CN103395990B - A kind of preparation method of glass fiber reinforcement fluorescent glass compound foil - Google Patents
A kind of preparation method of glass fiber reinforcement fluorescent glass compound foil Download PDFInfo
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- CN103395990B CN103395990B CN201310291551.3A CN201310291551A CN103395990B CN 103395990 B CN103395990 B CN 103395990B CN 201310291551 A CN201310291551 A CN 201310291551A CN 103395990 B CN103395990 B CN 103395990B
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Abstract
The present invention relates to the preparation method of a kind of glass fiber reinforcement fluorescent glass compound foil, including: (1) weighs fluorescent material and the glass dust of mass ratio 1:4～4:1, adds binding agent, is mixed to form fluorescent glass slurry；(2) by fiberglass braided one-tenth skeleton or network, it is combined with above-mentioned fluorescent glass slurry, forms compound foil by knife coating；(3) by above-mentioned compound foil baking sintering, last ground polishing, cutting, glass fiber reinforcement fluorescent glass compound foil is obtained.The present invention utilizes knife coating to prepare fluorescent glass thin slice, utilizes glass fibre that thin slice is carried out the enhancing of mechanical property simultaneously.Operation is simple, and raw material range is extensive, it is possible to use the fluorescent material of overwhelming majority system is combined with glass dust；The fluorescence thin section of preparation has preferable luminescent properties and mechanical property, may apply to high-power illumination or display field.
Description
Technical field
The invention belongs to field of light emitting materials, particularly to the preparation method of a kind of glass fiber reinforcement fluorescent glass compound foil.
Background technology
Fluorescent material, as typical solid embedded photoluminescent material, suffers from being widely applied at numerous areas such as illumination, displays, has become as one of Material Field direction the most popular.
Fixing and the protection on physical chemistry to fluorescent material be carried out certain position, needing fluorescent material is carried out certain encapsulation.Such as in early days LED production process utilize the high-molecular organic materials such as epoxy resin to be packaged fluorescent material as encapsulating material always.But because the physical and chemical stability of resin is poor, aged deterioration phenomenon easily occurs during working long hours.Silica gel has more preferable transmitance, thermal conductivity, physical and chemical stability and fluorescent material dispersibility relative to resinae encapsulating material, and therefore the great power LED of a new generation uses silica gel to be packaged.But when fluorescent material be applied to high-energy excite environment such as high-power illumination or laser excitation to show time, the encapsulation utilizing silica gel to carry out assembly has been unable to reach application standard.Under long laser irradiates, silica gel occurs in that the phenomenon of degradation and decomposition equally, directly affects the luminescent properties of Internal Fluorescent powder.Improveing encapsulating material and packaging technology and adjusting to meet high-energy-density excites environment to be the difficult problem that association area is faced.
Utilize glass that fluorescent material is packaged the good approach being to solve these problems.Because glass material also has extraordinary physical and chemical stability energy and high thermal stability on the basis of high-permeability, it would be preferable to support fluorescent material luminescent behavior under high-energy-density excites.CN102121591 discloses the preparation method of a kind of white LED light source and fluorophor thereof, it is incorporated into light emitting ionic in glass basis to be excited by blue chip and sends white light, this method successfully solves early stage encapsulation inequality, the problem of encapsulating material degradation and decomposition, but its luminescence system is single and luminous efficiency is relatively low, it is impossible to meet application demand.CN103043908 discloses a kind of novel fluorescence glass and preparation method thereof, through cast molding after fluorescent material and glass dust are calcined, anneal, cut and be prepared as fluorescent glass, application the method can effectively solve the problem that luminescence system is single, but its complex process, more difficult prepare fluorescence thin section, constrain the application of fluorescent glass.CN102723424 discloses the preparation method of a kind of LED fluorescence thin section, fluorescent material and the compressing sintering of particular glass powder is obtained fluorescence thin section, but its product mechanical strength is relatively low, it is impossible to ensure its serviceability.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of glass fiber reinforcement fluorescent glass compound foil, and the method, compared with conventional fluorescent powder packaged type, can be effectively improved the performances such as fluorescent powder packaging stability and dispersing uniformity；Compared with conventional fluorescent glass, the luminescence system that can select is more, and luminous intensity is higher；Compared with conventional fluorescent thin slice, have simpler Preparation equipment and technique, and higher mechanical property.
