanol, n-hexane, cyclohexane, propylene glycol methyl ether, dipropylene glycol methyl ether, ethylene glycol butyl ether.
The technical effects of the embodiments of the present application are discussed in the foregoing, and are not described herein again.
In a third aspect of the embodiments of the present application, an LED ceramic package substrate is provided, which includes a ceramic substrate and a white ink coating bonded to a surface of the ceramic substrate, wherein the white ink coating is made of white ink.
The LED ceramic packaging substrate provided by the third aspect of the embodiment of the application has the advantages that the white ink coating made of the white ink is combined on the surface of the ceramic substrate, the white ink coating is stably and firmly combined with the ceramic substrate, and the LED ceramic packaging substrate has the characteristics of aging resistance, high and low temperature cycle resistance, high reflectivity and the like, so that the packaging effect of the LED ceramic packaging substrate on an LED chip is improved, meanwhile, the loss of the light emitting efficiency of the LED chip is reduced, and the improvement of the light efficiency of a device is facilitated.
In some embodiments, preparing a white ink coating from a white ink comprises the steps of:
s20, depositing an accelerant on the surface of the cleaned ceramic substrate, and standing for 15-30 minutes at the temperature of 105-120 ℃ to obtain a pre-deposited ceramic substrate; the ceramic substrate is pretreated by the accelerant to form a functional active surface, and the interaction between the raw material components in the white ink and the functionally active surface realizes stronger wettability and adhesiveness for the ceramic substrate.
In some embodiments, the ceramic substrate is first cleaned using a Plasma cleaner to remove oxides and contaminants from the substrate surface.
In some embodiments, it is preferable that the deposition thickness of the accelerator on the surface of the ceramic substrate is not more than 30 μm, which is more advantageous to ensure the bonding stability and the adhesion of the white ink coating.
S30, mixing the main agent, the auxiliary agent and the solvent into slurry, defoaming, printing the slurry on the surface of a pre-deposited ceramic substrate, pre-curing the slurry by adopting a developing technology, drying the pre-deposited ceramic substrate for 10 to 20 minutes at the temperature of between 100 and 110 ℃, and drying the pre-deposited ceramic substrate for 2 to 4 hours at the temperature of between 150 and 170 ℃ to form a white ink coating.
In some embodiments, the pre-cure conditions include: baking for 10-30 minutes at 80-100 ℃ and drying the surface; a film sheet prepared in advance is placed on the 3D sprayed ink concave surface, and the gap between the film and the edge of the glass is about 0.1mm. Then, the film is exposed at a position 25-30 mm above the film by using an LED parallel light source, and the exposure energy is controlled to be 1000 +/-100 mj/cm 2 And the thickness of the pre-cured printing ink is 13-15um.
A fourth aspect of the embodiments of the present application provides a light source, where the light source includes an LED chip and a ceramic package substrate for packaging the LED chip, and the ceramic package substrate is an LED ceramic package substrate.
According to the light source provided by the fourth aspect of the embodiment of the application, the LED chip is packaged by adopting the ceramic packaging substrate of the LED chip, so that the stability of the LED chip is improved, and the ceramic packaging substrate of the LED chip has the characteristics of high reflectivity, aging resistance, high and low temperature cycle resistance and the like, so that the light efficiency of the light source is improved, and the service life of the light source is prolonged.
In order to make the details and operation of the present application clearly understood by those skilled in the art, and the examples of the present application, the white ink and the preparation method thereof, and the LED packaging ceramic substrate, the technical solution is illustrated by several examples.
Example 1
A white ink comprises the following raw material components: 50 parts of organic silicon modified acrylic resin, 50 parts of silane modified nano titanium dioxide with the particle size of 300nm, 3 parts of propyl trimethoxy silane dispersing agent, 1 part of TPO photosensitizer, 2 parts of TAPA thermal decomposition initiator, 80 parts of alcohol ether and 10 parts of silane accelerator.
