CN101215093A - Method for manufacturing integrated color luminous vycor glass - Google Patents
Method for manufacturing integrated color luminous vycor glass Download PDFInfo
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- CN101215093A CN101215093A CNA2007101730552A CN200710173055A CN101215093A CN 101215093 A CN101215093 A CN 101215093A CN A2007101730552 A CNA2007101730552 A CN A2007101730552A CN 200710173055 A CN200710173055 A CN 200710173055A CN 101215093 A CN101215093 A CN 101215093A
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Abstract
A method for manufacturing integral chromatic luminous vycor glass, which is characterized in that the method comprises: (1) preparing cellular glass, (2) preparing rare earth with certain concentration or transition metal luminous solion, (3) introducing the rare earth or transition metal luminous solion in the cellular glass by employing the segmental doping method, (4) drying the cellular glass doped with the rare earth or transition metal luminous solion in the air at a temperature of 200-800DEG C and (5)placing the dried cellular glass doped with the luminous solion in a high temperature furnace and eliminating micropores to form dense, transparent and integral chromatic luminous vycor glass via solid-phase sintering of air at a temperature of 1100-1250DEG C or reducing atmosphere. The glass of the invention is colorless in appearance, dense and transparent, and can emit light with a plurality of colors when being shined by ultraviolet lamp. The method is simple in manufacturing process, needless in binding agent and low in cost, and has perfect optical property, chemical stability and mechanical strength, which are similar to that of quartz glass.
Description
Technical field
The present invention relates to the manufacture method of colorful light-emitting glass, particularly a kind of integrated color luminous vycor glass.
Background technology
Glass is a kind of outstanding Material Used, has a series of very valuable characteristics: transparent, hard, and good chemical stability and optical property.For crystal and fluorescent material, the easier goods that are processed to all size shape of glass, and also cheap, cost of manufacture is low.Suitable rare earth or the transition metal ion that mix in glass can obtain the as seen luminous of various wavelength, is widely used in multicolor displaying, visible laser, colored lamp, fields such as advertisement lamp decoration.Yet in the classical production process, colorful light-emitting glass is that the combination by the monochromatic fluorescent glass of polylith realizes multiple chromatic mostly.Usually to prepare the monochromatic glass of multiple different colours in the manufacturing processed earlier, with binding agent monochromatic glass block be bondd after the cutting and polishing.This manufacturing approach craft is loaded down with trivial details, and the cycle is long, cost height, and problems such as the refractive index match of inevitable binding agent and glass, organic binder bond illumination ageing.
If can develop a kind of manufacture method, can will simplify manufacture craft greatly so at the same block of light that sends multiple color on glass, reduce manufacturing cost, have extremely important realistic meaning.Want to realize that the integrated color in the glass is luminous, just need segmentation in glass, to mix light emitting ionic.The micropore of sintered glass is evenly distributed, and specific surface area is big, and light emitting ionic is fully disperseed in glass.Because light emitting ionic immerses in the sintered glass by soaking, and prepares the integrated color fluorescent glass so might develop sectional doped method.In addition, the dioxide-containing silica in the vagcor surpasses 96%, and composition approaches pure silica glass, has the optical property similar to silica glass, chemical stability and physical strength.The integrated luminous vagcor that this method obtains is in multicolor displaying, and color bar code is discerned, colored lamp, and fields such as advertisement lamp decoration have a series of potential to use.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art, a kind of manufacture method of integrated color luminous vycor glass is provided, to obtain well behaved integrated color luminous vycor glass.So-called integrated color fluorescent glass, a monolithic glass can send the glass of multiple colorama under illumination exactly.Glass of the present invention, under ultra violet lamp, the monolithic vagcor can send the luminous of multiple color, and this method manufacture craft is simple, need not binding agent, and cost is lower.Glass appearance is colourless, closely knit, transparent, and wherein dioxide-containing silica has the good optical property, chemical stability and the physical strength that are similar to silica glass near 96%.