A kind of preparation method of the glass fiber reinforcement fluorescent glass compound foil of the present invention, including:
(1) weigh fluorescent material and the glass dust of mass ratio 1:4-4:1, add binding agent, be mixed to form fluorescent glass slurry；
(2) by fiberglass braided one-tenth skeleton or network, it is combined with above-mentioned fluorescent glass slurry, is formed the compound foil of required size and thickness by knife coating；
(3) above-mentioned compound foil is toasted 0.5-3h in 100 DEG C-200 DEG C, remove most of volatile binding agent, then under the atmosphere of air or nitrogen, 0.2-2h is sintered in 300 DEG C-900 DEG C, last ground polishing (improving its surface smoothness), cut into the product of required form size, obtain glass fiber reinforcement fluorescent glass compound foil.
Fluorescent material in described step (1) is one or several in the many body system fluorescent material such as rear-earth-doped oxide, nitride and oxynitride, and the granular size of fluorescent material is 1-20 μm.
The softening point of the glass dust in described step (1) is 300 DEG C-700 DEG C.
Binding agent in described step (1) is the volatile viscous liquids such as terpineol.
A diameter of 10-50 μm of the glass fibre in described step (2), the softening point of glass fibre higher than glass dust softening point 50 DEG C or more than.
Glass fibre in described step (2) and fluorescent glass slurry be complex as that long filament is compound or short silk is combined.
The step that described long filament is combined includes: scratch one layer of slurry, pulp layer is sprawled the glass fibre network that layer of glass long filament is woven into, scratching one layer of slurry on glass fibre network again, be repeated in forming compound foil, the number of plies of glass fibre network is one or more layers.
The step that described short silk is combined includes: mixed homogeneously with glass paste by the glass fibre of a length of 1cm-4cm, forms compound foil by blade coating.
The thickness of described compound foil is 100 μm-3000 μm.
Beneficial effect
(1) present invention utilizes knife coating to prepare fluorescent glass thin slice, utilizes glass fibre that thin slice is carried out the enhancing of mechanical property simultaneously.The method operation is simple, and raw material range is extensive, it is possible to use the fluorescent material of overwhelming majority system is combined with glass dust.The fluorescence thin section of preparation has preferable luminescent properties and mechanical property, may apply to high-power illumination or display field.
(2) compared with conventional fluorescent powder packaged type, the performances such as fluorescent powder packaging stability and dispersing uniformity can be effectively improved；Compared with conventional fluorescent glass, the luminescence system that can select is more, and luminous intensity is higher；Compared with conventional fluorescent thin slice, have simpler Preparation equipment and technique, and higher mechanical property.
Accompanying drawing explanation
Fig. 1 is the technological process that fluorescent glass slurry and filament of glass fiber are combined into glass fiber reinforcement fluorescent glass compound foil.
Fig. 2 is the technological process that fluorescent glass slurry and the short silk of glass fibre are combined into glass fiber reinforcement fluorescent glass compound foil.
Fig. 3 is the excitation-emission spectrum of the fluorescent glass compound foil that Ce doping oxide yellow fluorescent powder is formed with glass powder with low melting point, glass fibre.
Fig. 4 is different-thickness phosphor powder layer and prepared by Different Preparation different fluorescent material ratios, the emission spectrum of the fluorescent glass thin slice of different-thickness, wherein: curve " 400 μm phosphor powder layer " refers to the luminescence spectrum of the Ce doping oxide yellow fluorescence bisque that thickness is 400 μm；Curve " 1000 μm phosphor powder layer " refers to the luminescence spectrum of the Ce doping oxide yellow fluorescence bisque that thickness is 1000 μm；Curve " embodiment 1 " refers to that fluorescent material ratio is 50%, uses long filament to be combined, and thickness is the luminescence spectrum of the fluorescent glass compound foil of 400 μm；Curve " embodiment 2 " refers to that fluorescent material ratio is 75%, uses long filament to be combined, and thickness is the luminescence spectrum of the fluorescent glass compound foil of 400 μm；Curve " embodiment 3 " refers to that fluorescent material ratio is 67%, uses long filament to be combined, and thickness is the luminescence spectrum of the fluorescent glass compound foil of 1000 μm；Curve " embodiment 4 " refers to that fluorescent material ratio is 67%, uses short silk to be combined, and thickness is the luminescence spectrum of the fluorescent glass compound foil of 1000 μm.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention rather than limit the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, the present invention can be made various changes or modifications by those skilled in the art, and these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
1:1 in mass ratio weighs Ce doping oxide yellow fluorescent powder (granular size is 10 μm) and glass dust (softening point is 425 DEG C), adds terpineol and obtains required fluorescent slurry as binding agent by ball milling mixing.Substrate scratches one layer of slurry, pulp layer is sprawled glass fibre network (a diameter of 25 μm of glass that layer of glass long filament is woven into, softening point is 550 DEG C), glass fibre Internet scratches one layer of slurry again, is repeated in twice formation glass fiber reinforcement fluorescent glass compound foil (thickness is 400 μm).Thin slice is toasted in 150 DEG C of baking ovens 2h and removes terpineol.Thin slice heat treatment 1.2h sintering in 440 DEG C of air atmospheres is obtained required glass fiber reinforcement fluorescent glass compound foil.The fluorescent glass thin slice of required flatness and shape size is obtained by sanding and polishing and section.Fig. 3 is the excitation-emission spectrum of this thin slice, shows that this thin slice can excite lower effective transmitting gold-tinted at blue light.In Fig. 4, curve " embodiment 1 " is that it launches optical position and relative luminous intensity, preferably maintains the luminescent properties of fluorescent material compared with the phosphor powder layer that thickness is 400 μm.