An LED packaging ceramic substrate is prepared by the following steps:
(1) the method comprises the following steps of (1) cleaning a ceramic substrate by Plasma to remove oxides and pollutants on the surface of the substrate;
(2) spraying the accelerant on the surface of the substrate, standing at 105 ℃ for 15 minutes at constant temperature, wherein the coating thickness of the accelerant is preferably not higher than 30um for covering the surface of the substrate.
(3) Fully mixing other components of the white ink material in proportion and defoaming, and then printing the white ink material to a corresponding position of a substrate by adopting screen printing;
(4) carrying out precuring on the white ink material by adopting a developing technology, wherein the precuring conditions are as follows: baking at 80 ℃ for 10 minutes, and drying the surface; a film sheet prepared in advance is placed on the 3D sprayed ink concave surface, and the gap between the film and the edge of the glass is 0.1mm. Then, the film is exposed by a parallel light source of an LED at a position 25mm above the film, and the exposure energy is controlled to be 1000 +/-100 mj/cm 2 And the thickness of the ink is 13-15um.
(5) And baking the substrate at 105 ℃ for 15 minutes, and then baking the substrate at 160 ℃ for 3 hours to form a white ink coating, thereby obtaining the LED packaging ceramic substrate.
A light source is packaged by using an LED packaging ceramic substrate, specifically,
firstly, the LED packaging ceramic substrate is cleaned by Plasma to remove oxides and pollutants on the surface of the substrate; coating a nano silver colloid solid crystal material at the designed position; placing the LED chip at an appropriate position according to a designed program, baking to complete die bonding, and fixing the LED chip on the LED packaging ceramic substrate; and performing other packaging procedures on the solid crystal material to improve the light emitting effect and protect the chip, and finally obtaining the light source.
Example 2
A white ink comprises the following raw material components: 60 parts of organic silicon modified acrylic resin, 40 parts of silane modified nano titanium dioxide with the particle size of 300nm, 3 parts of propyl trimethoxy silane dispersing agent, 1 part of TPO photosensitizer, 2 parts of TAPA thermal decomposition initiator, 80 parts of alcohol ether and 10 parts of silane accelerator.
An LED packaging ceramic substrate is prepared by the following steps:
(1) the method comprises the following steps of (1) cleaning a ceramic substrate by Plasma to remove oxides and pollutants on the surface of the substrate;
(2) spraying the accelerant on the surface of the substrate, standing at 105 ℃ for 15 minutes at constant temperature, wherein the coating thickness of the accelerant is preferably not higher than 30um for covering the surface of the substrate.
(3) Fully mixing other components of the white ink material in proportion and defoaming, and then printing the white ink material to a corresponding position of a substrate by adopting screen printing;
(4) carrying out precuring on the white ink material by adopting a developing technology, wherein the precuring conditions are as follows: baking at 80 ℃ for 10 minutes, and drying the surface; a film sheet prepared in advance is placed on the 3D sprayed ink concave surface, and the gap between the film and the edge of the glass is 0.1mm. Then, the film is exposed by a parallel light source of an LED at a position 25mm above the film, and the exposure energy is controlled to be 1000 +/-100 mj/cm 2 And the thickness of the ink is 13-15um.
(5) And baking the substrate at 105 ℃ for 15 minutes, and then baking the substrate at 160 ℃ for 3 hours to form a white ink coating, thereby obtaining the LED packaging ceramic substrate.
A light source is packaged by using an LED packaging ceramic substrate, specifically,
firstly, the LED packaging ceramic substrate is cleaned by Plasma to remove oxides and pollutants on the surface of the substrate; coating a nano silver colloid solid crystal material at the designed position; placing the LED chip at an appropriate position according to a designed program, baking to complete die bonding, and fixing the LED chip on the LED packaging ceramic substrate; and performing other packaging procedures on the solid crystal material to improve the light emitting effect and protect the chip, and finally obtaining the light source.
