Laminate for manufacturing wavelength conversion member and method for manufacturing wavelength conversion member

By using a glass matrix and inorganic phosphor powder with specific compositions in the wavelength conversion component, combined with the configuration of a silica powder restriction layer and low-temperature firing, the problem of poor shape caused by uneven shrinkage of the printed circuit board is solved, and a wavelength conversion component with high transmittance and high refractive index is realized, which is suitable for light-emitting diodes.

CN120676767APending Publication Date: 2025-09-19DAEJOO ELECTRONICS MATERIALS CO LTD
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Patent Information

Application Number
CN202510878194.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Priority Date
2018-09-07
Filing Date
2019-09-09
Publication Date
2025-09-19

AI Technical Summary

Technical Problem

Conventional wavelength conversion components suffer from shape defects due to uneven shrinkage of the printed circuit board during firing, and the formation of the light reflection layer affects the light transmittance and refractive index.

Method used

A printed circuit board containing a glass matrix of specific components and inorganic phosphor powder is used. Silica powder is placed on both side surfaces as a restriction layer A, and a restriction layer B is placed on the non-contact surface. The restriction layers are removed after firing at a temperature below 800°C to form a wavelength conversion component with high transmittance and high refractive index.

Benefits of technology

After firing at a relatively low temperature, the wavelength conversion component has high transmittance and a good shape, making it suitable for light-emitting diodes, etc., and improving optical performance.

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Abstract

The present invention relates to a laminate for manufacturing a wavelength conversion member and a method for manufacturing a wavelength conversion member, and more particularly, to a laminate for manufacturing a wavelength conversion member, which can be fired at a temperature of 800 DEG C or less, preferably 700 DEG C or less, and which, after firing, has a high light transmittance, a high refractive index, and a good shape, and can be used for manufacturing a wavelength conversion member. Thus, the laminate for manufacturing a wavelength conversion member can be effectively used in a light-emitting diode or the like, and a method for effectively manufacturing the wavelength conversion member using a confinement layer formed from a specific component.
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Description

[0001] This patent application is a divisional application of the invention patent application with the application date of September 9, 2019, application number 201910847187.1, publication number CN110890454A, and invention name "Laminate for manufacturing wavelength conversion components and method for manufacturing wavelength conversion components". Technical Field

[0002] The present invention relates to a laminate for producing a wavelength conversion component and a method for producing a wavelength conversion component. More specifically, it relates to a laminate for producing a wavelength conversion component having high total light transmittance and excellent optical properties and a method for efficiently producing the above-mentioned wavelength conversion component using a restriction layer formed of a specific component. Background Art

[0003] Generally, a conventional light emitting diode (LED) used as a lighting lamp includes a blue LED and a wavelength converter. The wavelength converter absorbs the blue light emitted from the LED and emits yellow, green, or red light to produce white light.

[0004] Typically, the wavelength converter can be manufactured by fabricating a glass printed circuit board for forming the wavelength converter, laminating a restrictive layer for controlling the printed circuit board's shape on one or both surfaces of the printed circuit board, and then firing the laminated layer. However, if the restrictive layer is laminated only on one surface of the printed circuit board and then fired, the printed circuit board shrinks unevenly during firing, resulting in a poorly shaped wavelength converter.

[0005] As an example of a conventional wavelength conversion component manufacturing method, Korean Patent No. 10-0930165 discloses a method for fabricating a multilayer ceramic substrate by placing a first confinement layer composed of aluminum oxide powder on both surfaces of a printed circuit board containing a glass component, and a second confinement layer composed of a combustion material on the exposed surface of the first confinement layer. However, according to the manufacturing method of the aforementioned patent, during the high-temperature firing after lamination, the viscosity of the printed circuit board melt (i.e., the glass melt), which has a low viscosity, penetrates between the aluminum oxide components used as the first confinement layer, forming a thin layer at the interface between the two layers. After firing, the confinement layer is removed by grinding and / or etching. However, the layer formed between the printed circuit board and the confinement layer is not completely removed, but remains on the surface of the wavelength conversion component, thereby reflecting light emitted from the light source and reducing the amount of light reaching the phosphor. Summary of the Invention

[0006] The object of the present invention is to provide a laminate for making a wavelength conversion component that can be fired at a temperature below 800°C, preferably below 700°C, and has high transmittance, high refractive index and good shape after firing, as well as a method for effectively making the above-mentioned wavelength conversion component.

[0007] To achieve the above-mentioned objectives, the present invention provides a laminate for manufacturing a wavelength conversion component, comprising: a printed circuit board for forming a wavelength conversion component, the printed circuit board for forming a wavelength conversion component comprising a glass matrix and inorganic phosphor powder dispersed in the glass matrix; a printed circuit board for a restriction layer A, the printed circuit board for a restriction layer A being disposed on both side surfaces of the printed circuit board and comprising only silicon dioxide powder as inorganic oxide powder; and a printed circuit board for a restriction layer B, the printed circuit board for a restriction layer B being disposed on a non-contacting surface between the printed circuit board for forming the wavelength conversion component and the printed circuit board for the restriction layer A. The glass matrix comprises, based on the total molar amount of the glass powder, 0.1 to 15 mol percent of P2O5, 20 to 50 mol percent of ZnO, 8 to 40 mol percent of SiO2, and 10 to 30 mol percent of B2O3.