Embodiment 2
3:1 in mass ratio weighs Ce doping oxide yellow fluorescent powder (granular size is 15 μm) and glass dust (softening point is 450 DEG C), adds terpineol and obtains required fluorescent slurry as binding agent by ball milling mixing.Substrate scratches one layer of slurry, pulp layer is sprawled glass fibre network (a diameter of 25 μm of glass that layer of glass long filament is woven into, softening point is 600 DEG C), glass fibre Internet scratches one layer of slurry again, is repeated in twice formation glass fiber reinforcement fluorescent glass compound foil (thickness is 400 μm).Thin slice is toasted in 130 DEG C of baking ovens 2.5h and removes volatile terpineol.Thin slice is incubated in 460 DEG C of air atmospheres 1h sintering and obtains required glass fiber reinforcement fluorescent glass compound foil.The fluorescent glass thin slice of required flatness and shape size is obtained by sanding and polishing and section.In Fig. 4, curve " embodiment 2 " is that it launches optical position and relative luminous intensity, preferably maintains the luminescent properties of fluorescent material compared with the phosphor powder layer that thickness is 400 μm；Compare with embodiment 1, although thickness is identical, but owing to the content of fluorescent material is higher, so luminous intensity promotes the most accordingly.
Embodiment 3
2:1 in mass ratio weighs Ce doping oxide yellow fluorescent powder (granular size is 20 μm) and glass dust (softening point is 520 DEG C), adds terpineol and obtains required fluorescent slurry as binding agent by ball milling mixing.Substrate scratches one layer of slurry (thickness is 80 μm), pulp layer is sprawled glass fibre network (a diameter of 25 μm of glass that layer of glass long filament is woven into, softening point is 660 DEG C), glass fibre Internet scratches one layer of slurry again, is repeated in six times and forms glass fiber reinforcement fluorescent glass compound foil (thickness is 1000 μm).Thin slice is toasted in 160 DEG C of baking ovens 1.5h and removes volatile terpineol.Thin slice heat treatment 50min sintering in 530 DEG C of air atmospheres is obtained required glass fiber reinforcement fluorescent glass compound foil.The fluorescent glass thin slice of required flatness and shape size is obtained by sanding and polishing and section.In Fig. 4, curve " embodiment 2 " is that it launches optical position and relative luminous intensity, be 1000 μm left and right phosphor powder layers of the same race with thickness compared with preferably maintain the luminescent properties of fluorescent material；Compare with embodiment 1, although the ratio of fluorescent material declines, but be because thickness and increase, so luminous intensity has promoted.
Embodiment 4
2:1 in mass ratio weighs Ce doping oxide yellow fluorescent powder (granular size is 18 μm) and glass dust (softening point is 450 DEG C), add terpineol and glass fibre (short silk glass, a diameter of 25 μm, a length of 2cm, softening point 550 DEG C) the required fluorescent slurry of hand-ground mixing acquisition.Controlling blade coating benchmark, scratching a layer thickness in substrate is that the pulp layer of 1000 μm is to form glass fiber reinforcement fluorescent glass compound foil.Thin slice is toasted in 120 DEG C of baking ovens 3h and removes most of volatile terpineol.Thin slice heat treatment 1h sintering in 460 DEG C of air atmospheres is obtained required glass fiber reinforcement fluorescent glass compound foil.The fluorescent glass thin slice of required flatness and shape size is obtained by sanding and polishing and section.In Fig. 4, curve " embodiment 4 " is that it launches optical position and relative luminous intensity, compare with embodiment 3, in the case of fluorescent material, glass frit component and sheet thickness are identical, although glass complex method is different, but luminous intensity is basically identical, illustrate that fluorescent glass thin slice luminescent properties can't be caused the biggest impact by different glass complex methods.
