CN101209894A - Inorganic borosilicate luminescent glass and preparation thereof - Google Patents
Inorganic borosilicate luminescent glass and preparation thereof Download PDFInfo
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- CN101209894A CN101209894A CNA2007101727719A CN200710172771A CN101209894A CN 101209894 A CN101209894 A CN 101209894A CN A2007101727719 A CNA2007101727719 A CN A2007101727719A CN 200710172771 A CN200710172771 A CN 200710172771A CN 101209894 A CN101209894 A CN 101209894A
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Abstract
The invention discloses inorganic borosilicate luminescent glass which is characterized in that the glass adopts MgO, SiO2, Eu (NO3)3 or EuCl3 or Eu2O3, H3BO3 as raw materials, and then the raw materials are mixed, added with deionized water, well mixed, heated and ground into powder; the glass is obtained after drying and calcining. The general formula is that: mM (1-x) O nSiO2 1B2O3: Eu<2+>x. The invention has uniform luminescence, high brightness, wide range of emission spectrum from blue violet light, blue light to blue-green light and simple preparation method.
Description
Technical field
The present invention relates to the luminescent material technical field, specifically a kind of inorganic borosilicate luminescent glass and preparation method thereof.
Background technology
Make first after the novel optical glass that contains lanthanum, thorium, the contour refraction of tantalum, low scattering since Corning Incorporated, rare earth opticglass has obtained very fast development, can make the special glass of different purposes by the doping of rare earth ion.The J.Qiu of Japan and K.Hirao etc. have reported the optical storage performance of long-afterglow luminescent glass, and this at home and abroad attracts great attention.More noticeable is the new phenomenon of fluorescent glass under the femtosecond laser effect, shines the glass that contains rare earth ion with femtosecond laser, observes the steady persistence phenomenon.Because the transparency of long-afterglow luminescent glass uniqueness, it not only can be used for the applied every field of polycrystal powder, in photoelectron optical tech fields such as laser, optical amplifier, optical communication, energy storage and demonstrations the potential using value is arranged also.Long-range is unordered because the network structure of glass is closely in order, and the doping of rare earth ion in glass can be higher relatively, because the constructional feature of glass, often glass is luminous all very even.But the synthetic fluorescent glass is mainly rare earth ion doped silicate glass or zinc borosilicate glass at present, and brightness is not high.
Summary of the invention
The object of the present invention is to provide a kind of inorganic borosilicate luminescent glass, its luminous efficiency height, the preparation method is simple, and is with low cost.
The concrete technical scheme that realizes the object of the invention is:
A kind of inorganic borosilicate luminescent glass, characteristics are that this glass adopts MgO, SiO
2, Eu (NO
3)
3Or EuCl
3Or Eu
2O
3, H
3BO
3Be raw material, after it is mixed, add deionized water, mix, heat, be ground to powder, dry then, calcining and getting; Its general expression is:
mM
(1-x)O·nSiO
2·l?B
2O
3:Eu
2+ x
Wherein: x=0.002～0.026; M=35.5～45%; N=20～35.5%;
L=29～40%; M represents MAGNESIUM METAL.
A kind of method for preparing above-mentioned fluorescent glass, characteristics are: get MgO, SiO
2And H
3BO
3Mix by the dose ratio in the above-mentioned formula, add the Eu (NO that accounts for magnesium oxide quality 0.2～2.6%
3)
3Or EuCl
3Or Eu
2O
3Mix, add and the deionized water of its mixture dispersion amount can be mixed, the limit heating edge is ground to Powdered, put into baking oven in 80～100 ℃ dry 10～24 hours down, again in High Temperature Furnaces Heating Apparatus with activated carbon or N
2-H
2Reduction, in 1200～1600 ℃ of calcining at constant temperature 4～6 hours, target product.
The present invention is luminous evenly, brightness is high, and the scope of emmission spectrum is big: can be from royal purple light, and blue light is to blue green light; And the preparation method is simple.
Description of drawings
Fig. 1, Fig. 3, Fig. 5, Fig. 7, Fig. 9, Figure 11, Figure 13, Figure 15 are the emmission spectrum figure of different embodiments of the invention
Fig. 2, Fig. 4, Fig. 6, Fig. 8, Figure 10, Figure 12, Figure 14, Figure 16 are the exciting light spectrogram of different embodiments of the invention
Embodiment
Embodiment 1
MgO 2.0152g, H
3BO
35.0714g, the Eu (NO of 0.100mol/l
3)
3Solution 1.00ml, SiO
23.0052g
Take by weighing above-mentioned substance, add 20ml deionized water (as solvent) and mix, limit heating (promoting the volatilization of solvent) limit is ground to Powdered; With mixture put into baking oven in 100 ℃ dry 10 hours down, again in High Temperature Furnaces Heating Apparatus with the reduction of activated carbon reducing atmosphere, in 1200 ℃ of calcining at constant temperature 4 hours, 35.5%M
(1-x)O35.5%SiO
229%B
2O
3: Eu
2+ 0.002Fluorescent glass.
