CN106957146A - A kind of photosensitive glass material and preparation method - Google Patents
A kind of photosensitive glass material and preparation method Download PDFInfo
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- CN106957146A CN106957146A CN201710177892.6A CN201710177892A CN106957146A CN 106957146 A CN106957146 A CN 106957146A CN 201710177892 A CN201710177892 A CN 201710177892A CN 106957146 A CN106957146 A CN 106957146A
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- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
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- 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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- 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
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- Life Sciences & Earth Sciences (AREA)
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- Manufacturing & Machinery (AREA)
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Abstract
The invention belongs to technical field of glass materials there is provided a kind of photosensitive glass material and preparation method, the photosensitive glass material includes the component of following parts by weight：BaO is 29 parts, MoO3For 9 22 parts, SiO2For 15 23 parts, LaMnO3For 5 13 parts, Yb2O3For 7 14 parts, La2O3For 8 16 parts, Nb2O5For 5 18 parts.Glass prepared by the present invention, contains oxide LaMnO3, and rare earth ion doped heavy metal oxide glass is one of photonic device host material；The present invention is advantageously implemented the integrated of photonic device, and photonic device it is integrated be current photonic device development important trend.
Description
Technical field
The invention belongs to technical field of glass materials, in particular it relates to a kind of photosensitive glass material and preparation method.
Background technology
Photosensitive glass is that photosensitizing chemical reagent is introduced into vitreum, is allowed to a kind of novel glass of exposure heating.It is this
The structure of glass has the porous of height：Micropore of the total volume 30%, the diameter of each micropore only has 20 nanometers, about holds
Receive 4000 atoms.Chemical reagent almost all used by metal carbonyl class compound group into.After reagent exposure, one can be removed
Individual or multiple CO molecules, leave its half-naked metallic atom.Metallic atom " does not like " individualism, and looks round for some things
Matter, with the carbonyl for replacing it to lose.Metallic atom can be obtained being exactly the glass around it, so metallic atom and glass knot
It is combined.
When glass is heated to 200 DEG C, retained by the chemical reagent of light irradiation, and unexposed reagent then by except
Go, the photographic image common equivalent to " fixation ".The image is not obscured, because the aperture of micropore only has the several of visible wavelength
/ several, so micropore does not cause light scattering.When glass is heated to about 1200 DEG C, micropore disappears, and dense glass is formed, in glass
Lower permanent image is just retained in glass.By means of there is the glass of image, it can be used to produce image to other materials, in other words, it can
Mask as photoetching, thus cause the great interest of semiconductor chip manufacturer.
The Another Application field of photosensitive glass is in terms of the diffraction grating of optical system.Grating is the heart of optical instrument
Dirty, normal light can be resolved into monochromatic light by it.Its traditional preparation method is that the narrow each lines of separation are carved into the surface of a sheet glass.
Nowadays the lines of image are produced on this photosensitive glass surface to be played the same role, and preparation is easier to.In glass
In glass processing procedure, such as with other photosensitive reagents, the glass being made can be also set to produce different effects.Using this characteristic,
The lens array of complexity can be made, most strikingly in terms of optical communication.Because utilizing glass refraction in device
Controllable variations, can eliminate optical signal and pass through the distortion in fibre-optic cable.
Although passing through hydrogen bearing（H2-loading）, brush fire（Flame-brushing）Etc. post-processing technology, optical fiber can be made
Photorefraotive crystal reaches the 10-3 orders of magnitude.But long later stage treatment time, not only elapsed time, can also bring fused fiber splice
When danger.In addition, online write-in grating can not be realized using post-processing technique, thus the fast fast-growing of high-volume can not be met
Produce the requirement of grating.These problems are solved, it is necessary to starting with itself-improving for the light for making fiber grating material from material
Quick property.Abroad, by increasing germanium in silica fibre（Ge）Incorporation or pass through boron germanium（B/Ge）It is co-doped with improving optical fiber
Light sensitivity, but the highly doped germanium and B-Ge-codoped UV Photosensitivity in Optical Fiber developed are not enough（The generally 10-4 orders of magnitude）And axial light sensitivity
It is uneven, limit its application.Then, people explore and rare earth ion are mixed in quartz glass again, such as：Ta3+、Ce3+、Er3+、
Eu2+、Tb3+Deng.Although these rare earth elements can improve the light sensitivity of glass to a certain extent, it can not equally meet
The requirement of line no write de-lay high light grid.In recent years, in the world some optic communication research units it is numerous and confused research emphasis is turned to it is multigroup
Divide glass.