Example 3
A white ink comprises the following raw material components: 70 parts of organic silicon modified acrylic resin, 30 parts of silane modified nano titanium dioxide with the particle size of 300nm, 3 parts of propyl trimethoxy silane dispersing agent, 1 part of TPO photosensitizer, 2 parts of TAPA thermal decomposition initiator, 80 parts of alcohol ether and 10 parts of silane accelerator.
An LED packaging ceramic substrate is prepared by the following steps:
(1) the method comprises the following steps of (1) cleaning a ceramic substrate by Plasma to remove oxides and pollutants on the surface of the substrate;
(2) spraying the accelerant on the surface of the substrate, standing for 15 minutes at the constant temperature of 105 ℃, wherein the coating thickness of the accelerant is preferably not higher than 30um for covering the surface of the substrate.
(3) Fully mixing other components of the white ink material in proportion and defoaming, and then printing the white ink material to a corresponding position of a substrate by adopting screen printing;
(4) carrying out precuring on the white ink material by adopting a developing technology, wherein the precuring conditions are as follows: baking at 80 ℃ for 10 minutes, and drying the surface; a film sheet prepared in advance is placed on the 3D sprayed ink concave surface, and the gap between the film and the edge of the glass is 0.1mm. Then, the film is exposed by a parallel light source of an LED at a position 25mm above the film, and the exposure energy is controlled to be 1000 +/-100 mj/cm 2 And the thickness of the ink is 13-15um.
(5) And baking the substrate at 105 ℃ for 15 minutes, and then baking at 160 ℃ for 3 hours to form a white ink coating, thereby obtaining the LED packaging ceramic substrate.
A light source is packaged by using an LED packaging ceramic substrate, specifically,
firstly, the LED packaging ceramic substrate is cleaned by Plasma to remove oxides and pollutants on the surface of the substrate; coating a nano silver colloid solid crystal material at the designed position; placing the LED chip at an appropriate position according to a designed program, baking to complete die bonding, and fixing the LED chip on the LED packaging ceramic substrate; and performing other packaging procedures on the solid crystal material to improve the light emitting effect and protect the chip, and finally obtaining the light source.
Comparative example 1
A white ink comprises the following raw material components: 50 parts of acrylic resin, 50 parts of silane modified nano titanium dioxide with the particle size of 300nm, 3 parts of propyl trimethoxy silane dispersing agent, 1 part of TPO photosensitizer, 2 parts of TAPA thermal decomposition initiator, 80 parts of alcohol ether and 10 parts of silane accelerator.
An LED packaging ceramic substrate is prepared by the following steps:
(1) the method comprises the following steps of (1) cleaning a ceramic substrate by Plasma to remove oxides and pollutants on the surface of the substrate;
(2) spraying the accelerant on the surface of the substrate, standing at 105 ℃ for 15 minutes at constant temperature, wherein the coating thickness of the accelerant is preferably not higher than 30um for covering the surface of the substrate.
(3) Fully mixing other components of the white ink material in proportion and defoaming, and then printing the white ink material to a corresponding position of a substrate by adopting screen printing;
(4) carrying out pre-curing on the white ink material by adopting a developing technology, wherein the pre-curing conditions are as follows: baking at 80 ℃ for 10 minutes, and drying the surface; a film sheet prepared in advance is placed on the 3D sprayed ink concave surface, and the gap between the film and the edge of the glass is 0.1mm. Then, the film is exposed by a parallel light source of an LED at a position 25mm above the film, and the exposure energy is controlled to be 1000 +/-100 mj/cm 2 And the thickness of the ink is 13-15um.
(5) And baking the substrate at 105 ℃ for 15 minutes, and then baking the substrate at 160 ℃ for 3 hours to form a white ink coating, thereby obtaining the LED packaging ceramic substrate.
