CN1644543A - Erbium-doped lead-free germanium bismuth glass and preparation method thereof - Google Patents
Erbium-doped lead-free germanium bismuth glass and preparation method thereof Download PDFInfo
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- CN1644543A CN1644543A CN 200410093208 CN200410093208A CN1644543A CN 1644543 A CN1644543 A CN 1644543A CN 200410093208 CN200410093208 CN 200410093208 CN 200410093208 A CN200410093208 A CN 200410093208A CN 1644543 A CN1644543 A CN 1644543A
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- glass
- erbium
- preparation
- leadfree
- dosed
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Links
- 239000011521 glass Substances 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- CWCCJSTUDNHIKB-UHFFFAOYSA-N $l^{2}-bismuthanylidenegermanium Chemical compound [Bi]=[Ge] CWCCJSTUDNHIKB-UHFFFAOYSA-N 0.000 title abstract 3
- 230000007704 transition Effects 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims description 20
- 229910052797 bismuth Inorganic materials 0.000 claims description 16
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 16
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 229910052691 Erbium Inorganic materials 0.000 claims description 12
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 6
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims description 6
- 238000005273 aeration Methods 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000005352 clarification Methods 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 229910001882 dioxygen Inorganic materials 0.000 claims description 6
- 230000004927 fusion Effects 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 229910005793 GeO 2 Inorganic materials 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 239000010431 corundum Substances 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 7
- 238000002474 experimental method Methods 0.000 abstract description 3
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 abstract 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 abstract 1
- 238000000137 annealing Methods 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000004455 differential thermal analysis Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000005357 flat glass Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000004020 luminiscence type Methods 0.000 description 3
- 239000005385 borate glass Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000005365 phosphate glass Substances 0.000 description 2
- 239000005368 silicate glass Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 241000931526 Acer campestre Species 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007648 laser printing Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000004304 visual acuity Effects 0.000 description 1
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
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent 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
- C03C3/12—Silica-free oxide glass compositions
- C03C3/253—Silica-free oxide glass compositions containing germanium
Landscapes
- 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 invention relates to a novel glass material, in particular to erbium-doped lead-free bismuth germanium glass and a preparation method thereof. The glass comprises the following components in percentage by mole: GeO2 62％；Bi2O3 30～37％；Er2O30.5-2%; the transition temperature of the glass is 360-385 ℃, the stability parameter delta T of the glass is more than or equal to 80 ℃, and delta Tmax155 ℃. Experiments prove that the erbium-doped lead-free bismuth germanium glass has high transition temperature and high stability, and the system glass has strong up-conversion red and green light output, so that the glass is a good up-conversion material.
Description
Technical field
The present invention relates to the novel glass material, especially a kind of erbium dosed leadfree bismuth germanate glass and preparation method thereof.
Background technology
The up-conversion luminescence of er-doped material is having great application prospect aspect colour demonstration, optical storage, photoelectron and the medical diagnosis, is subjected to broad research in the last few years.For example in optical disc storage, since the quantity of information of optical disc storage be " read/write head " optical maser wavelength inverse square function, if the blue-green Laser with the short wavelength substitutes ruddiness " read/write head ", existing CD capacity can be improved about 4 times. it is reported, the researchist of Japan Sony company utilizes the 515nm laser apparatus, has successfully made the optical disc storage system of capacity 7.7G bit.In Laser Printing equipment, blue-green Laser can improve print speed and resolving power.Compare with crystalline material, glass material is convenient to be processed into optical waveguides and optical fiber, thereby become a kind of blue-green Laser that has a competitive power with substrate material (referring to technology P.V.dos Santos formerly, M.V.D.Vermelho, E.A.Gouveia, Efficientenergy upconversion emission in Tm
3+/ Yb
3+-codoped TeO
2-based opticalglasses excited at 1.064 μ m, Appl.Phys.Lett., 90 (2001) 6550-6552).The principal element that influences up-conversion luminescence efficient is the maximum phonon energy of substrate material, and maximum phonon can be more little, and non-radiative relaxation rate is just more little, and last efficiency of conversion is also just high more.The maximum phonon of glass can ordering from low to high be: bismuth germanate glass＜bismuth germanate glass＜silicate glass＜phosphate glass＜borate glass.Thereby the up-conversion luminescence efficient of bismuth germanate glass is far above bismuth germanate glass, silicate glass, phosphate glass and borate glass.(referring to technology Zhongmin Yang formerly, Shiqing Xu, Lili Hu, Zhonghong Jiang.Thermal analysis and opticalproperties of Yb
3+/ Er
3+-codoped oxyfluoride germanate glasses, J.Opt.Soc.Am.B 21 (2004) 951).But consider that from the angle of environment protection and preparation safety unleaded heavy metal glass has more widely to be used.Thereby in order to satisfy current needs, it is necessary exploring the unleaded heavy metal glass of novel er-doped that has good stability.