[0008] Furthermore, the present invention provides a method for manufacturing a wavelength conversion component, which comprises: a first step of preparing a printed circuit substrate for forming a wavelength conversion component comprising glass powder and inorganic phosphor powder; a second step of arranging a printed circuit substrate for a restriction layer A containing only silica powder as an inorganic oxide powder on both side surfaces of the printed circuit substrate for forming the wavelength conversion component; a third step of arranging and stacking a printed circuit substrate for a restriction layer B on a non-contact surface between the printed circuit substrate for forming the wavelength conversion component and the printed circuit substrate for the restriction layer A to obtain a laminate; a fourth step of firing the laminate; and a fifth step of removing the fired restriction layer A and restriction layer B from the fired laminate.

[0009] Furthermore, the present invention provides a wavelength conversion component produced by the above-mentioned production method.

[0010] The wavelength conversion component of the present invention can be fired at a temperature below 800°C, preferably below 700°C. After firing, it has high transmittance, high refractive index and good shape, and can be effectively used in light-emitting diodes, etc. DETAILED DESCRIPTION

[0011] The present invention provides a laminate for fabricating a wavelength conversion component, comprising: a printed circuit board for forming a wavelength conversion component, the printed circuit board for forming a wavelength conversion component comprising a glass matrix and inorganic phosphor powder dispersed in the glass matrix; a printed circuit board for a restriction layer A, the printed circuit board for the restriction layer A being disposed on both side surfaces of the printed circuit board and comprising only silicon dioxide powder as inorganic oxide powder; and a printed circuit board for a restriction layer B being disposed on a non-contacting surface between the printed circuit board for forming the wavelength conversion component and the printed circuit board for the restriction layer A. The glass matrix comprises, based on the total molar number of the glass powder, 0.1 to 15 mol percent of P2O5, 20 to 50 mol percent of ZnO, 8 to 40 mol percent of SiO2, and 10 to 30 mol percent of B2O3.

[0012] Glass matrix

[0013] Based on the total moles of the glass powder, the glass matrix comprises 0.1 to 15 mol% of P2O5, 20 to 50 mol% of ZnO, 8 to 40 mol% of SiO2, and 10 to 30 mol% of B2O3. Specifically, based on the total moles of the glass powder, the glass matrix may comprise 0.1 to 13 mol%, 0.1 to 10 mol%, or 0.2 to 10 mol% of P2O5; 25 to 50 mol%, 25 to 48 mol%, or 28 to 48 mol% of ZnO; 8 to 38 mol%, 8 to 36 mol%, or 8 to 35 mol% of SiO2; and 11 to 30 mol%, 11 to 28 mol%, or 11 to 27 mol% of B2O3.

[0014] Based on the total moles of the glass powder, the glass matrix may further include 0.1 to 20 mol% of SnO2 and 0.1 to 20 mol% of Al2O3. Specifically, based on the total moles of the glass powder, the glass matrix may further include 0.1 to 15 mol%, 0.1 to 10 mol%, 0.1 to 8 mol%, or 0.1 to 6 mol% of SnO2; and 0.1 to 15 mol%, 0.5 to 15 mol%, 1 to 13 mol%, or 1 to 11 mol% of Al2O3.

[0015] The glass matrix may further include 1 to 30 mol % of one or more alkaline earth metal oxides selected from the group consisting of BaO, SrO, and CaO, based on the total moles of the glass powder. Specifically, the glass matrix may further include 1 to 20 mol %, 1 to 10 mol %, or 1 to 8 mol % of one or more alkaline earth metal oxides selected from the group consisting of BaO, SrO, and CaO, based on the total moles of the glass powder.

[0016] The glass matrix may further include 1 to 30 mol % of one or more alkali metal oxides selected from the group consisting of Na2O, KO, and Li2O, based on the total moles of the glass powder. Specifically, the glass matrix may further include 1 to 20 mol %, 1 to 18 mol %, or 2 to 17 mol %, based on the total moles of the glass powder, of one or more alkali metal oxides selected from the group consisting of Na2O, KO, and Li2O. More specifically, the glass matrix may include 1 to 10 mol % or 1.5 to 8 mol % of Na2O; 0 to 10 mol %, 0 to 8 mol %, or 0 to 7 mol % of KO; and 0 to 10 mol %, 0 to 8 mol %, or 0 to 7 mol % of Li2O, based on the total moles of the glass powder.

[0017] Specifically, the alkali metal oxide may include Na2O and K2O; Na2O and Li2O; or Na2O, K2O, and Li2O.

[0018] The glass matrix may be selected from a glass having a refractive index of 1.4 to 1.7, a softening point (Ts) of 400°C to 700°C and an average particle size (D 50 ) is 0.1 μm to 20 μm. Specifically, the glass matrix can be derived from a glass powder having a refractive index of 1.45 to 1.7, 1.5 to 1.66, 1.55 to 1.65 or 1.58 to 1.66, a softening point (Ts) of 400°C to 700°C, 500°C to 700°C, 550°C to 700°C or 550°C to 650°C, and an average particle size (D 50 ) is derived from glass powder with a diameter of 0.1 μm to 20 μm, 1 μm to 20 μm or 1 μm to 10 μm.

[0019] Inorganic phosphor powder

[0020] The inorganic phosphor powder may include one or more phosphor powders selected from the group consisting of yttrium-aluminum-garnet (YAG), ruthenium-aluminum-garnet (LuAG), nitride, sulfide, and silicate materials.