Oxide glass with excellent high stability turns into after quartz glass by the multicomponent of broad scale research
Glass.Such as, Sn is added in Ge-Si, P-Si glass and improves the light sensitivity of glass, by mix Sn glass-pullings into optical fiber, its
The variable quantity of photon-induced refractive index is maximum up to 10-3, and SnO remains relatively low absorption in third communication window, under its high temperature
Stability it is more much better than B/Ge optical fiber.In addition, the High-tech Material research center of University of New Mexico of the U.S. and Britain
Discovery is studied recently in Southampton universities photoelectron research center：Lead-silica glass is after 266nm ultraviolet light, and it is rolled over
The maximum of rate change is penetrated up to 0.1, and they study discovery：With the increase of PbO contents, the light sensitivity of glass increases.
And quartz glass only has the addition from Pb of light sensitivity in very weak light sensitivity, therefore silicon lead glass.In the periodic table of elements
Middle Pb is the element of the 4th main group, and atomic number is 82, and peripheral electron arrangement is 6s2 6p2, therefore it can lose 2 electronics
Or 4 electronics and form stable compound.Pb can change the characteristic of valence state so that flint glass has light sensitivity.In purple
Under the irradiation of outer light, transition-metal ions pb2+Valence state produce change, form point defect in glass.Point in glass network structure
Defect absorbs UV photon energy, defect sturcture is changed.So as to cause the change of glass absorption coefficient, finally cause glass
The change of glass refractive index.
The content of the invention
For defect of the prior art, it is an object of the invention to provide a kind of photosensitive glass material, it is intended to solves common
Glass material because its photosensitive property is poor, thermal coefficient of expansion it is too high so as to not light sensitivity environment, by thermally labile the problem of.
It is another object of the present invention to provide the preparation method of the photosensitive glass material.
A kind of photosensitive glass material is provided according to an aspect of the present invention, and the photosensitive glass material includes following weight
The component of number：BaO is 2-9 parts, MoO3For 9-22 parts, SiO2For 15-23 parts, LaMnO3For 5-13 parts, Yb2O3For 7-14 parts,
La2O3For 8-16 parts, Nb2O5For 5-18 parts.
Preferably, BaO is 3-8 parts, MoO3For 11-21 parts, SiO2For 16-21 parts, LaMnO3For 7-12 parts, Yb2O3For 8-
13 parts, La2O3For 9-15 parts, Nb2O5For 7-15 parts.
Preferably, BaO is 5 parts, MoO3For 16 parts, SiO2For 17 parts, LaMnO3For 9 parts, Yb2O3For 11 parts, La2O3For 12
Part, Nb2O5For 14 parts.
There is provided described photosensitive glass material preparation method according to another aspect of the present invention, it is characterised in that：It is described
Method comprises the following steps：
（1）The glass ingredient weight ratio is taken to be：BaO is 2-9 parts, MoO3For 9-22 parts, SiO2For 15-23 parts, LaMnO3For 5-13
Part, Yb2O3For 7-14 parts, La2O3For 8-16 parts, Nb2O5For 5-18 parts, the corresponding raw material of above-mentioned oxide is mixed；
（2）Frit after mixing is crushed using micronizer, the powder passed through is filtered out after crushing with sieve；
（3）It will be added in corundum crucible, corundum crucible heated, temperature reaches that keeping temperature is not after highest by the powder of sieve
Become, while being stirred to glass metal；
（4）Stirring is ventilated after terminating and clarified；
（5）Glass precursor solution is poured into mould after clarification；
（6）Glass is annealed after cast, then cooled, room temperature is finally cooled to, photosensitive glass material is prepared into.
Preferably, the powder passed through is filtered out after the crushing with 300-350 mesh sieve.
Preferably, it is described that corundum crucible is heated to 1310-1400 DEG C.
Preferably, the temperature reaches the constant 2-5h of keeping temperature after highest.
Compared with prior art, the present invention has following beneficial effect：
（1）Glass prepared by the present invention, contains oxide LaMnO3, and rare earth ion doped heavy metal oxide glass is
One of photonic device host material；
（2）The present invention is advantageously implemented the integrated of photonic device, and the integrated of photonic device is current photonic device development
Important trend.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.
Embodiment 1
The present embodiment provides a kind of photosensitive glass material, and the photosensitive glass material includes the component of following parts by weight：BaO is
9 parts, MoO3For 9 parts, SiO2For 23 parts, LaMnO3For 5 parts, Yb2O3For 14 parts, La2O3For 8 parts, Nb2O5For 18 parts.