A light source is packaged by using an LED packaging ceramic substrate, specifically,
firstly, the LED packaging ceramic substrate is cleaned by Plasma to remove oxides and pollutants on the surface of the substrate; coating a nano silver colloid solid crystal material at the designed position; placing the LED chip at an appropriate position according to a designed program, baking to complete die bonding, and fixing the LED chip on the LED packaging ceramic substrate; and performing other packaging procedures on the solid crystal material to improve the light emitting effect and protect the chip, and finally obtaining the light source.
Comparative example 2
A white ink comprises the following raw material components: 50 parts of organic silicon modified acrylic resin, 50 parts of nano titanium dioxide with the particle size of 300nm, 3 parts of propyl trimethoxy silane dispersing agent, 1 part of TPO photosensitizer, 2 parts of TAPA thermal decomposition initiator, 80 parts of alcohol ether and 10 parts of silane accelerator.
An LED packaging ceramic substrate is prepared by the following steps:
(1) the method comprises the following steps of (1) cleaning a ceramic substrate by Plasma to remove oxides and pollutants on the surface of the substrate;
(2) spraying the accelerant on the surface of the substrate, standing at 105 ℃ for 15 minutes at constant temperature, wherein the coating thickness of the accelerant is preferably not higher than 30um for covering the surface of the substrate.
(3) Fully mixing other components of the white ink material in proportion and defoaming, and then printing the white ink material to a corresponding position of a substrate by adopting screen printing;
(4) carrying out pre-curing on the white ink material by adopting a developing technology, wherein the pre-curing conditions are as follows: baking at 80 ℃ for 10 minutes, and drying the surface; a film is prepared in advance and is placed on the 3D ink-sprayed concave surface, and the gap between the film and the edge of the glass is 0.1mm. Then, the film is exposed by a parallel light source of an LED at a position 25mm above the film, and the exposure energy is controlled to be 1000 +/-100 mj/cm 2 And the thickness of the ink is 13-15um.
(5) And baking the substrate at 105 ℃ for 15 minutes, and then baking the substrate at 160 ℃ for 3 hours to form a white ink coating, thereby obtaining the LED packaging ceramic substrate.
A light source is packaged by using an LED packaging ceramic substrate, specifically,
firstly, the LED packaging ceramic substrate is cleaned by Plasma to remove oxides and pollutants on the surface of the substrate; coating a nano silver adhesive die bonding material at a designed position; placing the LED chip at an appropriate position according to a designed program, baking to complete die bonding, and fixing the LED chip on the LED packaging ceramic substrate; and carrying out other packaging procedures on the solid crystal material to improve the light emitting effect and protect the chip, and finally obtaining the light source.
Comparative example 3
A commercial white ink comprising the raw material components: 50 parts of epoxy modified resin, 50 parts of silane modified nano titanium dioxide with the particle size of 300nm, 3 parts of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane dispersing agent, 1 part of TPO photosensitizer, 2 parts of TAPA thermal decomposition initiator, 80 parts of alcohol ether and 10 parts of silane accelerator.
An LED packaging ceramic substrate is prepared by the following steps:
(1) the method comprises the following steps of (1) cleaning a ceramic substrate by Plasma to remove oxides and pollutants on the surface of the substrate;
(2) spraying the accelerant on the surface of the substrate, standing at 105 ℃ for 15 minutes at constant temperature, wherein the coating thickness of the accelerant is preferably not higher than 30um for covering the surface of the substrate.
(3) Fully mixing other components of the white ink material in proportion and defoaming, and then printing the white ink material to a corresponding position of a substrate by adopting screen printing;
(4) carrying out pre-curing on the white ink material by adopting a developing technology, wherein the pre-curing conditions are as follows: baking at 80 ℃ for 10 minutes, and drying the surface; a film sheet prepared in advance is placed on the 3D sprayed ink concave surface, and the gap between the film and the edge of the glass is 0.1mm. Then, the film is exposed by a parallel light source of an LED at a position 25mm above the film, and the exposure energy is controlled to be 1000 +/-100 mj/cm 2 And the thickness of the ink is 13-15um.