[0021] The average particle size of the inorganic phosphor powder (D 50 ) can be 1 μm to 50 μm. Specifically, the average particle size (D 50 ) may be 1 μm to 50 μm, 5 μm to 40 μm, or 10 μm to 30 μm.

[0022] Printed circuit board for forming wavelength conversion component

[0023] The wavelength conversion member forming green sheet includes a glass matrix and inorganic phosphor powder, and the inorganic phosphor powder is dispersed in the glass matrix.

[0024] The wavelength conversion component-forming printed circuit board can be produced from a glass composition comprising glass powder, inorganic phosphor powder, a binder resin, and a solvent. Specifically, the glass composition can contain 3 to 160 parts by weight of inorganic phosphor powder and 120 to 280 parts by weight of glass powder, based on 100 parts by weight of the binder resin.

[0025] The solvent may contain an amount suitable for the properties of the composition and the drying conditions. Specifically, based on the total weight of the glass composition, the solvent may contain 30 weight percent to 50 weight percent.

[0026] The solvent has a low boiling point in order to rapidly produce the printed circuit board. Specifically, the boiling point of the solvent may be 30°C to 150°C. More specifically, the boiling point of the solvent may be 60°C to 130°C.

[0027] Furthermore, the solvent may include one or more selected from the group consisting of toluene, ethanol, butanol, acetone, and methanol. Specifically, the solvent may include one or more selected from the group consisting of toluene, ethanol, and butanol. More specifically, the solvent may include toluene, ethanol, and butanol.

[0028] The binder resin may include at least one selected from the group consisting of polyvinyl butyral (PVB), polyvinyl alcohol (PVA), and polyvinyl acetate (PVAc). Specifically, the binder resin may include polyvinyl butyral or polyvinyl alcohol.

[0029] The weight average molecular weight of the binder resin may be 1000 g / mol to 70000 g / mol, specifically, the weight average molecular weight of the binder resin may be 20000 g / mol to 60000 g / mol.

[0030] The glass composition may further include a plasticizer. The plasticizer may include one or more selected from the group consisting of dioctyl phthalate (DOP), dioctyl adipate (DOA), and tricresyl phosphate (TCP). Specifically, the plasticizer may include dioctyl phthalate or dioctyl adipate.

[0031] Furthermore, the plasticizer may be included in an amount of 10 to 200 parts by weight based on 100 parts by weight of the binder resin, and more specifically, may be included in an amount of 30 to 90 parts by weight based on 100 parts by weight of the binder resin.

[0032] The glass composition can be prepared by mixing a solvent and a binder resin, removing air bubbles, and then adding glass powder, inorganic phosphor powder, and a plasticizer. The present invention uses a solvent with a low boiling point, so that the binder resin and the solvent can be mixed at room temperature when preparing the glass composition.

[0033] The wavelength conversion component-forming printed circuit board may include 30 to 100 weight percent of the glass matrix and 5 to 50 weight percent of the inorganic phosphor powder, based on the total weight of the printed circuit board. Specifically, the wavelength conversion component-forming printed circuit board may include 40 to 90 weight percent of the glass matrix and 8 to 30 weight percent of the inorganic phosphor powder, based on the total weight of the printed circuit board.

[0034] The thickness of the wavelength conversion member-forming printed circuit board may be 10 μm to 2000 μm. Specifically, the thickness of the wavelength conversion member-forming printed circuit board may be 20 μm to 1200 μm.

[0035] The inorganic phosphor powder described above does not melt or react at firing temperatures and can therefore be used as a material for the restricting layer. However, to function as a restricting layer component, the inorganic phosphor powder must be densely packed. As mentioned above, this densely packed inorganic phosphor powder reduces the refractive index and light transmittance by preventing light from entering the interior of the wavelength conversion component. Therefore, the printed circuit board for restricting layer A and the printed circuit board for restricting layer B preferably do not contain inorganic phosphor powder.

[0036] Printed circuit board for restriction layer A

[0037] The green sheet for the restriction layer A comprises only silica powder as an inorganic oxide powder. Furthermore, when fired, the green sheet for the restriction layer A controls the shape of the green sheet for forming the wavelength conversion component and assists in the function of the wavelength conversion component.

[0038] Unlike alumina used for chemical layer formation, which reacts with the printed circuit board melt to reflect light and reduce the amount of light reaching the phosphor, silica powder has excellent light transmission properties and does not cause a reduction in light. After firing and polishing, it remains on the surface of the wavelength conversion component and acts as a light diffuser, thereby improving the optical properties of the wavelength conversion component.

[0039] The average particle size of the silicon dioxide powder (D 50 ) can be 0.1 μm to 30 μm. Specifically, the average particle size (D 50 ) may be 0.2 μm to 20 μm or 0.5 μm to 10 μm.

[0040] The green sheet for restricting layer A can be prepared from a composition for restricting layer A comprising silica powder, a binder resin, and a solvent. Specifically, the composition for restricting layer A can contain 500 to 1500 parts by weight of silica powder per 100 parts by weight of the binder resin.

[0041] The solvent may comprise 30 weight percent to 50 weight percent based on the total weight of the composition for the restricting layer A.

[0042] The binder resin and solvent are as described above in connection with the wavelength conversion member-forming printed circuit board.