The concrete technical solution of the present invention is as follows:
A kind of manufacture method of integrated color luminous vycor glass is characterized in that this method comprises the following steps:
1. prepare sintered glass, the composition of this sintered glass is as follows:
Ingredient w t%
Silicon-dioxide (SiO
2) 〉=96.0
Boron oxide (B
2O
3) 1.0～3.0
Aluminum oxide (Al
2O
3) 1.0～3.0
The aperture of this sintered glass is 1.0～10 nanometers, and aperture accounts for 25～40% of glass volume;
2. prepare certain density rare earth or transition metal light emitting ionic solution; By selecting the kind and the concentration of dopant ion, the glow color and the luminous intensity of control colorful light-emitting glass;
3. adopt sectional doped method, rare earth or transition metal light emitting ionic are incorporated in the described sintered glass.
The sintered glass that 4. will be mixed with rare earth or transition metal light emitting ionic carries out drying under in 200～800 ℃ air;
5. dried light emitting ionic doped porous glass is put into High Temperature Furnaces Heating Apparatus, through the solid state sintering of 1100～1250 ℃ of air or reducing atmosphere, eliminating micropore becomes closely knit transparent integrated color luminous vycor glass;
The preparation light emitting ionic solution of above-mentioned steps described in 2. can be the aqueous solution, organic solution or acid solution.
The light emitting ionic kind of above-mentioned steps described in 2. comprises singly mixing of rare earth ion and transition metal ion or mixes altogether, comprise europium (Eu), terbium (Tb), cerium (Ce), samarium (Sm), yttrium (Y), copper (Cu), tin (Sn), vanadium (V), (Ag) is isoionic singly mixes or mix altogether for silver.Realize glass different colours luminous under ultraviolet lamp by changing doping ionic species.
The concentration of the light emitting ionic of above-mentioned steps described in 2. is 0.01-0.2mol/L.
Above-mentioned steps sectional doped described in 3. can be taked two kinds of methods:
A) doping method is soaked in segmentation.Segmentation immersion doping is meant sintered glass is divided into plurality of sections (A, B, C ...), each section is soaked in respectively in the different light emitting ionics.
B) segmentation coats doping method.The segmentation coating-doping is meant paper slip or cloth is dipped in the light emitting ionic solution, will inhale rapidly after the taking-up on each section that paper slip or cloth be coated to sintered glass respectively, and the light emitting ionic on sintered glass absorption paper slip or the cloth is realized mixing.
Technique effect of the present invention is:
The present invention adopts physical method that rare earth or transition metal light emitting ionic are incorporated in the sintered glass.By sectional doped method different light emitting ionics are incorporated in the sintered glass, obtain integrated color luminous vycor glass after the sintering.
The integrated color luminous vycor glass that the present invention obtains is under ultra violet lamp, and same block of glass can send the light of different colours.
The present invention adopts specific surface very big, and the strong sintered glass of surfactivity is as the original principle dopant material, and rare earth or transition metal ion can full and uniform dispersion in glass.And because sintering process need not high-temperature fusion, thereby can suppress the concentration quenching of light emitting ionic effectively, the glass luminous intensity strengthens.
Dioxide-containing silica approaches silica glass in the integrated color luminous vycor glass of manufacturing of the present invention, therefore has to be similar to quartzy optical property, chemical stability and physical strength.In multicolor displaying, color bar code identification, colored lamp, fields such as advertisement lamp decoration have a series of potential to use.
Description of drawings
Fig. 1 soaks the doping method synoptic diagram for segmentation.Among the figure: 1-solution; The 4-sintered glass.
Fig. 2 coats the doping method synoptic diagram for segmentation.Among the figure: 1-solution; 2-inhales paper; 3-is soaked with the suction paper of light emitting ionic; The 4-sintered glass.
Fig. 3 is that europium, copper mix the blue light emitting spectrum of A section in the integrated color vagcor and the green luminescence spectrum of B section respectively.
Embodiment
Table 1 has been listed the glow color under doping ionic species main in the integrated color luminous vycor glass of the present invention, sintering atmosphere, the ultra violet lamp.Combination by light emitting ionic in the his-and-hers watches 1 is mixed (comprising the combination of any two or more different colours light emitting ionics in the table 1), and the present invention is further illustrated to enumerate embodiment, but should not limit protection scope of the present invention with this.