(5) And baking the substrate at 105 ℃ for 15 minutes, and then baking the substrate at 160 ℃ for 3 hours to form a white ink coating, thereby obtaining the LED packaging ceramic substrate.
A light source is packaged by adopting an LED packaging ceramic substrate, and specifically comprises the following components:
firstly, the LED packaging ceramic substrate is cleaned by Plasma to remove oxides and pollutants on the surface of the substrate; coating a nano silver colloid solid crystal material at the designed position; placing the LED chip at an appropriate position according to a designed program, baking to complete die bonding, and fixing the LED chip on the LED packaging ceramic substrate; and carrying out other packaging procedures on the solid crystal material to improve the light emitting effect and protect the chip, and finally obtaining the light source.
Further, in order to verify the advancement of the examples of the present application, the following performance tests were respectively performed on each of the examples and comparative examples:
1. reflectance ratio: the reflectance of the white ink coating formed on the LED encapsulating ceramic substrates prepared in each of the examples and comparative examples and the reflectance after 1000 hours of aging were measured according to the GJB 5023.2-2003 standard, and the results are shown in table 1 below:
2. peel strength: the peel strength of the white ink coating formed on the ceramic substrate for LED package prepared in each of the examples and comparative examples was measured using a portable adhesion tester according to ASTM D4541-17, and the results are shown in table 1 below:
3. salt spray test: according to GB/T2423.17-2008' test Ka of basic environmental test rules of electrical and electronic products: salt spray test method and GB/T2423.18-2000 environmental test for Electrical and electronic products part 2: test Kb: salt spray, alternating (sodium chloride solution) standard, salt spray tests were performed on the white ink coatings formed on the LED-encapsulated ceramic substrates prepared in each of the examples and comparative examples, and the test results are shown in table 1 below:
TABLE 1
According to the test results, the white ink coatings prepared on the LED packaging ceramic substrate by the white ink formulas in the embodiments 1 to 3 of the application show high reflectivity and aging resistance, keep high reflectivity after aging for 1000 hours, and have good bonding stability with the ceramic substrate, high peel strength and low possibility of falling off of the white ink coatings. In addition, the white ink coating has excellent stability in a salt spray test, and further shows that the white ink coating formed on the ceramic substrate has good bonding stability with the ceramic substrate, chemical corrosion resistance, excellent weather resistance and long service life of the LED packaging ceramic substrate.
In contrast, the white ink used in comparative example 1, which is not modified with silane, formed a white ink coating with low adhesion strength to the substrate, and which has bubbles in the salt spray test, poor stability, poor chemical resistance, poor weather resistance, and large attenuation of reflectivity after aging. The white ink used in comparative example 2 had pigment particles that were not silane-modified, resulting in poor dispersibility, a white ink coating formed having a low reflectance and poor reflectance stability, and a large attenuation in reflectance after aging. The white ink coating formed by the existing commercial white ink formulation used in comparative example 3 had poor reflection stability and had a large attenuation in reflectance after aging.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. The white ink is characterized by comprising the following raw material components in parts by weight:
wherein the main agent comprises 50-75 parts of acrylic resin system, 25-48 parts of nano pigment particles and 0-2 parts of initiator.
2. The white ink according to claim 1, wherein the acrylic resin system comprises: at least one of organosilicon modified acrylic resin and acrylic resin;
and/or, the nanopigment particles comprise silane-modified nano titanium dioxide;
and/or the initiator comprises a photosensitizer and a thermal decomposition initiator.
3. The white ink according to claim 2, wherein the nanopigment particles have a particle size of 200 to 400nm;
and/or in the initiator, the mass ratio of the photosensitizer to the thermal decomposition initiator is 1: (3-5);
and/or, the photosensitizer comprises at least one of TPO, 184;
and/or the thermal decomposition initiator comprises at least one of TAPO, TBPA and TAPA.