[0043] The composition for the restricting layer A may further contain a plasticizer. The type and content of the plasticizer are as described above in the printed circuit board for forming a wavelength conversion member.

[0044] The composition for the restricting layer A can be prepared by mixing a solvent and a binder resin, removing air bubbles, and then adding silica powder and a plasticizer. The present invention uses a solvent with a low boiling point, so that the binder resin and the solvent can be mixed at room temperature when preparing the composition for the restricting layer A.

[0045] The printed circuit substrate for the restriction layer A may have a thickness of 5 to 200 μm. Specifically, the printed circuit substrate for the restriction layer A may have a thickness of 10 to 200 μm, 10 to 100 μm, 10 to 50 μm, 20 to 100 μm, 20 to 80 μm, or 20 to 50 μm.

[0046] The printed circuit board for the restriction layer A needs to be placed on both sides of the printed circuit board for forming the wavelength conversion component. If the printed circuit board for the restriction layer A is placed on one side of the printed circuit board for forming the wavelength conversion component and fired, the printed circuit board shrinks unevenly, resulting in warping or cracking of the resulting wavelength conversion component.

[0047] Printed circuit board for restriction layer B

[0048] During firing, the green sheet for the restriction layer B is used to control the shape of the green sheet for forming the wavelength conversion member.

[0049] The printed circuit board for restriction layer B needs to be placed on a non-contacting surface of the printed circuit board for restriction layer A, or on a non-contacting surface of the printed circuit board for forming the wavelength conversion member. If the printed circuit board for restriction layer B is placed on one surface of a single printed circuit board for restriction layer A, the printed circuit board shrinks unevenly, resulting in warping or cracking of the resulting wavelength conversion member.

[0050] The green sheet for the restriction layer B may include one or more inorganic oxide powders selected from the group consisting of alumina, silica, magnesia, and zirconia. Specifically, the green sheet for the restriction layer B may include alumina or magnesia.

[0051] The average particle size of the inorganic oxide powder (D 50 ) can be 0.1 μm to 30 μm. Specifically, the average particle size (D 50 ) may be 0.5 μm to 25 μm, 0.5 μm to 20 μm, or 1 μm to 15 μm.

[0052] The printed circuit board for restriction layer B can be prepared from a composition for restriction layer B comprising the inorganic oxide powder, a binder resin, and a solvent. Specifically, the composition for restriction layer B can contain 500 to 1500 parts by weight of the inorganic oxide powder based on 100 parts by weight of the binder resin.

[0053] Based on the total weight of the composition for the restricting layer B, the solvent may comprise 30 weight percent to 50 weight percent.

[0054] The binder resin and solvent are as described above in connection with the wavelength conversion member-forming printed circuit board.

[0055] The composition for the restricting layer B may further contain a plasticizer. The type and content of the plasticizer are as described above in the printed circuit board for forming a wavelength conversion member.

[0056] The composition for the restricting layer B can be prepared by mixing a solvent and a binder resin, removing air bubbles, and then adding an inorganic oxide powder and a plasticizer. The present invention uses a solvent with a low boiling point, so that the binder resin and solvent can be mixed at room temperature when preparing the composition for the restricting layer B.

[0057] The printed circuit substrate for the restriction layer B may have a thickness of 5 to 200 μm. Specifically, the printed circuit substrate for the restriction layer B may have a thickness of 10 to 200 μm, 10 to 100 μm, 10 to 50 μm, 20 to 100 μm, 20 to 80 μm, 20 to 50 μm, or 30 to 50 μm.

[0058] The total number of layers of the printed circuit substrate for restriction layer A and the printed circuit substrate for restriction layer B may be 40 to 50. Specifically, the total number of layers of the printed circuit substrate for restriction layer A and the printed circuit substrate for restriction layer B may be 4 to 40, 8 to 30, or 10 to 30.

[0059] Method for manufacturing wavelength conversion component

[0060] The present invention provides a method for manufacturing a wavelength conversion component, which comprises: a first step of preparing a printed circuit substrate for forming a wavelength conversion component comprising glass powder and inorganic phosphor powder; a second step of arranging printed circuit substrates for a restriction layer A containing only silica powder as inorganic oxide powder on both side surfaces of the printed circuit substrate for forming the wavelength conversion component; a third step of arranging and stacking printed circuit substrates for a restriction layer B on non-contact surfaces between the printed circuit substrate for forming the wavelength conversion component and the printed circuit substrate for the restriction layer A to obtain a laminate; a fourth step of firing the laminate; and a fifth step of removing the fired restriction layer A and restriction layer B from the fired laminate.

[0061] Step 1

[0062] In this step, a green sheet for forming a wavelength conversion member containing glass powder and inorganic phosphor powder is prepared.