There is provided described photosensitive glass material preparation method according to another aspect of the present invention, it is characterised in that：It is described
Method comprises the following steps：
（1）The glass ingredient weight ratio is taken to be：BaO is 9 parts, MoO3For 9 parts, SiO2For 23 parts, LaMnO3For 5 parts, Yb2O3For 14
Part, La2O3For 8 parts, Nb2O5For 18 parts, the corresponding raw material of above-mentioned oxide is mixed；
（2）Frit after mixing is crushed using micronizer, the powder passed through is filtered out after crushing with sieve；
（3）It will be added in corundum crucible, corundum crucible heated, temperature reaches that keeping temperature is not after highest by the powder of sieve
Become, while being stirred to glass metal；
（4）Stirring is ventilated after terminating and clarified；
（5）Glass precursor solution is poured into mould after clarification；
（6）Glass is annealed after cast, then cooled, room temperature is finally cooled to, photosensitive glass material is prepared into.
The powder passed through is filtered out after the crushing with 350 mesh sieve.
It is described that corundum crucible is heated to 1310 DEG C.
The temperature reaches the constant 5h of keeping temperature after highest.
Embodiment 2
The present embodiment provides a kind of photosensitive glass material, and the photosensitive glass material includes the component of following parts by weight：BaO is
2 parts, MoO3For 22 parts, SiO2For 15 parts, LaMnO3For 13 parts, Yb2O3For 7 parts, La2O3For 16 parts, Nb2O5For 5 parts.
There is provided described photosensitive glass material preparation method according to another aspect of the present invention, it is characterised in that：It is described
Method comprises the following steps：
（1）The glass ingredient weight ratio is taken to be：BaO is 2 parts, MoO3For 22 parts, SiO2For 15 parts, LaMnO3For 13 parts, Yb2O3For 7
Part, La2O3For 16 parts, Nb2O5For 5 parts, the corresponding raw material of above-mentioned oxide is mixed；
（2）Frit after mixing is crushed using micronizer, the powder passed through is filtered out after crushing with sieve；
（3）It will be added in corundum crucible, corundum crucible heated, temperature reaches that keeping temperature is not after highest by the powder of sieve
Become, while being stirred to glass metal；
（4）Stirring is ventilated after terminating and clarified；
（5）Glass precursor solution is poured into mould after clarification；
（6）Glass is annealed after cast, then cooled, room temperature is finally cooled to, photosensitive glass material is prepared into.
The powder passed through is filtered out after the crushing with 300 mesh sieve.
It is described that corundum crucible is heated to 1400 DEG C.
The temperature reaches the constant 2h of keeping temperature after highest.
Embodiment 3
The present embodiment provides a kind of photosensitive glass material, and the photosensitive glass material includes the component of following parts by weight：BaO is
8 parts, MoO3For 11 parts, SiO2For 21 parts, LaMnO3For 7 parts, Yb2O3For 13 parts, La2O3For 9 parts, Nb2O5For 15 parts.
There is provided described photosensitive glass material preparation method according to another aspect of the present invention, it is characterised in that：It is described
Method comprises the following steps：
（1）The glass ingredient weight ratio is taken to be：BaO is 8 parts, MoO3For 11 parts, SiO2For 21 parts, LaMnO3For 7 parts, Yb2O3For 13
Part, La2O3For 9 parts, Nb2O5For 15 parts, the corresponding raw material of above-mentioned oxide is mixed；
（2）Frit after mixing is crushed using micronizer, the powder passed through is filtered out after crushing with sieve；
（3）It will be added in corundum crucible, corundum crucible heated, temperature reaches that keeping temperature is not after highest by the powder of sieve
Become, while being stirred to glass metal；
（4）Stirring is ventilated after terminating and clarified；
（5）Glass precursor solution is poured into mould after clarification；
（6）Glass is annealed after cast, then cooled, room temperature is finally cooled to, photosensitive glass material is prepared into.
The powder passed through is filtered out after the crushing with 320 mesh sieve.
It is described that corundum crucible is heated to 1350 DEG C.
The temperature reaches the constant 3h of keeping temperature after highest.
Embodiment 4
The present embodiment provides a kind of photosensitive glass material, and the photosensitive glass material includes the component of following parts by weight：BaO is
3 parts, MoO3For 21 parts, SiO2For 16 parts, LaMnO3For 12 parts, Yb2O3For 8 parts, La2O3For 15 parts, Nb2O5For 7 parts.
