CN107010830A - A kind of infrared sulphur system magnetic rotation glass and preparation method thereof - Google Patents
A kind of infrared sulphur system magnetic rotation glass and preparation method thereof Download PDFInfo
- Publication number
- CN107010830A CN107010830A CN201710224787.3A CN201710224787A CN107010830A CN 107010830 A CN107010830 A CN 107010830A CN 201710224787 A CN201710224787 A CN 201710224787A CN 107010830 A CN107010830 A CN 107010830A
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- magnetic rotation
- glass
- sulphur system
- rotation glass
- system magnetic
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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
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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
- C03C3/12—Silica-free oxide glass compositions
- C03C3/253—Silica-free oxide glass compositions containing germanium
Abstract
The invention belongs to photoelectric functional material field, and in particular to a kind of to work in sulphur system magnetic rotation glass of infrared band and preparation method thereof.The raw material of the glass is constituted and molal weight fraction is:13.5 58.5% GeS2, 31.5 76.5% Sb2S3With 10% PbI2.Magnetic rotation glass provided by the present invention, its Field constant is temperature independent, therefore the device prepared with it is without temperature compensation system so that device architecture is simple, and stability is more preferable.The magnetic rotation glass of the present invention has outstanding infrared transmission ability, in can be widely applied in infrared and far infrared band magnetic-optic devices.Magnetic rotation glass provided by the present invention is up to 0.211minG in infrared band Field constant‑1·cm‑1@980nm, are significantly higher than existing diamagnetism magneto-optic glass, are that the practical of antimagnetic glass is laid a good foundation.
Description
Technical field
The invention belongs to photoelectric functional material field, and in particular to a kind of sulphur system magnetic rotation glass for working in infrared band
And preparation method thereof.
Background technology
The principle that magneto-optic memory technique is utilized is magnetic rotation luminous effect, also known as Faraday effect:I.e. linearly polarized light is propagated in media as well
When, if adding an additional field on the direction of propagation parallel to light, the direction of the vibration plane of light will deflect, the rotation of plane of polarization
Turn direction and depend on magnetic direction, and it is unrelated with the direction of propagation of light.The characterization parameter of magneto-optic glass is Field constant, generally
In the case of, it is intended that material has high Field constant, so can be that institute can be achieved with small sample or low magnetic field
The anglec of rotation needed.
Magneto-optic glass has weight in terms of magneto optic isolator, magneto-optic shutter, magneto-optic modulator and fibre optic current sensor
Apply.The magneto optic isolator such as made of magneto-optic glass can eliminate the reflected light being harmful in optical system, be widely used in
In the laser systems such as multi-stage laser amplifier, optical parametric oscillator;Magneto-optic shutter based on magneto-optic glass, can be by controlling magnetic field
To realize the switching of light path, relative to other photoswitches, magneto-optic shutter speed is fast, consumes energy small, stability is good, and can be fabricated to
Block, film-form and optical-fiber type three types, it is convenient integrated in various equipment.
Magneto-optic glass is divided into paramagnetism glass and diamagnetism glass.Conventional magneto-optic glass is mainly rare earth ion and mixed at present
Miscellaneous paramagnetism glass.The glass is applied in large laser system, but the shortcoming of the material is:Field constant is by temperature
Degree change influence is larger, and IR-cut side is in 1.5 microns, it is impossible to applied to middle-infrared band.It is different from paramagnetic glass
It is that the Field constant of antimagnetic glass is hardly affected by temperature, therefore the device prepared with it is without temperature compensation mechanism, knot
Structure is simple, small volume.Be based especially on the diamagnetism magneto-optic memory technique of chalcogenide glass, its through wave band up to far infrared band,
There is irreplaceable advantage in infrared magnetic-optic devices.The presence problem of antimagnetic glass is that Field constant is smaller, generally than suitable
Small 1~2 order of magnitude of magnetic glass, limits the application of antimagnetic glass.Therefore, how to improve the Field constant of antimagnetic glass is
Current research emphasis, due to being limited by glass ingredient, the progress of antimagnetic glass is slow, seriously limits inverse magnetic glass
The application of glass.
Inverse magneto-optic glass disclosed in CN106477882A, its Field constant reaches 0.189minG in 980 nano wavebands-1·cm-1, it is about 20 times of quartz material, but how further to improve the weight that the Field constant of antimagnetic glass is still research
Point.
The content of the invention
In order to solve the technical problem that existing antimagnetic glass Field constant is relatively low, the present invention provides a kind of new sulfur system
Magnetic rotation glass and preparation method thereof.