[0063] Based on the total molar amount of the glass powder, the glass powder may contain 0.1 to 15 mol% of P2O5, 20 to 50 mol% of ZnO, 8 to 40 mol% of SiO2, 10 to 30 mol% of B2O3, 0.1 to 20 mol% of SnO2, and 0.1 to 20 mol% of Al2O3. Specifically, based on the total molar amount of the glass powder, the glass powder may contain 0.1 to 13 mol%, 0.1 to 10 mol%, or 0.2 to 10 mol% of P2O5; 25 to 50 mol%, 25 to 48 mol%, or 28 to 48 mol% of ZnO; 8 to 38 mol%, 8 to 36 mol%, or 8 to 35 mol% of SiO2; and 11 to 30 mol%, 11 to 30 mol%, or 11 to 30 mol% of SnO2. % to 28 mol percent or 11 mol percent to 27 mol percent of B2O3; 0.1 mol percent to 20 mol percent, 0.1 mol percent to 15 mol percent, 0.1 mol percent to 10 mol percent, 0.1 mol percent to 8 mol percent or 0.1 mol percent to 6 mol percent of SnO2; and 0.1 mol percent to 20 mol percent, 0.1 mol percent to 15 mol percent, 0.5 mol percent to 15 mol percent, 1 mol percent to 13 mol percent or 1 mol percent to 11 mol percent of Al2O3.

[0064] The glass powder further includes one or more oxides selected from the group consisting of BaO, SrO, CaO, Na2O, K2O, and Li2O. Based on the total molar number of the glass powder, the oxide may include 1 mol% to 60 mol%.

[0065] Specifically, the glass powder may further include 1 to 30 mol % of one or more alkaline earth metal oxides selected from the group consisting of BaO, SrO, and CaO, based on the total moles of the glass powder. More specifically, the glass powder may include 1 to 20 mol %, 1 to 10 mol %, or 1 to 8 mol % of one or more alkaline earth metal oxides selected from the group consisting of BaO, SrO, and CaO, based on the total moles of the glass powder.

[0066] Specifically, based on the total moles of the glass powder, the glass powder may further comprise 1 to 30 mol % of one or more alkali metal oxides selected from the group consisting of Na2O, KO, and Li2O. More specifically, based on the total moles of the glass powder, the glass powder may further comprise 1 to 20 mol %, 1 to 18 mol %, or 2 to 17 mol % of one or more alkali metal oxides selected from the group consisting of Na2O, KO, and Li2O. i2 More specifically, based on the total moles of the glass powder, the glass powder may include 1 mol % to 10 mol % or 1.5 mol % to 8 mol % of Na2O; 0 mol % to 10 mol %, 0 mol % to 8 mol %, or 0 mol % to 7 mol % of K2O; and 0 mol % to 10 mol %, 0 mol % to 8 mol %, or 0 mol % to 7 mol % of Li2O.

[0067] The glass powder may have a refractive index of 1.4 to 1.7, a softening point of 400° C. to 700° C., and an average particle size (D 50 Specifically, the glass powder may have a refractive index of 1.45 to 1.7, 1.5 to 1.66, 1.55 to 1.65, or 1.58 to 1.66, a softening point (Ts) of 400°C to 700°C, 500°C to 700°C, 550°C to 700°C, or 550°C to 650°C, and an average particle size (D 50 ).

[0068] The type and average particle size (D 50 ) As already described in the above-mentioned laminate for wavelength conversion components.

[0069] The wavelength conversion member-forming green sheet can be produced from a glass composition comprising glass powder and inorganic phosphor powder. The glass composition is as described above in connection with the wavelength conversion member-forming laminate.

[0070] The wavelength conversion component printed circuit board can be produced by casting the glass composition onto a substrate. Specifically, the wavelength conversion component printed circuit board can be a single sheet, or it can be formed by stacking multiple sheets of a cast printed circuit board and then compressing them. In this case, the number of stacked printed circuit boards is not particularly limited. For example, after compression, the wavelength conversion component printed circuit board can have a thickness of 50 μm to 1500 μm.

[0071] The compression may be performed at a pressure of 1 MPa to 100 MPa. Specifically, the compression may be performed at a pressure of 2 MPa to 50 MPa.

[0072] Step 2

[0073] In this step, green sheets for restriction layer A containing only silica powder as inorganic oxide powder are placed on both sides of the green sheet for wavelength conversion member formation. The green sheets for restriction layer A are formed of silica powder.

[0074] The average particle size of the silicon dioxide powder (D 50 ) can be 0.1 μm to 30 μm. Specifically, the average particle size (D 50 ) may be 0.2 μm to 20 μm or 0.5 μm to 10 μm.

[0075] The green sheet for the restricting layer A can be prepared from a composition for the restricting layer A containing silica powder, a binder resin, and a solvent.

[0076] The composition for the restricting layer A, the binder resin, and the solvent are as described above in the laminate for the wavelength conversion member.

[0077] The printed circuit substrate for the restriction layer A may have a thickness of 5 to 200 μm. Specifically, the printed circuit substrate for the restriction layer A may have a thickness of 10 to 200 μm, 10 to 100 μm, 10 to 50 μm, 20 to 100 μm, 20 to 80 μm, or 20 to 50 μm.

[0078] Step 3

[0079] In this step, the green sheets for the restricting layer B are arranged and stacked on the non-contact surfaces of the green sheets for the restricting layer A and the wavelength conversion member forming green sheets, thereby obtaining a stacked body.

[0080] The green sheet for the restriction layer B may include one or more inorganic oxide powders selected from the group consisting of aluminum oxide, silicon dioxide, magnesium oxide, and zirconium oxide. Specifically, the green sheet for the restriction layer B may include aluminum oxide or magnesium oxide.

[0081] The average particle size of the inorganic oxide powder (D 50 ) can be 0.1 μm to 30 μm. Specifically, the average particle size (D 50 ) may be 0.5 μm to 25 μm, 0.5 μm to 20 μm, or 1 μm to 15 μm.

