CN1239421C - Glass material with photosensitivity - Google Patents
Glass material with photosensitivity Download PDFInfo
- Publication number
- CN1239421C CN1239421C CN 200410027831 CN200410027831A CN1239421C CN 1239421 C CN1239421 C CN 1239421C CN 200410027831 CN200410027831 CN 200410027831 CN 200410027831 A CN200410027831 A CN 200410027831A CN 1239421 C CN1239421 C CN 1239421C
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- Prior art keywords
- glass
- photosensitivity
- glass material
- irradiation
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- 239000011521 glass Substances 0.000 title claims abstract description 83
- 239000000463 material Substances 0.000 title claims abstract description 24
- 206010034972 Photosensitivity reaction Diseases 0.000 title claims abstract description 22
- 230000036211 photosensitivity Effects 0.000 title claims abstract description 22
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000835 fiber Substances 0.000 abstract description 9
- 239000013307 optical fiber Substances 0.000 abstract description 7
- 239000000377 silicon dioxide Substances 0.000 abstract description 4
- 229910003439 heavy metal oxide Inorganic materials 0.000 abstract description 3
- 230000003287 optical effect Effects 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 4
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 239000011162 core material Substances 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 230000010354 integration Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 239000012298 atmosphere Substances 0.000 description 14
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000003723 Smelting Methods 0.000 description 8
- 230000001590 oxidative effect Effects 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
- 238000004891 communication Methods 0.000 description 4
- 239000000306 component Substances 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000009423 ventilation Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000075 oxide glass Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- VTYDSHHBXXPBBQ-UHFFFAOYSA-N boron germanium Chemical compound [B].[Ge] VTYDSHHBXXPBBQ-UHFFFAOYSA-N 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000005308 flint glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000010365 information processing Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000005355 lead glass Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000382 optic material Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000006089 photosensitive glass Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/04—Compositions for glass with special properties for photosensitive glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The present invention discloses glass material with photosensitivity. The glass material is prepared from 3 to 10 parts of Na2O, 10 to 30 parts of Bi2O3 and 50 to 70 parts of SiO2 measured by mol fraction. The glass material of the present invention can be used for manufacturing fiber core material of optical fibers, substrate material of integrated photonic wave guide devices, and optical storage medium material with refractivity change caused by ultraviolet lights. The glass material contains a heavy metal oxide of Bi2O3, which is favorable to the integration of photonic devices.
Description
Technical field
The present invention relates to a kind of glass material with photosensitivity.
Background technology
Continuous increase along with information processing capacity, the dense wave division multipurpose that combines with fiber grating (DWDM) system is the trend of following optical communication development, has dispersion compensation, filtering, the signal gain amplifier is smooth and multi-functional fiber grating such as sensing will be an indispensable core component in the following all-optical network.To be faced with huge demand as fiber grating with photosensitive fiber optic materials.And after the standard traffic optical fiber of use was subjected to UV-irradiation now, its variations in refractive index was about 10
-5The order of magnitude.This is for the grating device of making high-reflectivity, wide bandwidth (bandwidth is greater than 1nm, and reflectivity reaches 100%), and this value is too little beyond doubt.Right figure shows is the relation of grating reflection rate and bandwidth under the different modulating specific refractory power, as can be seen from the figure, wants to make and adapts to the high-speed communications grating, and the photon-induced refractive index variable quantity will reach 10
-3More than.
Though carry (H by hydrogen
2-loading), brush fire post-processing technologies such as (Flame-brushing), the photon-induced refractive index of optical fiber is changed reach 10
-3The order of magnitude.But the long post-processed time, elapsed time not only, the danger in the time of also can bringing fused fiber splice.In addition, use post-processing technique can not realize the online grating that writes, thereby can not satisfy requirement of producing grating fast in enormous quantities.Address these problems, need starting with from material---the photosensitivity that raising is used for making the fiber grating material itself.Abroad, mix the photosensitivity that improves optical fiber altogether by the incorporation of germanium (Ge) in the increase silica fibre or by boron germanium (B/Ge), but the height of development mixes germanium and B-Ge-codoped optical fiber photosensitivity deficiency (is generally 10
-4The order of magnitude) and axially photosensitivity is inhomogeneous, has limited its application.Subsequently, people explore again and mix rare earth ion in silica glasss, as: Ta
3+, Ce
3+, Er
3+, Eu
2+, Tb
3+Deng.Though these rare earth elements can improve the photosensitivity of glass to a certain extent, can not satisfy the online requirement that writes the high light grid fast equally.In recent years, some optical communication research units turn to multicomponent glass with research emphasis one after another in the world.