The present invention technical solution be:A kind of infrared sulphur system magnetic rotation glass, it is characterized in that:Raw material is constituted
And molal weight fraction is:13.5-58.5% GeS2, 31.5-76.5% Sb2S3With 10% PbI2。
Further, raw material composition and molal weight fraction are:13.5-22.5% GeS2, 67.5-76.5% Sb2S3
With 10% PbI2。
Further, raw material composition and molal weight fraction are:13.5% GeS2, 76.5% Sb2S3With 10%
PbI2。
The present invention also provides a kind of preparation method of diamagnetism sulphur system magnetic rotation glass, and it is characterized in that:Including with
Lower step:
1】Raw material is weighed according to following molal weight fraction proportion speed:13.5-58.5% GeS2, 31.5-76.5%
Sb2S3With 10% PbI2;
2】Raw material is positioned in quartz ampoule, sealed after vacuumizing;
3】Quartz ampoule after sealing is founded 12-24 hours at a temperature of 900-1000 DEG C;
4】880 DEG C are cooled to after the completion of founding, then quartz ampoule is placed in the water of room temperature and is transferred to annealing furnace after quenching
It is middle to be made annealing treatment;
5】After the completion of annealing, quartz ampoule is broken or diamagnetism sulphur system magnetic rotation glass is in control with hydrofluoric acid etch quartz
Glass.
Further, step 1】In material quality fraction proportioning be:13.5-22.5% GeS2, 67.5-76.5%
Sb2S3With 10% PbI2。
Further, step 1】In material quality fraction proportioning be:13.5% GeS2, 76.5% Sb2S3With 10%
PbI2。
Further, step 3】In glass melting temperature be 980 DEG C, melting time be 18 hours.
Further, step 3】In quartz ampoule be to be founded in rocking furnace.
Further, step 4】In be that the quartz ampoule after quenching is transferred in the annealing furnace for having risen to annealing temperature, protect
Temperature 2 hours, was then down to room temperature with 12 hours.
The advantage of the invention is that:
1st, magnetic rotation glass provided by the present invention is up to 0.211minG in infrared band Field constant-1·cm-1@
980nm, being significantly higher than existing diamagnetism magneto-optic glass, (such as magneto-optic glasses of Xiao Te SF 59, Field constant is 0.028min
G-1·cm-1@1060nm;The Fei Er of 60GeS215In2S325PbI2 diamagnetisms magneto-optic glass disclosed in CN106477882A
Moral constant is 0.189minG-1cm-1@980nm), it is that the practical of antimagnetic glass is laid a good foundation.
2nd, magnetic rotation glass provided by the present invention, its Field constant is temperature independent, therefore the device prepared with it
Without temperature compensation system so that device architecture is simple, and stability is more preferable.
3rd, magnetic rotation glass of the invention has outstanding infrared transmission ability, infrared in can be widely applied to and far infrared
In the magnetic-optic devices of wave band.
Brief description of the drawings
Fig. 1 is the transmission spectrogram of magnetic rotation glass of the present invention.
Embodiment
The present invention provides a kind of infrared sulphur system magnetic rotation glass, and its component is 13.5-58.5% in mole percent
GeS2, 31.5-76.5% Sb2S3With 10% PbI2.According to formula accurate weighing raw material, raw material is placed in quartz ampoule
And vacuumize, seal.Quartz ampoule is put into rocking furnace afterwards and founded, 900~1000 DEG C of glass melting temperature, the time 12~24 is small
When.Be cooled to after the completion of founding 880 DEG C come out of the stove, quenching, and be quickly transferred to have risen in the annealing furnace of annealing temperature and anneal.This
The diamagnetism chalcogenide glass component of invention has outstanding infrared transmission ability, high Field constant.Relative to containing rare earth from
For the paramagnetism glass of son, the Field constant of the material has small temperature coefficient, so that negligible temperature is to system
Influence.
Referring to Fig. 1, magnetic rotation glass H103 resin of the invention can covering visible light, near-infrared, in it is infrared and remote red
Outer four wave bands, in being particularly suitable for use in infrared and far infrared band magnetic-optic devices.
Technical scheme is described in detail with reference to specific embodiment.
Each embodiment of diamagnetism sulphur system magnetic rotation glass of the present invention concrete component in mole percent and corresponding
Field constant V (minG-1·cm-1) as follows:
Embodiment 1:
1) formula composition is 58.5%GeS2, 31.5%Sb2S3, 10%PbI2.Accurate weighing raw material, is placed in quartz ampoule,
Vacuumized, sealed with oxyhydrogen flame with vavuum pump.
2) quartz ampoule is put into rocking furnace and founded, 1000 DEG C of glass melting temperature, 18 hours time.
3) be cooled to after melting 880 DEG C come out of the stove, quenching, and be quickly transferred to have risen to and moved back in the annealing furnace of annealing temperature
Fire.
Embodiment 2:
1) formula composition is 49.5%GeS2, 40.5%Sb2S3, 10%PbI2.Accurate weighing raw material, is placed in quartz ampoule,
Vacuumized, sealed with oxyhydrogen flame with vavuum pump.
2) quartz ampoule is put into rocking furnace and founded, 1000 DEG C of glass melting temperature, 12 hours time.
3) be cooled to after melting 880 DEG C come out of the stove, quenching, and be quickly transferred to have risen to and moved back in the annealing furnace of annealing temperature
Fire.