Present embodiment gained fluorescent glass can be excited well by the visible light of 254～450nm wavelength region, under the 330nm ultraviolet excitation, glow color presents bright bluish voilet, the brightness height is surveyed emmission spectrum (accompanying drawing 1) and excitation spectrum (accompanying drawing 2), and the emission peak wavelength is positioned at about 434nm.
Embodiment 2
MgO 2.0156g, H
3BO
35.0716g, the Eu of 0.100mol/1
2O
30.0880g, SiO
23.0054g
Take by weighing above-mentioned substance, add 25ml deionized water (as solvent) and mix, limit heating (promoting the volatilization of solvent) limit is ground to Powdered; With mixture put into baking oven in 100 ℃ dry 10 hours down, again in High Temperature Furnaces Heating Apparatus with the reduction of activated carbon reducing atmosphere, in 1200 ℃ of calcining at constant temperature 4 hours, 35.5%M
(1-x)O35.5%SiO
229%B
2O
3: Eu
2+ 0.005Fluorescent glass.
Present embodiment gained fluorescent glass can be excited well by the visible light of 254～450nm wavelength region, under the 346nm ultraviolet excitation, glow color presents bright bluish voilet, the brightness height is surveyed emmission spectrum (accompanying drawing 3) and excitation spectrum (accompanying drawing 4), and the emission peak wavelength is positioned at about 446nm.
Embodiment 3
MgO 2.0155g, H
3BO
35.0713g, the Eu (NO of 0.100mol/l
3)
3Solution 3.80ml, SiO
23.0055g
Take by weighing above-mentioned substance, add 20ml deionized water (as solvent) and mix, limit heating (promoting the volatilization of solvent) limit is ground to Powdered; With mixture put into baking oven in 100 ℃ dry 10 hours down, again in High Temperature Furnaces Heating Apparatus with the reduction of activated carbon reducing atmosphere, in 1200 ℃ of calcining at constant temperature 4 hours, 35.5%Mg
(1-x)O35.5%SiO
229%3B
2O
3: Eu
0.007Luminescent material.
Present embodiment gained fluorescent glass can be excited well by the visible light of 254～450nm wavelength region, under the 349nm ultraviolet excitation, glow color presents bright blueness, the brightness height is surveyed emmission spectrum (accompanying drawing 5) and excitation spectrum (accompanying drawing 6), and the emission peak wavelength is positioned at about 452nm.
Embodiment 4
MgO 2.0154g, H
3BO
35.0718g, the Eu (NO of 0.100mol/l
3)
3Solution 12.8ml, SiO
23.0053g
Take by weighing above-mentioned substance, add 15ml deionized water (as solvent) and mix, limit heating (promoting the volatilization of solvent) limit is ground to Powdered; With mixture put into baking oven in 100 ℃ dry 10 hours down, again in High Temperature Furnaces Heating Apparatus with the reduction of activated carbon reducing atmosphere, in 1600 ℃ of calcining at constant temperature 4 hours, 35.5%M
(1-x)O35.5%SiO
229%B
2O
3: Eu
2+ 0.026Fluorescent glass.
Present embodiment gained fluorescent glass can be excited well by the visible light of 254～450nm wavelength region, under the 443nm ultraviolet excitation, the blue-greenish colour that glow color presents, the brightness height is surveyed emmission spectrum (accompanying drawing 7) and excitation spectrum (accompanying drawing 8), and the emission peak wavelength is positioned at about 505nm.
Embodiment 5
MgO 2.0154g, H
3BO
34.1224g, the Eu (NO of 0.100mol/l
3)
3Solution 2.5ml, SiO
21.6688g
Take by weighing above-mentioned substance, add 25ml deionized water (as solvent) and mix, limit heating (promoting the volatilization of solvent) limit is ground to Powdered; With mixture put into baking oven in 100 ℃ dry 15 hours down, again in High Temperature Furnaces Heating Apparatus with the reduction of activated carbon reducing atmosphere, in 1300 ℃ of calcining at constant temperature 4 hours, 45%Mg
(1-x)O25%SiO
230%B
2O
3: Eu
2+ 0.005Fluorescent glass.
Present embodiment gained fluorescent glass can be excited well by the visible light of 254～450nm wavelength region, under the 359nm ultraviolet excitation, glow color presents bright blueness, the brightness height is surveyed emmission spectrum (accompanying drawing 9) and excitation spectrum (accompanying drawing 10), and the emission peak wavelength is positioned at about 463nm.
MgO 2.0154g, H
3BO
34.1226g, the Eu (NO of 0.100mol/l
3)
3Solution 7.50ml, SiO
21.6686g
Take by weighing above-mentioned substance, add 20ml deionized water (as solvent) and mix, limit heating (promoting the volatilization of solvent) limit is ground to Powdered; With mixture put into baking oven in 100 ℃ dry 24 hours down, again in High Temperature Furnaces Heating Apparatus with the reduction of activated carbon reducing atmosphere, in 1300 ℃ of calcining at constant temperature 4 hours, 45%Mg
(1-x)O25%SiO
230%B
2O
3: Eu
2+ 0.015Fluorescent glass.