Summary of the invention
For solving the deficiencies in the prior art, the invention provides a kind of erbium dosed leadfree bismuth germanate glass and preparation method thereof.
Technical solution of the present invention is as follows:
A kind of erbium dosed leadfree bismuth germanate glass comprises following component, in molar percentage:
GeO
2 62％；
Bi
2O
3 30～37％；
Er
2O
30.5～2%; The transition temperature of this glass is at 360～385 ℃, stability, glass parameter Δ T 〉=80 ℃, Δ T
Max=155 ℃.
Above-mentioned erbium dosed leadfree bismuth germanate glass can comprise that also molar percentage is 0～7% La
2O
3
A kind of preparation method of erbium dosed leadfree bismuth germanate glass, step is as follows:
1.: the molar percentage of forming by glass calculates weight of glass per-cent, takes by weighing raw material then, mixes;
2.: compound is put into crucible, place 1200～1250 ℃ electric furnace fusion, melting time is controlled at 20～30min;
3.: behind the glass melting, be cooled to 1150～1200 ℃, feed high purity oxygen gas and dewater, what of raw material aeration time be decided by;
4.: stop logical oxygen, glass metal is warmed up to 1200～1250 ℃ carries out clarification and homogenization, then glass metal is poured in the mould of preheating;
5.: glass put into be warming up to transition temperature (T
g) retort furnace in, be incubated after 2 hours, be annealed to about 150 ℃ with 15 ℃/hour speed, and then after being annealed to 80 ℃ with 20 ℃/hour speed, close retort furnace, be cooled to room temperature and get final product.
Above-mentioned crucible is corundum or platinum crucible, and electric furnace is a silicon carbon rod electric furnace.
The experiment proved that: erbium dosed leadfree bismuth germanate glass of the present invention has high transition temperature, high stability, and this system glass has very strong upward conversion red-green glow output simultaneously, illustrates that this glass is a kind of good up-conversion.
Description of drawings
Fig. 1 is the last transition diagram of erbium dosed leadfree bismuth germanate glass of the present invention.
Embodiment
4 specific embodiments of erbium dosed leadfree bismuth germanate glass of the present invention are as shown in table 1:
Table 1
Component (mol%) embodiment 1 embodiment 2 embodiment 3 embodiment 4
GeO
2 62 62 62 62
Bi
2O
3 37 35 32 30
La
2O
3 0 2.5 4 7
Er
2O
3 1 0.5 2 1
T
g(℃) 465 475 488 490
T
x(℃) 546 565 599 635
ΔT(℃) 81 90 111 145
Annotate: T
gBe glass transformation temperature, T
xBe the crystallization starting temperature, Δ T=T
x-T
g
Embodiment 1:
Composition is shown in embodiment in the table 11, and concrete preparation method comprises the following steps:
1.: the molar percentage of forming by glass (mol%) calculates weight of glass per-cent, takes by weighing raw material then, mixes;
2.: compound is put into corundum crucible, place 1200 ℃ silicon carbon rod electric furnace fusion, according to the length that how much determines melting time of raw material;
3.: behind the glass melting, be cooled to 1150 ℃, feed high purity oxygen gas and dewater, what of raw material aeration time be decided by;
4.: stop logical oxygen, glass metal is warmed up to 1200 ℃ carries out clarification and homogenization, what of raw material its time also depend on, then glass metal poured in the mould of preheating;
5.: fast glass is put into the retort furnace that is warming up to 465 ℃, be incubated after 2 hours, be annealed to about 150 ℃, and then after being annealed to 80 ℃ with 20 ℃/hour speed, close retort furnace, be cooled to room temperature with 15 ℃/hour speed.