Table 1
| Dopant ion | Sintering atmosphere | Glow color |
| Eu-Y-V Sm Mn Tb Cu V Eu Sn Ag Ce | Air or redox reduction reduction reduction reduction reduction or air reduction process reduction reduction | Red red greenish-yellow blue purple |
With the analytically pure europium nitrate of 0.50g (Eu (NO
3)
39H
2O) be dissolved in the Eu that is mixed with 0.05mol/L in the distilled water of 20ml fully
3+Solution; With the analytically pure cupric chloride (CuCl of 0.135g
2) be dissolved in the Cu that is mixed with 0.05mol/L in the distilled water of 20ml fully
2+Solution.The sintered glass bar of choosing is divided into two sections of A, B, adopts segmentation to soak doping method and in the A section, immerse Eu
3+Solution immerses Cu again in the B section
2+Solution.The sintered glass that is soaked with light emitting ionic is put into corundum crucible with cover after the thorough drying in 200 ℃ of air, and puts 10g graphite or carbon dust around glass, puts into the High Temperature Furnaces Heating Apparatus sintering then.In sintering process, be raised to 900 ℃ with the heat-up rate of 10 ℃/min from room temperature, with from 900 to 1150 ℃ of the heat-up rates of 5 ℃/min, at 1150 ℃ of insulation 30min, glass is with the High Temperature Furnaces Heating Apparatus cool to room temperature afterwards then.Through the following 1150 ℃ solid state sintering of reducing atmosphere, become closely knit transparent integrated color luminous vycor glass.This transparent glass is under the ultra violet lamp of wavelength 254nm, and the A section is sent near the blue light the wavelength 425nm, and the B section is sent near the green glow the wavelength 475nm.Fig. 3 has shown the blue light emitting curve of spectrum of A section and the green luminescence curve of spectrum of B section.
Embodiment 2
With the analytically pure Eu (NO of 0.10g
3)
39H
2O, the analytically pure Yttrium trinitrate of 0.70g (Y (NO
3)
39H
2O) and (vanadylic sulfate) VOSO of 0.27g content 97%
4Be dissolved in fully in the distilled water of 20ml and be mixed with mixing solutions, Eu in the solution
3+Concentration be 0.01mol/L, Y
3+Concentration be 0.08mol/L, V
4+Concentration be 0.08mol/L, this solution note is made solution 1; With the analytically pure cerous nitrate of 0.43g (Ce (NO
3)
36H
2O) be dissolved in fully in the distilled water of 20ml, be mixed with the Ce of 0.05mol/L
3+Solution, note is made solution 2; With the analytically pure Terbium trinitrate of 0.30g (Tb (NO
3)
39H
2O) be dissolved in the Tb that is mixed with 0.30mol/L in the distilled water of 20ml fully
3+Solution, note is made solution 3.The sintered glass bar of choosing is divided into three sections of A, B, C, adopts segmentation to coat doping method and in the A section, immerse solution 1, in the B section, immerse solution 2, in the C section, immerse solution 3.The sintered glass that is soaked with light emitting ionic is put into corundum crucible with cover after the thorough drying in 300 ℃ of air, put into the High Temperature Furnaces Heating Apparatus sintering then.In sintering process, be raised to 900 ℃ with the heat-up rate of 10 ℃/min from room temperature, with from 900 to 1150 ℃ of the heat-up rates of 5 ℃/min, at 1150 ℃ of insulation 30min, glass is with the High Temperature Furnaces Heating Apparatus cool to room temperature afterwards then.Through 1150 ℃ solid state sintering, become closely knit transparent integrated color luminous vycor glass.This transparent glass is under the ultra violet lamp of wavelength 254nm, and the A section is sent near the ruddiness the wavelength 613nm, and the B section is sent near the blue light the wavelength 405nm, and the C section is sent near the green glow the wavelength 542nm.