Claims (6)
1. a preparation method for glass fiber reinforcement fluorescent glass compound foil, including:
(1) weigh fluorescent material and the glass dust of mass ratio 4:1, add binding agent, be mixed to form fluorescent glass slurry；
(2) by fiberglass braided one-tenth skeleton or network, it is combined with above-mentioned fluorescent glass slurry, forms compound foil by knife coating；
Wherein, a diameter of 10-50 μm of glass fibre, the softening point of glass fibre higher than glass dust softening point 50 DEG C or more than；Glass
The softening point of glass powder is 300 DEG C-700 DEG C；
(3) above-mentioned compound foil is toasted 0.5-3h in 100 DEG C-200 DEG C, then in 300 DEG C-900 DEG C under the atmosphere of air or nitrogen
Sintering 0.2-2h, last ground polishing, cutting, obtain glass fiber reinforcement fluorescent glass compound foil.
The preparation method of a kind of glass fiber reinforcement fluorescent glass compound foil the most according to claim 1, it is characterised in that: institute
Stating the fluorescent material in step (1) is one or several in rear-earth-doped oxide, nitride and oxynitride, fluorescence
The granular size of powder is 1-20 μm.
The preparation method of a kind of glass fiber reinforcement fluorescent glass compound foil the most according to claim 1, it is characterised in that: institute
Stating the binding agent in step (1) is terpineol.
The preparation method of a kind of glass fiber reinforcement fluorescent glass compound foil the most according to claim 1, it is characterised in that: institute
The long filament that is complex as stating the glass fibre in step (2) and fluorescent glass slurry is combined.
The preparation method of a kind of glass fiber reinforcement fluorescent glass compound foil the most according to claim 4, it is characterised in that: institute
The step stating long filament compound includes: scratches one layer of slurry, sprawls the glass that layer of glass long filament is woven on pulp layer
Network of fibers, scratches one layer of slurry on glass fibre network again, is repeated in forming compound foil, the layer of glass fibre network
Number is one or more layers.
The preparation method of a kind of glass fiber reinforcement fluorescent glass compound foil the most according to claim 5, it is characterised in that: institute
The thickness stating compound foil is 100 μm-3000 μm.
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| CN104953014B (en) | 2014-03-28 | 2019-01-29 | 深圳光峰科技股份有限公司 | A kind of multilayered structure glass phosphor sheet and preparation method thereof and light emitting device |
| CN113789008B (en) * | 2021-10-09 | 2022-12-13 | 合肥圆融新材料有限公司 | Superstrong continuous fiber reinforced polyolefin composite material and preparation method thereof |
Citations (4)
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| CN102633440A (en) * | 2012-04-26 | 2012-08-15 | 南通脉锐光电科技有限公司 | Glass coating containing fluorophor and method for producing glass coating, and light-emitting device and method for manufacturing light-emitting device |
| CN102709445A (en) * | 2012-06-02 | 2012-10-03 | 王双喜 | Light-emitting diode (LED) packaging structure with fluorescent glass layer |
| CN102745893A (en) * | 2012-06-20 | 2012-10-24 | 武汉理工大学 | Composite phosphor luminescent glass and preparation method for same |
| CN103011614A (en) * | 2012-11-28 | 2013-04-03 | 武汉利之达科技有限公司 | Fluorescent glass sheet and preparation method thereof |
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| JP5316232B2 (en) * | 2009-06-04 | 2013-10-16 | コニカミノルタ株式会社 | Method for producing phosphor-dispersed glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633440A (en) * | 2012-04-26 | 2012-08-15 | 南通脉锐光电科技有限公司 | Glass coating containing fluorophor and method for producing glass coating, and light-emitting device and method for manufacturing light-emitting device |
| CN102709445A (en) * | 2012-06-02 | 2012-10-03 | 王双喜 | Light-emitting diode (LED) packaging structure with fluorescent glass layer |
| CN102745893A (en) * | 2012-06-20 | 2012-10-24 | 武汉理工大学 | Composite phosphor luminescent glass and preparation method for same |
| CN103011614A (en) * | 2012-11-28 | 2013-04-03 | 武汉利之达科技有限公司 | Fluorescent glass sheet and preparation method thereof |
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