[0082] The green sheet for the restriction layer B can be produced from a composition for the restriction layer B containing the inorganic oxide powder, a binder resin, and a solvent.

[0083] The composition for the restricting layer B, the binder resin, and the solvent are as described above in connection with the laminate for producing the wavelength conversion member.

[0084] The printed circuit substrate for the restriction layer B may have a thickness of 5 to 200 μm. Specifically, the printed circuit substrate for the restriction layer B may have a thickness of 10 to 200 μm, 10 to 100 μm, 10 to 50 μm, 20 to 100 μm, 20 to 80 μm, 20 to 50 μm, or 30 to 50 μm.

[0085] The total number of printed circuit substrates for restriction layer A and restriction layer B stacked together may be 4 to 50. Specifically, the total number of printed circuit substrates for restriction layer A and restriction layer B stacked together may be 4 to 30, 8 to 30, or 10 to 30.

[0086] The lamination can be performed for 5 to 90 seconds under conditions of a pressure of 12 MPa to 200 MPa and a temperature of 40° C. to 80° C. Specifically, the lamination can be performed for 5 to 60 seconds under conditions of a pressure of 12 MPa to 180 MPa, 12 MPa to 160 MPa, or 13 MPa to 150 MPa and a temperature of 40° C. to 70° C. More specifically, the lamination can be performed using a lamination apparatus having an upper temperature of 60° C. to 70° C. and a lower temperature of 40° C. to 60° C.

[0087] Step 4

[0088] In this step, the above-mentioned laminated body is fired.

[0089] The sintering may be performed at a temperature of 500° C. to 800° C. for 10 minutes to 72 hours. Specifically, the sintering may be performed at a temperature of 500° C. to 700° C. for 10 minutes to 52 hours.

[0090] Step 5

[0091] In this step, the fired restricting layers A and B are removed from the fired laminate. Specifically, ultrasonic cleaning can be used to remove the fired restricting layers A and B from the fired laminate. In this case, the ultrasonic cleaning can be performed using ultrasonic waves at 10,000 to 100,000 Hz for 5 seconds to 2 hours. Specifically, the ultrasonic cleaning can be performed using ultrasonic waves at 30,000 to 50,000 Hz for 30 seconds to 1 hour.

[0092] The thickness of the wavelength conversion member may be 100 μm to 1000 μm. Specifically, the thickness of the wavelength conversion member may be 100 μm to 800 μm, 100 μm to 500 μm, or 100 μm to 300 μm.

[0093] The wavelength conversion component may have a light transmission rate of 70% to 80%, specifically, 72% to 80%, 74% to 78%, or 76% to 78%.

[0094] The method for manufacturing the wavelength conversion component as described above uses a limiting layer formed by a specific component, which can be fired at a temperature below 800°C, preferably below 700°C. After firing, it has high light transmittance, high refractive index and good shape, so that it can be effectively used in organic light-emitting diodes, etc.

[0095] Hereinafter, the present invention will be described in more detail by way of the following examples. However, the following examples are merely illustrative of the present invention, and the scope of the present invention is not limited to these examples.

[0096] Example

[0097] Preparation Example 1. Making a glass plate

[0098] The components were mixed to form the composition shown in Table 1 below and melted at 1200°C to 1400°C to produce a glass material. The resulting glass material was pulverized to produce a glass powder with an average particle size of 5.9 μm. The glass powder was placed in a mold and compression-molded for 5 minutes at a pressure of 5 tons. It was then placed in a firing furnace and fired at 620°C for 30 minutes. The glass surface was then abraded to a surface roughness of 0.2 μm to produce a 200 μm thick glass plate.

[0099] Preparation Example 2 to Preparation Example 12

[0100] A glass plate was prepared by the same method as in Preparation Example 1, except that the content of each component was adjusted to have the composition shown in Table 1 below.

[0101] Experimental Example 1

[0102] The physical properties of the glass plates of Preparation Examples 1 to 12 were evaluated by the following methods. The results are shown in Table 1.

[0103] (1) Glass transition temperature (Tg) and softening temperature (Ts)

[0104] The glass transition temperature and softening temperature were measured using a thermal analyzer (SDT: Q600, TA Instruments, USA) at a heating rate of 10°C / min from room temperature to 1000°C.

[0105] In this case, the temperature dilatometer softening point (Tdsp) refers to the dilatometer softening point temperature.

[0106] (2) Light projection rate (%)

[0107] The light transmittance of light at a reference wavelength of 550 nm was measured using a recording spectrophotometer (U-350, manufactured by Hitachi, Japan), with the state without a sample being defined as 100%.

[0108] (3) Refractive index

[0109] Measurements were performed using a professional gemstone refractometer (Kruess model ER601 LED, Germany). After the test piece was machined to a thickness of 1 mm (1 T), a prescribed amount of refractive fluid was applied to the test piece until it adhered perfectly to the measurement area, and the refractive index value was confirmed visually.

[0110] Table 1

[0111]

[0112] As shown in Table 1, the glass plates of Examples 1 to 10 exhibit high transmittance and excellent refractive index properties, with glass transition temperatures below 650°C and suitable softening characteristics. Furthermore, the wavelength conversion component's optical properties were subsequently verified based on the results of the study, which show that the light transmittance and refractive index of the glass matrix affect its optical properties.