With 0.17g analytical pure Silver Nitrate (Ag (NO
3)
3) be dissolved in the Ag that is mixed with 0.05mol/L in rare nitric acid of 1mol/L of 20ml fully
+Solution, note is made solution 1; Vanadylic sulfate (VOSO with 0.17g content 97%
4) be dissolved in the V that is mixed with 0.05mol/L in the distilled water of 20ml fully
4+Solution, note is made solution 2; With the analytically pure tin chloride (SnCl of 0.26g
4) be dissolved in the Sn that is mixed with 0.05mol/L in the ethanol of 20ml fully
4+Solution, note is made solution 3.The sintered glass bar of choosing is divided into three sections of A, B, C, adopts segmentation to coat doping method and in the A section, immerse solution 1, in the B section, immerse solution 2, in the C section, immerse solution 3.The sintered glass that is soaked with light emitting ionic is put into corundum crucible with cover after the thorough drying in 400 ℃ of air, and puts 15g graphite or carbon dust around glass, puts into the High Temperature Furnaces Heating Apparatus sintering then.In sintering process, be raised to 900 ℃ with the heat-up rate of 10 ℃/min from room temperature, with from 900 to 1100 ℃ of the heat-up rates of 5 ℃/min, at 1100 ℃ of insulation 30min, glass is with the High Temperature Furnaces Heating Apparatus cool to room temperature afterwards then.Through the following 1100 ℃ solid state sintering of reducing atmosphere, become closely knit transparent integrated color luminous vycor glass.This transparent glass is under the ultra violet lamp of wavelength 254nm, and the A section is sent near the royal purple light the wavelength 372nm, and the B section is sent near the gold-tinted the wavelength 514nm, and the C section is sent near the blue light the wavelength 400nm.
With the analytically pure Eu (NO of 0.25g
3)
39H
2O, the analytically pure Y (NO of 0.44g
3)
39H
2The VOSO of O and 0.27g content 97%
4Be dissolved in fully in the distilled water of 20ml and be mixed with mixing solutions, Eu in the solution
3+Concentration be 0.025mol/L, Y
3+Concentration be 0.05mol/L, V
4+Concentration be 0.08mol/L, this solution note is made solution 1; With the analytically pure Tb (NO of 0.20g
3)
39H
2O is dissolved in the Tb that is mixed with 0.20mol/L in the distilled water of 20ml fully
3+Solution, note is made solution 2; With the analytically pure Eu (NO of 0.25g
3)
36H
2O is dissolved in the distilled water of 20ml fully, is mixed with the Eu of 0.025mol/L
3+Solution, note is made solution 3; The sintered glass bar of choosing is divided into three sections of A, B, C, adopts segmentation to coat doping method and in the A section, immerse solution 1, in the B section, immerse solution 2, in the C section, immerse solution 3.The sintered glass that is soaked with light emitting ionic is put into corundum crucible with cover after the thorough drying in 300 ℃ of air, put into the High Temperature Furnaces Heating Apparatus sintering then.In sintering process, be raised to 900 ℃ with the heat-up rate of 10 ℃/min from room temperature, with from 900 to 1250 ℃ of the heat-up rates of 5 ℃/min, at 1150 ℃ of insulation 30min, glass is with the High Temperature Furnaces Heating Apparatus cool to room temperature afterwards then.Through 1250 ℃ solid state sintering, become closely knit transparent integrated color luminous vycor glass.This transparent glass is under the ultra violet lamp of wavelength 254nm, and the A section is sent near the ruddiness the wavelength 613nm, and the B section is sent near the green glow the wavelength 542nm, and the C section is sent near the blue light the wavelength 425nm.