Oxide glass with excellent high stability becomes after silica glass by the multicomponent glass of broad scale research.As, in Ge-Si, P-Si glass, add the photosensitivity that Sn improves glass, by mixing the optical fiber that the Sn glass-pulling becomes, the variable quantity maximum of its photon-induced refractive index can reach 10
-3, and SnO keeping lower absorption at third communication window, and the stability under its high temperature is more much better than B/Ge optical fiber.In addition, the hi-tech investigation of materials center of U.S. University of New Mexico and Britain Southampton university photoelectron research centre are discovered recently: lead-silica glass is after the UV-irradiation of 266nm, the maximum value of its variations in refractive index can reach 0.1, and they discover: along with the increase of PbO content, the photosensitivity of glass increases.And silica glass has only very weak photosensitivity, so the adding that derives from Pb of photosensitivity in the silicon lead glass.Pb is the element of the 4th main group in the periodic table of elements, and ordination number is 82, and peripheral electron is arranged and is 6s
26p
2, so it can lose 2 electronics or 4 electronics and forms stable compound.Pb can change the characteristic of valence state, makes flint glass have photosensitivity.Under the irradiation of UV-light, ion pb appraises at the current rate
2+Valence state change, in glass, form point defect.Point defect in the glass network structure absorbs the ultraviolet photon energy, and defect structure is changed.Thereby cause the variation of glass uptake factor, finally cause the variation of glass refraction.
Summary of the invention
The object of the present invention is to provide a kind of photosensitivity glass material with ultraviolet light induced variations in refractive index.
For achieving the above object, the present invention has taked following technical scheme:
A kind of glass material with photosensitivity in molar part, is grouped into by following one-tenth:
Na
2O 3～10
Bi
2O
3 10～30
SiO
2 50～70；
The fusion-cast method is adopted in the preparation of glass: promptly by said components proportioning raw materials weighing powder weight, load weighted each raw material is mixed in crucible, place SiC electric furnace internal heating to 1100～1250 ℃ then, glass metal is through stirring, being cast on the stainless steel template after the ventilation clarification.Adopt two kinds of atmosphere in the glass smelting process, a kind of is logical exsiccant oxygen in glass metal; Another kind is a logical exsiccant nitrogen in glass metal.After glass smelting finishes, be prepared into glass sample by operations such as annealing, cutting, polishings.
Compared with the prior art, the present invention has following beneficial effect: in prepared glass, contain heavy metal oxide Bi
2O
3, and rare earth ion doped heavy metal oxide glass is one of photonic device usefulness substrate material, realization of the present invention helps realizing the integrated of photonic device, and the integrated of photonic device is the important trend of current photonic device development.
Description of drawings
Fig. 1 be under the different modulating specific refractory power grating reflection rate and broadband concern synoptic diagram;
Fig. 2 is the testing method of glass variations in refractive index after UV-irradiation;
Fig. 3 under the 248nm UV-irradiation, the variation of the glass transmitance of founding under the oxidizing atmosphere;
Fig. 4 under the 248nm UV-irradiation, the variation of the glass transmitance of founding under the nitrogen atmosphere;
Fig. 5 is under the 248nm UV-irradiation, and the variation of glass colour is under the A nitrogen atmosphere; Under the B oxygen atmosphere.
Embodiment
The invention will be further described below in conjunction with Figure of description and specific embodiment.