Present embodiment gained fluorescent glass, can be excited well by the visible light of 254～450nm wavelength region, under the 421nm ultraviolet excitation, glow color presents bright blue-greenish colour, the brightness height, survey emmission spectrum (accompanying drawing 11) and excitation spectrum (accompanying drawing 12), the emission peak wavelength is positioned at about 490nm.
Embodiment 7
MgO 2.0152g, H
3BO
34.1225g, the EuCl of 0.100mol/l
3Solution 10.0ml, SiO
21.6686g
Take by weighing above-mentioned substance, add about 20ml deionized water (as solvent) and mix, limit heating (promoting the volatilization of solvent) limit is ground to Powdered; With mixture put into baking oven in 100 ℃ dry 24 hours down, again in High Temperature Furnaces Heating Apparatus with the reduction of gac reducing atmosphere, in 1300 ℃ of calcining at constant temperature 4 hours, Mg
(1-x)O45%SiO
225%B
2O
330%:Eu
2+ 0.020Fluorescent glass.
Present embodiment gained fluorescent glass, can be excited well by the visible light of 254～450nm wavelength region, under the 428nm ultraviolet excitation, glow color presents bright blue-greenish colour, the brightness height, survey emmission spectrum (accompanying drawing 13) and excitation spectrum (accompanying drawing 14), the emission peak wavelength is positioned at about 492nm.
Embodiment 8
MgO 2.0152g, H
3BO
36.1836g, the Eu (NO of 0.100mol/l
3)
3Solution 2.5ml, SiO
21.5026g
Take by weighing above-mentioned substance, add 20ml deionized water (as solvent) and mix, limit heating (promoting the volatilization of solvent) limit is ground to Powdered; With mixture put into baking oven in 80 ℃ dry 24 hours down, again in High Temperature Furnaces Heating Apparatus with N
2-H
2Reducing atmosphere reduction, in 1300 ℃ of calcining at constant temperature 6 hours, 40%Mg
(1-x)O20%SiO
240%B
2O
3: Eu
2+ 0.005Fluorescent glass.
Present embodiment gained fluorescent glass can be excited well by the visible light of 254 ~ 450nm wavelength region, under the 365nm ultraviolet excitation, glow color presents bright blueness, the brightness height is surveyed emmission spectrum (accompanying drawing 15) and excitation spectrum (accompanying drawing 16), and the emission peak wavelength is positioned at about 454nm.
Claims (2)
1. an inorganic borosilicate luminescent glass is characterized in that this glass adopts MgO, SiO
2, Eu (NO
3)
3Or EuCl
3Or Eu
2O
3, H
3BO
3Be raw material, after it is mixed, add deionized water, mix, heat, be ground to powder, dry then, calcining and getting; Its general expression is:
mM
(1-x)O·nSiO
2·l?B
2O
3:Eu
2+ x
Wherein: x=0.002～0.026; M=35.5～45%; N=20～35.5%;
L=29～40%; M represents MAGNESIUM METAL.
2. a method for preparing the described fluorescent glass of claim 1 is characterized in that getting MgO, SiO
2And H
3BO
3Mix by the dose ratio in the above-mentioned formula, add the Eu (NO that accounts for magnesium oxide quality 0.2～2.6%
3)
3Or EuCl
3Or Eu
2O
3Mix, add and the deionized water of its mixture dispersion amount can be mixed, the limit heating edge is ground to Powdered, put into baking oven in 80～100 ℃ dry 10～24 hours down, again in High Temperature Furnaces Heating Apparatus with activated carbon or N
2-H
2Reduction, in 1200～1600 ℃ of calcining at constant temperature 4～6 hours, target product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101727719A CN101209894A (en) | 2007-12-21 | 2007-12-21 | Inorganic borosilicate luminescent glass and preparation thereof |
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|---|---|---|---|
| CNA2007101727719A CN101209894A (en) | 2007-12-21 | 2007-12-21 | Inorganic borosilicate luminescent glass and preparation thereof |
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|---|---|
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ID=39610173
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830638A (en) * | 2009-03-13 | 2010-09-15 | 中国科学院福建物质结构研究所 | Novel europium ion-doped high-brightness cyan silicate light emitting glass |
| CN108059338A (en) * | 2017-12-26 | 2018-05-22 | 陕西科技大学 | A kind of preparation method of red light emitting glass |
| CN108164132A (en) * | 2017-12-26 | 2018-06-15 | 陕西科技大学 | A kind of preparation method for mixing yttrium jaundice green light glass |
-
2007
- 2007-12-21 CN CNA2007101727719A patent/CN101209894A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830638A (en) * | 2009-03-13 | 2010-09-15 | 中国科学院福建物质结构研究所 | Novel europium ion-doped high-brightness cyan silicate light emitting glass |
| CN108059338A (en) * | 2017-12-26 | 2018-05-22 | 陕西科技大学 | A kind of preparation method of red light emitting glass |
| CN108164132A (en) * | 2017-12-26 | 2018-06-15 | 陕西科技大学 | A kind of preparation method for mixing yttrium jaundice green light glass |
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Open date: 20080702 |