Embodiment 5
With 0.35g analytical pure Samarium trioxide (Sm
2O
3) be dissolved in the Sm that is mixed with 0.10mol/L in rare nitric acid of 1mol/L of 20ml fully
3+Solution, note is made solution 1; With the analytically pure Ce (NO of 0.22g
3)
36H
2O is dissolved in the distilled water of 20ml fully, is mixed with the Ce of 0.025 mol/L
3+Solution, note is made solution 2; Manganous nitrate (Mn (NO with 0.72g content 50%
3)
3) be dissolved in fully in the distilled water of 20ml, be mixed with the Mn of 0.1mol/L
2+Solution, note is made solution 3; With the analytically pure CuCl of 0.07g
2Be dissolved in the Cu that is mixed with 0.025mol/L in the distilled water of 20ml fully
2+Solution, note is made solution 4; VOSO with 0.67g content 97%
4Be dissolved in the V that is mixed with 0.20mol/L in the distilled water of 20ml fully
4+Solution, note is made solution 5.The sintered glass bar of choosing is divided into five sections of A, B, C, D, E, adopts segmentation to coat doping method and in the A section, immerses solution 1, in the B section, immerse solution 2, in the C section, immerse solution 3, in the D section, immerse solution 4, immersion solution 5 in the E section.The sintered glass that is soaked with light emitting ionic is put into corundum crucible with cover after the thorough drying in 800 ℃ of air, and puts 20g graphite or carbon dust around glass, puts into the High Temperature Furnaces Heating Apparatus sintering then.In sintering process, be raised to 900 ℃ with the heat-up rate of 10 ℃/min from room temperature, with from 900 to 1150 ℃ of the heat-up rates of 5 ℃/min, at 1150 ℃ of insulation 30min, glass is with the High Temperature Furnaces Heating Apparatus cool to room temperature afterwards then.Through the following 1150 ℃ solid state sintering of reducing atmosphere, become closely knit transparent integrated color luminous vycor glass.This transparent glass is under the ultra violet lamp of wavelength 254nm, and that five sections of A, B, C, D, E send respectively simultaneously is orange red, the light of bluish voilet, redness, green, yellow five kinds of different colours.
Claims (5)
1. the manufacture method of an integrated color luminous vycor glass is characterized in that this method comprises the following steps:
1. prepare sintered glass, the composition of this sintered glass is as follows:
Ingredient w t%
SiO
2 ≥96.0
B
2O
3 1.0～3.0
Al
2O
3 1.0～3.0
The aperture of this sintered glass is 1.0～10 nanometers, and aperture accounts for 25～40% of glass volume;
2. according to the glow color of colorful light-emitting glass and the requirement of luminous intensity, select the kind and the concentration of Doped Rare Earth or transition metal light emitting ionic, and be mixed with corresponding rare earth or transition metal light emitting ionic solution;
3. choose the 1. the sintered glass of step preparation be raw material, adopt sectional doped method, described rare earth or transition metal light emitting ionic solution middle-weight rare earths or transition metal light emitting ionic are incorporated in the described sintered glass;
4. will be mixed with the sintered glass of rare earth or transition metal light emitting ionic, in 200～800 ℃ air, carry out drying;
5. dried light emitting ionic doped porous glass is put into High Temperature Furnaces Heating Apparatus, solid state sintering under 1100～1250 ℃ air or reducing atmosphere, eliminating micropore becomes closely knit transparent integrated color luminous vycor glass.
2. the manufacture method of integrated color luminous vycor glass according to claim 1 is characterized in that the preparation light emitting ionic solution described in described step 2. is the aqueous solution, organic solution or acid solution.
3. the manufacture method of integrated color luminous vycor glass according to claim 1 is characterized in that described light emitting ionic kind comprises singly mixing of rare earth ion and transition metal ion or mixes altogether, comprises Eu, Tb, Ce, Cu, V, Ag, Sm or Y ionic list are mixed or are mixed altogether.
4. the manufacture method of integrated color luminous vycor glass according to claim 1, the strength of solution that it is characterized in that described light emitting ionic is 0.01-0.2mol/L.
5. the manufacture method of integrated color luminous vycor glass according to claim 1 is characterized in that describedly sectional dopedly can taking two kinds of methods:
A) doping method is soaked in segmentation, and this segmentation immersion doping is meant sintered glass is divided into plurality of sections (A, C ...), each section is soaked in respectively in the different light emitting ionic solution;
B) segmentation coats doping method, this segmentation coating-doping is meant paper slip or cloth is dipped in the light emitting ionic solution, rapidly this paper slip or cloth are coated to respectively on each section of sintered glass after the taking-up, so that the light emitting ionic on sintered glass absorption paper slip or the cloth is realized mixing.
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|---|---|---|---|
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|---|---|---|---|
| CN2007101730552A CN101215093B (en) | 2007-12-26 | 2007-12-26 | Method for manufacturing integrated colorful luminous vycor glass |
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| CN101215093B CN101215093B (en) | 2010-06-09 |
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