Embodiment 1
The prescription of glass material and preparation method: (following is molfraction)
Na
2O 7
Bi
2O
3 21
SiO
2 65；
By said components proportioning raw materials weighing powder, load weighted each raw material is mixed in crucible, place SiC electric furnace internal heating to 1200 ℃ then, glass metal through stir, ventilation is cast on the stainless steel template after clarifying.Adopt two kinds of atmosphere in the glass smelting process, a kind of is logical exsiccant oxygen in glass metal; Another kind is a logical exsiccant nitrogen in glass metal.After glass smelting finishes, be prepared into glass sample by operations such as annealing, cutting, polishings.
Embodiment 2
The prescription of glass material and preparation method: (following is the molar part proportioning)
Na
2O 3
Bi
2O
3 10
SiO
2 50
By said components proportioning raw materials weighing powder weight, load weighted each raw material is mixed in crucible, place SiC electric furnace internal heating to 1100 ℃ then, glass metal through stir, ventilation is cast on the stainless steel template after clarifying.Adopt two kinds of atmosphere in the glass smelting process, a kind of is logical exsiccant oxygen in glass metal; Another kind is a logical exsiccant nitrogen in glass metal.After glass smelting finishes, be prepared into glass sample by operations such as annealing, cutting, polishings.
Embodiment 3
The prescription of glass material and preparation method: (molar part proportioning)
Na
2O 10
Bi
2O
3 30
SiO
2 70；
By said components proportioning raw materials weighing powder weight, load weighted each raw material is mixed in crucible, place SiC electric furnace internal heating to 1250 ℃ then, glass metal through stir, ventilation is cast on the stainless steel template after clarifying.Adopt two kinds of atmosphere in the glass smelting process, a kind of is logical exsiccant oxygen in glass metal; Another kind is a logical exsiccant nitrogen in glass metal.After glass smelting finishes, be prepared into glass sample by operations such as annealing, cutting, polishings.
Below embodiment 1 preparation-obtained glass is tested:
Fig. 2 is the testing method of glass variations in refractive index after UV-irradiation: ultraviolet source adopts 248nmKrF excimer laser, repetition rate 10Hz, single pulse energy 0～1000mJ/cm
2Glass is after UV-irradiation, and change of refractive adopts legal test of prism lotus root, and the precision of this method of testing is 5 * 10
-5
Fig. 3 is 400mJ/cm for preparation glass under the oxidizing atmosphere through single pulse energy
2Laser radiation before and after see through spectrographic and change.
Fig. 4 is the spectrum that sees through of nitrogen atmosphere lower-glass.No matter be in oxidizing atmosphere or the glass that in nitrogen atmosphere, prepares, through after the UV-irradiation, glass reduces in the transmitance of visible region, and the variation of the transmitance of the glass for preparing under the oxidizing atmosphere is maximum, and the photon-induced refractive index that can be calculated glass by formula (1) changes.
Table 1 and 2 has shown the glass for preparing after UV-irradiation under oxidizing atmosphere, the test result of variations in refractive index.Along with the increase of UV-irradiation energy, the glass refraction variation reaches the used time shortening of maximum value.Along with the prolongation of irradiation time, the variation of glass refraction reduces gradually subsequently, last even reinstatement.Shown the distinctive character of photosensitive glass, promptly the change of refractive that causes of UV-light can realize wiping by heat or light, and glass is restored to the original state.The plumbous germanite glass for preparing under the oxidizing atmosphere after tested, its ultraviolet light induced change of refractive is 2～3 * 10
-4
Table 3 is the change of refractive of institute's fusion cast glass under the nitrogen atmosphere, and the variations in refractive index maximum of glass reaches 6 * 10 when 2min
-4Its value is greater than the ultraviolet change of refractive of institute's fusion cast glass under the oxidizing atmosphere, but the spectrum that sees through from glass, it is high that the ultraviolet light induced variations in refractive index of the glass of founding under the oxidizing atmosphere is wanted, but test result is on the contrary, and the size of this description defect concentration is relevant with the atmosphere of fusion cast glass.