Test result to this glass is as follows:
Get 10 milligrams sample after the annealing, be ground into very thin powder, carry out differential thermal analysis with agate mortar.The T that records
gBe 465 ℃, T
xIt is 546 ℃.Can calculate Δ T according to above two characteristic temperatures is 81 ℃.
Sample after the annealing is processed into the sheet glass of 3 mm thick of six mirror polish, and inversion spectrum test in is found to export just can obtaining to change red-green glow on very strong under the laser pumping of 80mW.
Embodiment 2:
Composition is shown in embodiment in the table 12, and concrete preparation method comprises the following steps:
1.: the molar percentage of forming by glass (mol%) calculates weight of glass per-cent, takes by weighing raw material then, mixes;
2.: compound is put into platinum crucible, place 1200 ℃ silicon carbon rod electric furnace fusion, according to the length that how much determines melting time of raw material;
3.: behind the glass melting, be cooled to 1150 ℃, feed high purity oxygen gas and dewater, what of raw material aeration time be decided by;
4.: stop logical oxygen, glass metal is warmed up to 1200 ℃ carries out clarification and homogenization, what of raw material its time also depend on, then glass metal poured in the mould of preheating;
5.: fast glass is put into the retort furnace that is warming up to 475 ℃, be incubated after 2 hours, be annealed to about 150 ℃, and then after being annealed to 80 ℃ with 20 ℃/hour speed, close retort furnace, be cooled to room temperature with 15 ℃/hour speed.
Test result to this glass is as follows:
Get 10 milligrams sample after the annealing, be ground into very thin powder, carry out differential thermal analysis with agate mortar.The T that records
gBe 475 ℃, T
xIt is 565 ℃.Can calculate Δ T according to above two characteristic temperatures is 90 ℃.
Sample after the annealing is processed into the sheet glass of 3 mm thick of six mirror polish, and inversion spectrum test in is found to export just can obtaining to change red-green glow on very strong under the laser pumping of 80mW.
Embodiment 3:
Composition is shown in embodiment in the table 13, and concrete preparation method comprises the following steps:
1.: the molar percentage of forming by glass (mol%) calculates weight of glass per-cent, takes by weighing raw material then, mixes;
2.: compound is put into platinum crucible, place 1250 ℃ silicon carbon rod electric furnace fusion, according to the length that how much determines melting time of raw material;
3.: behind the glass melting, be cooled to 1200 ℃, feed high purity oxygen gas and dewater, what of raw material aeration time be decided by;
4.: stop logical oxygen, glass metal is warmed up to 1250 ℃ carries out clarification and homogenization, what of raw material its time also depend on, then glass metal poured in the mould of preheating;
5.: fast glass is put into the retort furnace that is warming up to 488 ℃, be incubated after 2 hours, be annealed to about 150 ℃, and then after being annealed to 80 ℃ with 20 ℃/hour speed, close retort furnace, be cooled to room temperature with 15 ℃/hour speed.
Test result to this glass is as follows:
Get 10 milligrams sample after the annealing, be ground into very thin powder, carry out differential thermal analysis with agate mortar.The T that records
gBe 488 ℃, T
xIt is 599 ℃.Can calculate Δ T according to above two characteristic temperatures is 111 ℃.
Sample after the annealing is processed into the sheet glass of 3 mm thick of six mirror polish, and inversion spectrum test in is found to export just can obtaining to change red-green glow on very strong under the laser pumping of 80mW.
Embodiment 4:
Composition is shown in embodiment in the table 14, and concrete preparation method comprises the following steps:
1.: the molar percentage of forming by glass (mol%) calculates weight of glass per-cent, takes by weighing raw material then, mixes;
2.: compound is put into platinum crucible, place 1250 ℃ silicon carbon rod electric furnace fusion, according to the length that how much determines melting time of raw material;
3.: behind the glass melting, be cooled to 1200 ℃, feed high purity oxygen gas and dewater, what of raw material aeration time be decided by;
4.: stop logical oxygen, glass metal is warmed up to 1250 ℃ carries out clarification and homogenization, what of raw material its time also depend on, then glass metal poured in the mould of preheating;
5.: fast glass is put into the retort furnace that is warming up to 490 ℃, be incubated after 2 hours, be annealed to about 150 ℃, and then after being annealed to 80 ℃ with 20 ℃/hour speed, close retort furnace, be cooled to room temperature with 15 ℃/hour speed.