There is provided described photosensitive glass material preparation method according to another aspect of the present invention, it is characterised in that：It is described
Method comprises the following steps：
（1）The glass ingredient weight ratio is taken to be：BaO is 3 parts, MoO3For 21 parts, SiO2For 16 parts, LaMnO3For 12 parts, Yb2O3For 8
Part, La2O3For 15 parts, Nb2O5For 7 parts, the corresponding raw material of above-mentioned oxide is mixed；
（2）Frit after mixing is crushed using micronizer, the powder passed through is filtered out after crushing with sieve；
（3）It will be added in corundum crucible, corundum crucible heated, temperature reaches that keeping temperature is not after highest by the powder of sieve
Become, while being stirred to glass metal；
（4）Stirring is ventilated after terminating and clarified；
（5）Glass precursor solution is poured into mould after clarification；
（6）Glass is annealed after cast, then cooled, room temperature is finally cooled to, photosensitive glass material is prepared into.
The powder passed through is filtered out after the crushing with 330 mesh sieve.
It is described that corundum crucible is heated to 1380 DEG C.
The temperature reaches the constant 4h of keeping temperature after highest.
Embodiment 5
The present embodiment provides a kind of photosensitive glass material, and the photosensitive glass material includes the component of following parts by weight：BaO is
5 parts, MoO3For 16 parts, SiO2For 17 parts, LaMnO3For 9 parts, Yb2O3For 11 parts, La2O3For 12 parts, Nb2O5For 14 parts.
There is provided described photosensitive glass material preparation method according to another aspect of the present invention, it is characterised in that：It is described
Method comprises the following steps：
（1）The glass ingredient weight ratio is taken to be：BaO is 5 parts, MoO3For 16 parts, SiO2For 17 parts, LaMnO3For 9 parts, Yb2O3For 11
Part, La2O3For 12 parts, Nb2O5For 14 parts, the corresponding raw material of above-mentioned oxide is mixed；
（2）Frit after mixing is crushed using micronizer, the powder passed through is filtered out after crushing with sieve；
（3）It will be added in corundum crucible, corundum crucible heated, temperature reaches that keeping temperature is not after highest by the powder of sieve
Become, while being stirred to glass metal；
（4）Stirring is ventilated after terminating and clarified；
（5）Glass precursor solution is poured into mould after clarification；
（6）Glass is annealed after cast, then cooled, room temperature is finally cooled to, photosensitive glass material is prepared into.
The powder passed through is filtered out after the crushing with 310 mesh sieve.
It is described that corundum crucible is heated to 1340 DEG C.
The temperature reaches the constant 2h of keeping temperature after highest.
Embodiment 6
The present embodiment provides a kind of photosensitive glass material, and the photosensitive glass material includes the component of following parts by weight：BaO is
3 parts, MoO3For 15 parts, SiO2For 19 parts, LaMnO3For 12 parts, Yb2O3For 13 parts, La2O3For 14 parts, Nb2O5For 11 parts.
There is provided described photosensitive glass material preparation method according to another aspect of the present invention, it is characterised in that：It is described
Method comprises the following steps：
（1）The glass ingredient weight ratio is taken to be：BaO is 3 parts, MoO3For 15 parts, SiO2For 19 parts, LaMnO3For 12 parts, Yb2O3For
13 parts, La2O3For 14 parts, Nb2O5For 11 parts, the corresponding raw material of above-mentioned oxide is mixed；
（2）Frit after mixing is crushed using micronizer, the powder passed through is filtered out after crushing with sieve；
（3）It will be added in corundum crucible, corundum crucible heated, temperature reaches that keeping temperature is not after highest by the powder of sieve
Become, while being stirred to glass metal；
（4）Stirring is ventilated after terminating and clarified；
（5）Glass precursor solution is poured into mould after clarification；
（6）Glass is annealed after cast, then cooled, room temperature is finally cooled to, photosensitive glass material is prepared into.
The powder passed through is filtered out after the crushing with 340 mesh sieve.
It is described that corundum crucible is heated to 1350 DEG C.
The temperature reaches the constant 5h of keeping temperature after highest.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substance of the present invention.