Fig. 5 is the shape appearance figure of glass after UV-irradiation.As can be seen, glass is after UV-irradiation, and its color all deepens, and illustrates to have formed the oxide compound of Bi at a low price.
In sum: under the 248nmKrF excimer laser irradiation, found that there is photosensitivity in the bismuth silex glass.The amplitude of bismuth silex glass variations in refractive index is 2～6 * 10
-4Between, the photosensitivity that this value and B/Ge annotate silica fibre altogether is suitable.
Table 1 laser single-pulse energy is 30mJ/cm
2The time glass refraction with the variation of irradiation time
The specific refractory power of the specific refractory power 1550nm of time (min) 632nm
0 1.96349(TE) 1.96330(TM) 1.91322(TE) 1.91312(TM)
2.5 1.96349(TE) 1.96340(TM) 1.91323(TE) 1.91312(TM)
5 1.96359(TE) 1.96349(TM) 1.91333(TE) 1.91322(TM)
10 1.96378(TE) 1.96349(TM) 1.91343(TE) 1.91333(TM)
15 1.96349(TE) 1.96349(TM) 1.91333(TE) 1.91322(TM)
Table 2 laser single-pulse energy is 400mJ/cm
2The time glass refraction with the variation of irradiation time
The specific refractory power at the specific refractory power 1550nm place at time (min) 632nm place
0 1.96349(TE) 1.96330(TM) 1.91322(TE) 1.91312(TM)
5 1.96368(TE) 1.96359(TM) 1.91343(TE) 1.91333(TM)
10 1.96340(TE) 1.96330(TM) 1.91322(TE) 1.91312(TM)
15 1.96349(TE) 1.96349(TM) 1.91333(TE) 1.91322(TM)
Table 3 laser single-pulse energy is 30mJ/cm
2The time glass refraction with the variation of irradiation time
The specific refractory power at time (S) 632nm place
0 1.89278
5 1.89290
10 1.89302
30 1.89314
60 1.89326
120 1.89338
180 1.89302
300 1.89302
Claims (4)
1, a kind of glass material with photosensitivity is characterized in that in molar part, is made up of following material:
Na
2O 3～10
Bi
2O
3 10～30
SiO
2 50～70。
2, the glass material with photosensitivity according to claim 1 is characterized in that in molar part, is made up of following material:
Na
2O 7
Bi
2O
3 21
SiO
2 65。
3, the glass material with photosensitivity according to claim 1 is characterized in that in molar part, is made up of following material:
Na
2O 3
Bi
2O
3 10
SiO
2 50。
4, the glass material with photosensitivity according to claim 1 is characterized in that in molar part, is made up of following material:
Na
2O 10
Bi
2O
3 30
SiO
2 70。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410027831 CN1239421C (en) | 2004-06-30 | 2004-06-30 | Glass material with photosensitivity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410027831 CN1239421C (en) | 2004-06-30 | 2004-06-30 | Glass material with photosensitivity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1594162A CN1594162A (en) | 2005-03-16 |
| CN1239421C true CN1239421C (en) | 2006-02-01 |
Family
ID=34664036
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410027831 Expired - Lifetime CN1239421C (en) | 2004-06-30 | 2004-06-30 | Glass material with photosensitivity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1239421C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110407466A (en) * | 2019-06-17 | 2019-11-05 | 江苏双兴工贸有限公司 | A kind of formula and its manufacturing method of Full-color photosensitive glass vessel |
| CN111505842B (en) * | 2020-04-30 | 2023-11-10 | 温州激光与光电子协同创新中心 | Passive photosensitive device for improving laser power stability and implementation and test method thereof |
| CN115818957B (en) * | 2022-12-06 | 2024-06-25 | 中国建筑材料科学研究总院有限公司 | High-photosensitivity low-elastic modulus optical glass, and preparation method and application thereof |
-
2004
- 2004-06-30 CN CN 200410027831 patent/CN1239421C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| CN1594162A (en) | 2005-03-16 |
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