4. The white ink according to claim 3, wherein the accelerator comprises a silane coupling agent;
and/or the auxiliary agent comprises at least one of a defoaming agent, a leveling agent, a plasticizer, a thickening agent, a toughening agent, a filler, a surfactant, an emulsifier, a dispersing agent, an antistatic agent, a mildew inhibitor, an anti-skinning agent, a delustering agent, a light stabilizer and an antioxidant;
and/or the solvent comprises at least one of toluene, xylene, methanol, ethanol, n-propanol, n-hexane, cyclohexane, propylene glycol methyl ether, dipropylene glycol methyl ether and ethylene glycol butyl ether.
5. The white ink according to claim 4, wherein the silane coupling agent includes but is not limited to at least one of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, glycidoxypropyltrimethoxysilane, methacryloxypropyltrimethoxysilane, mercaptopropyltrimethoxysilane, aminoethylaminopropyltrimethoxysilane;
and/or the auxiliary agent comprises at least one dispersing agent of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, glycidyloxypropyltrimethoxysilane, methacryloxypropyltrimethoxysilane, mercaptopropyltrimethoxysilane, aminoethylaminopropyltrimethoxysilane, a monoalkoxy titanate coupling agent, a monoalkoxy phosphate titanate coupling agent, a monoalkoxy unsaturated fatty acid titanate, and oxyacetate bis (dioctyl phosphate) titanate.
6. The white ink according to claim 5, comprising the following raw material components in parts by weight:
wherein the main agent comprises 50-75 parts of acrylic resin system, 25-48 parts of nano pigment particles and 0.1-2 parts of initiator.
7. A preparation method of white ink is characterized by comprising the following steps:
the white ink is obtained by mixing the main agent, the auxiliary agent, the accelerator and the solvent in the amounts specified in the white ink according to any one of claims 1 to 6.
8. An LED ceramic package substrate, characterized in that the LED ceramic package substrate comprises a ceramic substrate and a white ink coating bonded on the surface of the ceramic substrate, wherein the white ink coating is made of the white ink according to any one of claims 1 to 6 or the white ink prepared by the method according to claim 7.
9. The LED ceramic package substrate according to claim 8, wherein preparing the white ink coating from the white ink comprises the steps of:
depositing an accelerant on the surface of the cleaned ceramic substrate, and standing for 15-30 minutes at the temperature of 105-120 ℃ to obtain a pre-deposited ceramic substrate;
mixing a main agent, an auxiliary agent and a solvent into slurry, printing the slurry on the surface of the pre-deposited ceramic substrate, pre-curing the slurry by adopting a developing technology, drying the slurry for 10 to 20 minutes at the temperature of between 100 and 110 ℃, and drying the slurry for 2 to 4 hours at the temperature of between 150 and 170 ℃ to form the white ink coating.
10. A light source, comprising an LED chip and a ceramic package substrate for packaging the LED chip, wherein the ceramic package substrate is the LED ceramic package substrate according to any one of claims 8 to 9.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104955905A (en) * | 2013-02-27 | 2015-09-30 | 株式会社朝日橡胶 | Ink for white reflective film, powder coating, white reflective film and production method thereof, light source mount, and lighting device shade |
| CN114591648A (en) * | 2020-12-07 | 2022-06-07 | 深圳光启高端装备技术研发有限公司 | Ink composition, ink coating and application in printing field |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104955905A (en) * | 2013-02-27 | 2015-09-30 | 株式会社朝日橡胶 | Ink for white reflective film, powder coating, white reflective film and production method thereof, light source mount, and lighting device shade |
| CN114591648A (en) * | 2020-12-07 | 2022-06-07 | 深圳光启高端装备技术研发有限公司 | Ink composition, ink coating and application in printing field |
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| Title |
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| 贺曼罗, vol. 1, 中国石化出版社, pages: 158 - 160 * |
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