[0113] Example 1. Fabrication of wavelength conversion components

[0114] 1-1: Fabrication of a printed circuit board for wavelength conversion components

[0115] 27 g of polyvinyl butyral (PVB, weight average molecular weight: 50,000 g / mol) was added to 81 g of a solvent (containing toluene, ethanol, and butanol in a volume ratio of 3:1:1) and dissolved at room temperature for 1 hour to prepare a binder solution.

[0116] Mix 11 parts by weight of yttrium aluminum garnet phosphor powder (average particle size (D 50A glass composition was prepared by adding 89 parts by weight of the glass powder from Preparation Example 5, 89 parts by weight of a binder solution, and 11 parts by weight of a plasticizer. This glass composition was applied to a PET film using a tape casting method to form a sheet, yielding a 50 μm thick printed circuit board. Twenty-one of these printed circuit boards were stacked and pressed at 14 MPa to produce a printed circuit board for forming a wavelength conversion component.

[0117] 1-2: Fabrication of a printed circuit board for the restriction layer A

[0118] Mix 160g of the binder solution of Example 1-1, silica powder (average particle size (D 50 ): 4.9 μm) 500 g and 20 g of plasticizer were added to prepare a composition for the restricting layer A. Then, a restricting layer A plate having a thickness of 30 μm was prepared from the restricting layer A composition by the same tape casting method as in Example 1-1.

[0119] 1-3: Fabrication of printed circuit board for restriction layer B

[0120] Mix 160g of the binder solution of Example 1-1, aluminum oxide powder (average particle size (D 50 ): 2.2 μm) 500 g and 20 g of plasticizer were added to prepare a composition for a restricting layer B. Then, a restricting layer B plate having a thickness of 30 μm was prepared from the restricting layer B composition in the same manner as in Example 1-1.

[0121] 1-4: Making wavelength conversion components

[0122] A laminate was prepared by placing printed circuit boards for restriction layer A of Example 1-2 on both sides of the printed circuit board for forming a wavelength conversion component of Example 1-1. Printed circuit boards for restriction layer B of Example 1-3 were placed on the non-contacting surfaces of the printed circuit boards for forming a wavelength conversion component. The laminate was then placed in a laminator at an upper temperature of 65°C and a lower temperature of 50°C, and a pressure of 14 MPa was applied for 30 seconds. The laminate was then placed in a sintering chamber at 600°C and sintered for 0.5 hours. The laminate was then ultrasonically cleaned for 10 minutes using 45,000 Hz ultrasonic waves to remove the sintered restriction layers A and B, producing a wavelength conversion component with an average thickness of 100 μm.

[0123] Examples 2 to 6 and Comparative Examples 1 to 4.

[0124] A wavelength conversion member was produced by the same method as in Example 1 except that the types of glass powder used and the types of inorganic oxides contained in the green sheets for restriction layer A and restriction layer B were adjusted as shown in Table 2 below.

[0125] Experimental Example 2

[0126] The wavelength conversion members of Examples 1 to 6 and Comparative Examples 1 to 4 were used as subjects, and their characteristics were measured by the following methods. The results are shown in Table 2 below.

[0127] (1) State of the fired body

[0128] The fired state of the wavelength conversion member was evaluated by visual inspection.

[0129] (2) Light projection rate (%)

[0130] The light transmittance of light at a reference wavelength of 550 nm was measured using a recording spectrophotometer (U-350, manufactured by Hitachi, Japan), with the state without a sample being defined as 100%.

[0131] (3) Chromaticity distribution diagram (Cx, Cy, light beam (Φv, lumen (lm)) and converted light beam (%))

[0132] The chromaticity distribution diagram was measured using an integrating sphere measurement device (LMS-200, J&C Tech.) with a wavelength conversion member placed under an excitation light source of 445 nm.

[0133] Table 2

[0134]

[0135] As shown in Table 2, the optical properties of the produced wavelength conversion members differed due to differences in transmittance depending on the glass composition. In particular, the wavelength conversion members of Examples 4 to 6 exhibited significantly superior optical properties.

[0136] In contrast, the wavelength conversion members of Comparative Examples 1 to 4 have remarkably low transmittances and remarkably low optical characteristics.

Claims

1. A laminate for producing a wavelength conversion component, characterized in that: include: A printed circuit board for forming a wavelength conversion component, comprising a glass matrix and inorganic phosphor powder dispersed in the glass matrix; A printed circuit board for the restriction layer A is disposed on both sides of the printed circuit board, and the inorganic oxide powder only comprises silicon dioxide powder; and The printed circuit board for the restriction layer B is disposed on a non-contact surface between the printed circuit board for forming the wavelength conversion member and the printed circuit board for the restriction layer A. Based on the total molar amount of the glass powder, the glass matrix comprises 0.1 mol % to 15 mol % of P2O5, 20 mol % to 50 mol % of ZnO, 8 mol % to 40 mol % of SiO2, and 10 mol % to 30 mol % of B2O3.

2. The laminate for producing a wavelength conversion member according to claim 1, wherein: Based on the total molar amount of the glass powder, the glass matrix further comprises 0.1 mol % to 20 mol % of SnO 2 and 0.1 mol % to 20 mol % of Al 2 O 3 .

3. The laminate for producing a wavelength conversion member according to claim 2, wherein: The glass matrix includes 1 mol % to 30 mol % of one or more alkaline earth metal oxides selected from the group consisting of BaO, SrO, and CaO, based on the total molar amount of the glass powder.