Test result to this glass is as follows:
Get 10 milligrams sample after the annealing, be ground into very thin powder, carry out differential thermal analysis with agate mortar.The T that records
gBe 490 ℃, T
xIt is 635 ℃.Can calculate Δ T according to above two characteristic temperatures is 145 ℃.
Sample after the annealing is processed into the sheet glass of 3 mm thick of six mirror polish, and inversion spectrum test in is found to export just can obtaining to change red-green glow on very strong under the laser pumping of 80mW.
In the process of founding, melting technology is controlled improper meeting and is caused the small devitrification of glass edge.The transition temperature of this glass that we obtain in the experiment is at 465～490 ℃, stability, glass parameter Δ T 〉=81 ℃, Δ T
Max=145 ℃, this system glass has very strong upward conversion red-green glow output simultaneously, illustrates that this glass is a kind of good up-conversion.
Claims (4)
1, a kind of erbium dosed leadfree bismuth germanate glass, it comprises following component, in molar percentage:
GeO
2 62％；
Bi
2O
3 30～37％；
Er
2O
3 0.5～2％；
The transition temperature of this glass is at 360～385 ℃, stability, glass parameter Δ T 〉=80 ℃, Δ T
Max=155 ℃.
2, erbium dosed leadfree bismuth germanate glass according to claim 1 is characterized in that comprising that molar percentage is 0～7% La
2O
3
3, a kind of preparation method of erbium dosed leadfree bismuth germanate glass, step is as follows:
1.: the molar percentage of forming by claim 1,2 described glass calculates weight of glass per-cent, takes by weighing raw material then, mixes;
2.: compound is put into crucible, place 1200～1250 ℃ electric furnace fusion, melting time is controlled at 20～30min;
3.: behind the glass melting, be cooled to 1150～1200 ℃, feed high purity oxygen gas and dewater, what of raw material aeration time be decided by;
4.: stop logical oxygen, glass metal is warmed up to 1200～1250 ℃ carries out clarification and homogenization, then glass metal is poured in the mould of preheating;
5.: glass put into be warming up to transition temperature (T
g) retort furnace in, be incubated after 2 hours, be annealed to about 150 ℃ with 15 ℃/hour speed, and then after being annealed to 80 ℃ with 20 ℃/hour speed, close retort furnace, be cooled to room temperature and get final product.
4, method for glass preparation according to claim 3 is characterized in that described crucible is corundum or platinum crucible, and electric furnace is a silicon carbon rod electric furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410093208 CN1269756C (en) | 2004-12-17 | 2004-12-17 | Erbium-doped lead-free germanium bismuth glass and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410093208 CN1269756C (en) | 2004-12-17 | 2004-12-17 | Erbium-doped lead-free germanium bismuth glass and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1644543A true CN1644543A (en) | 2005-07-27 |
| CN1269756C CN1269756C (en) | 2006-08-16 |
Family
ID=34869380
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410093208 Expired - Fee Related CN1269756C (en) | 2004-12-17 | 2004-12-17 | Erbium-doped lead-free germanium bismuth glass and preparation method thereof |
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| Country | Link |
|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674690A (en) * | 2012-05-31 | 2012-09-19 | 中国科学院上海光学精密机械研究所 | 3 mu m rare earth ion doped bismuth-germinate laser glass and preparation method thereof |
| CN109467315A (en) * | 2018-10-23 | 2019-03-15 | 温州大学新材料与产业技术研究院 | A kind of sodium base glass and preparation method thereof adulterating InN |
-
2004
- 2004-12-17 CN CN 200410093208 patent/CN1269756C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674690A (en) * | 2012-05-31 | 2012-09-19 | 中国科学院上海光学精密机械研究所 | 3 mu m rare earth ion doped bismuth-germinate laser glass and preparation method thereof |
| CN109467315A (en) * | 2018-10-23 | 2019-03-15 | 温州大学新材料与产业技术研究院 | A kind of sodium base glass and preparation method thereof adulterating InN |
| CN109467315B (en) * | 2018-10-23 | 2022-04-05 | 温州大学新材料与产业技术研究院 | InN-doped sodium-based glass and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1269756C (en) | 2006-08-16 |
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