Claims (8)
1. a kind of photosensitive glass material, it is characterised in that：The photosensitive glass material includes the component of following parts by weight：BaO
For 2-9 parts, MoO3For 9-22 parts, SiO2For 15-23 parts, LaMnO3For 5-13 parts, Yb2O3For 7-14 parts, La2O3For 8-16 parts,
Nb2O5For 5-18 parts.
2. photosensitive glass material according to claim 1, it is characterised in that：The photosensitive glass material includes following weight
The component of number：BaO is 3-8 parts, MoO3For 11-21 parts, SiO2For 16-21 parts, LaMnO3For 7-12 parts, Yb2O3For 8-13 parts,
La2O3For 9-15 parts, Nb2O5For 7-15 parts.
3. photosensitive glass material according to claim 1, it is characterised in that：The photosensitive glass material includes following weight
The component of number：BaO is 5 parts, MoO3For 16 parts, SiO2For 17 parts, LaMnO3For 9 parts, Yb2O3For 11 parts, La2O3For 12 parts,
Nb2O5For 14 parts.
4. realize the preparation method of the photosensitive glass material as described in claim 1-3, it is characterised in that：Comprise the following steps：
（1）The glass ingredient weight ratio is taken to be：BaO is 2-9 parts, MoO3For 9-22 parts, SiO2For 15-23 parts, LaMnO3For 5-13
Part, Yb2O3For 7-14 parts, La2O3For 8-16 parts, Nb2O5For 5-18 parts, the corresponding raw material of above-mentioned oxide is mixed；
（2）Frit after mixing is crushed using micronizer, the powder passed through is filtered out after crushing with sieve；
（3）It will be added in corundum crucible, corundum crucible heated, temperature reaches that keeping temperature is not after highest by the powder of sieve
Become, while being stirred to glass metal；
（4）Stirring is ventilated after terminating and clarified；
（5）Glass precursor solution is poured into mould after clarification；
（6）Glass is annealed after cast, then cooled, room temperature is finally cooled to, photosensitive glass material is prepared into.
5. the preparation method of photosensitive glass material according to claim 4, it is characterised in that：300- is used after the crushing
350 mesh sieve filter out the powder passed through.
6. the preparation method of photosensitive glass material according to claim 4, it is characterised in that：It is described to heat corundum crucible
To 1310-1400 DEG C.
7. the preparation method of photosensitive glass material according to claim 4, it is characterised in that：The temperature is reached after highest
The constant 2-5h of keeping temperature.
8. the preparation method of photosensitive glass material according to claim 4, it is characterised in that：The first stage is first from most
Keep 2.6-3.5h when high annealing is to 800-850 DEG C, then be down to temperature for 300 DEG C when keep 1-2h.
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Cited By (1)
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58204839A (en) * | 1982-05-24 | 1983-11-29 | Toshiba Glass Co Ltd | Photosensitive glass |
| CN87102740A (en) * | 1987-04-16 | 1988-11-02 | 天津市硅酸盐研究所 | The manufacture method of color photosensitive glassware and device |
| US6228787B1 (en) * | 1998-07-27 | 2001-05-08 | Eugen Pavel | Fluorescent photosensitive glasses and process for the production thereof |
-
2017
- 2017-03-23 CN CN201710177892.6A patent/CN106957146B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58204839A (en) * | 1982-05-24 | 1983-11-29 | Toshiba Glass Co Ltd | Photosensitive glass |
| CN87102740A (en) * | 1987-04-16 | 1988-11-02 | 天津市硅酸盐研究所 | The manufacture method of color photosensitive glassware and device |
| US6228787B1 (en) * | 1998-07-27 | 2001-05-08 | Eugen Pavel | Fluorescent photosensitive glasses and process for the production thereof |
Cited By (1)
| 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 |
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| CN106957146B (en) | 2019-10-08 |
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| TR01 | Transfer of patent right |
Effective date of registration: 20200701 Address after: 233100 Fengyang County, Anhui Province, the town of Taiwan gate Patentee after: ANHUI QIANLI GLASSWORK Co.,Ltd. Address before: Workshop 3, Hefei Xinyuan metal products Co., Ltd., Yangjing Road, Taohua Town, Feixi County, Hefei City, Anhui Province, 230000 Patentee before: HEFEI XIEYAO GLASSWARE Co.,Ltd. |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A photosensitive glass material and its preparation method Effective date of registration: 20230911 Granted publication date: 20191008 Pledgee: Fengyang County Zhongdu Financing Guarantee Co.,Ltd. Pledgor: ANHUI QIANLI GLASSWORK Co.,Ltd. Registration number: Y2023980056166 |