4. The laminate for producing a wavelength conversion member according to claim 2 or 3, wherein: The glass matrix includes 1 mol % to 30 mol % of one or more alkali metal oxides selected from the group consisting of Na 2 O, K 2 O, and Li 2 O, based on the total molar number of the glass powder.

5. The laminate for producing a wavelength conversion member according to claim 1, wherein The glass matrix is ​​derived from glass powder having a refractive index of 1.4 to 1.7, a softening point of 400° C. to 700° C., and an average particle size of 0.1 μm to 20 μm.

6. The laminate for producing a wavelength conversion member according to claim 1, wherein: The inorganic phosphor powder includes one or more phosphor powders selected from the group consisting of yttrium aluminum garnet, ruthenium aluminum garnet, nitride, sulfide, and silicate substances.

7. The laminate for producing a wavelength conversion member according to claim 1, wherein: The average particle size of the inorganic phosphor powder is 1 μm to 50 μm.

8. The laminate for producing a wavelength conversion member according to claim 1, wherein The average particle size of the silicon dioxide powder of the above-mentioned restriction layer A printed circuit board is 0.1 μm to 30 μm. The thickness of the green sheet for the restriction layer A is 5 μm to 200 μm.

9. The laminate for producing a wavelength conversion member according to claim 1, wherein The green sheet for the restriction layer B comprises one or more inorganic oxide powders selected from the group consisting of alumina, silica, magnesia, and zirconia. The average particle size of the inorganic oxide powder is 0.1 μm to 30 μm. The thickness of the green sheet for the restriction layer B is 5 μm to 200 μm.

10. A method for manufacturing a wavelength conversion component, characterized in that: include: The first step is to prepare a printed circuit board for forming a wavelength conversion component containing glass powder and inorganic phosphor powder; In a second step, a green sheet for a restriction layer A containing only silicon dioxide powder as the inorganic oxide powder is disposed on both sides of the green sheet for forming the wavelength conversion member; The third step is to arrange and stack the restriction layer B printed circuit board on the non-contact surface between the restriction layer A printed circuit board and the wavelength conversion member forming printed circuit board to form a laminated body; The fourth step is to sinter the laminated body; and In the fifth step, the fired restriction layer A and the restriction layer B are removed from the fired laminate.

11. The method for manufacturing a wavelength conversion component according to claim 10, wherein: Based on the total molar number of the glass powder, the above-mentioned glass powder contains 0.1 mol% to 15 mol% of P2O5, 20 mol% to 50 mol% of ZnO, 8 mol% to 40 mol% of SiO2, 10 mol% to 30 mol% of B2O3, 0.1 mol% to 20 mol% of SnO2 and 0.1 mol% to 20 mol% of Al2O3.

12. The method for manufacturing a wavelength conversion component according to claim 11, wherein: The glass powder further comprises 1 mol % to 60 mol % of one or more oxides selected from the group consisting of BaO, SrO, CaO, Na2O, K2O, and Li2O, based on the total molar number of the glass powder.

13. The method for manufacturing a wavelength conversion component according to claim 10, wherein: The glass powder has a refractive index of 1.4 to 1.7, a softening point of 400° C. to 700° C., and an average particle size of 0.1 μm to 20 μm.

14. The method for manufacturing a wavelength conversion component according to claim 10, wherein: The inorganic phosphor powder includes one or more phosphor powders selected from the group consisting of yttrium aluminum garnet, ruthenium aluminum garnet, nitride, sulfide, and silicate substances.

15. The method for manufacturing a wavelength conversion component according to claim 10, wherein: The average particle size of the inorganic phosphor powder is 1 μm to 50 μm.

16. The method for manufacturing a wavelength conversion component according to claim 10, wherein: The average particle size of the silicon dioxide powder of the above-mentioned restriction layer A printed circuit board is 0.1 μm to 30 μm. The thickness of the green sheet for the restriction layer A is 5 μm to 200 μm.

17. The method for manufacturing a wavelength conversion component according to claim 10, wherein: The green sheet for the restriction layer B comprises one or more inorganic oxide powders selected from the group consisting of alumina, silica, magnesia, and zirconia. The average particle size of the inorganic oxide powder is 0.1 μm to 30 μm. The thickness of the green sheet for the restriction layer B is 5 μm to 200 μm.

18. The method for manufacturing a wavelength conversion component according to claim 10, wherein: The lamination in the third step is performed under the conditions of a pressure of 12 MPa to 200 MPa and a temperature of 40° C. to 80° C. for 5 seconds to 90 seconds.

19. The method for manufacturing a wavelength conversion component according to claim 10, wherein: The firing in the fourth step is performed at a temperature of 500° C. to 800° C. for 10 minutes to 72 hours.

20. The method for manufacturing a wavelength conversion component according to claim 10, wherein: The fifth step is performed by ultrasonic cleaning.

21. A wavelength conversion component, characterized in that: It is produced by the production method according to any one of claims 10 to 20.

22. The wavelength conversion component according to claim 21, wherein The wavelength conversion member has a thickness of 100 μm to 1000 μm.

23. The wavelength conversion component according to claim 21, wherein The wavelength conversion member has a light transmittance of 70% to 80%.

Citation Information

Patent Citations

  • Constraining green sheet and manufacturing method of multi-layer ceramic substrate using the same

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