Embodiment 3:
1) formula composition is 40.5%GeS2, 49.5%Sb2S3, 10%PbI2.Accurate weighing raw material, is placed in quartz ampoule,
Vacuumized, sealed with oxyhydrogen flame with vavuum pump.
2) quartz ampoule is put into rocking furnace and founded, 980 DEG C of glass melting temperature, 15 hours time.
3) be cooled to after melting 880 DEG C come out of the stove, quenching, and be quickly transferred to have risen to and moved back in the annealing furnace of annealing temperature
Fire.
Embodiment 4:
1) formula composition is 31.5%GeS2, 58.5%Sb2S3, 10%PbI2.Accurate weighing raw material, is placed in quartz ampoule,
Vacuumized, sealed with oxyhydrogen flame with vavuum pump.
2) quartz ampoule is put into rocking furnace and founded, 980 DEG C of glass melting temperature, 15 hours time.
3) be cooled to after melting 880 DEG C come out of the stove, quenching, and be quickly transferred to have risen to and moved back in the annealing furnace of annealing temperature
Fire.
Embodiment 5:
1) formula composition is 22.5%GeS2, 67.5%Sb2S3, 10%PbI2.Accurate weighing raw material, is placed in quartz ampoule,
Vacuumized, sealed with oxyhydrogen flame with vavuum pump.
2) quartz ampoule is put into rocking furnace and founded, 950 DEG C of glass melting temperature, 20 hours time.
3) be cooled to after melting 880 DEG C come out of the stove, quenching, and be quickly transferred to have risen to and moved back in the annealing furnace of annealing temperature
Fire.
Embodiment 6:
1) formula composition is 13.5%GeS2, 76.5%Sb2S3, 10%PbI2.Accurate weighing raw material, is placed in quartz ampoule,
Vacuumized, sealed with oxyhydrogen flame with vavuum pump.
2) quartz ampoule is put into rocking furnace and founded, 900 DEG C of glass melting temperature, 24 hours time.
3) be cooled to after melting 880 DEG C come out of the stove, quenching, and be quickly transferred to have risen to and moved back in the annealing furnace of annealing temperature
Fire.
Above example is only to technical solution of the present invention for example, being not construed as protecting the claims in the present invention
The limitation of scope, those skilled in the art beyond all doubt from the basic scheme of the present invention be able to should be inferred to, according to this hair
Bright technical scheme can realize the purpose of the present invention.
Claims (9)
1. a kind of infrared sulphur system magnetic rotation glass, it is characterised in that:Raw material is constituted and molal weight fraction is:13.5-58.5%
GeS2, 31.5-76.5% Sb2S3With 10% PbI2。
2. a kind of infrared sulphur system magnetic rotation glass according to claim 1, it is characterised in that:Raw material is constituted and molal weight
Fraction is:13.5-22.5% GeS2, 67.5-76.5% Sb2S3With 10% PbI2。
3. a kind of infrared sulphur system magnetic rotation glass according to claim 2, it is characterised in that:Raw material is constituted and molal weight
Fraction is:13.5% GeS2, 76.5% Sb2S3With 10% PbI2。
4. a kind of preparation method of infrared sulphur system magnetic rotation glass, it is characterised in that:Comprise the following steps:
1】Raw material is weighed according to following molal weight fraction proportion speed:13.5-58.5% GeS2, 31.5-76.5%
Sb2S3With 10% PbI2;
2】By the step 1】Each raw material weighed is positioned in quartz ampoule, is sealed after vacuumizing;
3】By the step 2】Quartz ampoule after sealing is founded 12-24 hours at a temperature of 900-1000 DEG C;
4】By the step 3】Quartz ampoule after the completion of founding is cooled to 880 DEG C, quartz ampoule is placed in the water of room temperature after quenching
It is transferred in annealing furnace and is made annealing treatment;
5】By the step 4】Quartz ampoule after the completion of annealing breaks or is in control with hydrofluoric acid etch quartz diamagnetism sulphur system
Magnetic rotation glass.
5. a kind of preparation method of infrared sulphur system magnetic rotation glass according to claim 4, it is characterised in that:Step 1】In
Material quality fraction proportioning be:13.5-22.5% GeS2, 67.5-76.5% Sb2S3With 10% PbI2。
6. a kind of preparation method of infrared sulphur system magnetic rotation glass according to claim 5, it is characterised in that:Step 1】In
Material quality fraction proportioning be:13.5% GeS2, 76.5% Sb2S3With 10% PbI2。
7. according to a kind of preparation method of any described infrared sulphur system magnetic rotation glass in claim 4-6, it is characterised in that:
Step 3】In glass melting temperature be 980 DEG C, melting time be 18 hours.
8. a kind of preparation method of infrared sulphur system magnetic rotation glass according to claim 7, it is characterised in that:Step 3】In
Quartz ampoule be to be founded in rocking furnace.
9. a kind of preparation method of infrared sulphur system magnetic rotation glass according to claim 8, it is characterised in that:Step 4】In
It is that the quartz ampoule after quenching is transferred in the annealing furnace for having risen to annealing temperature, is incubated 2 hours, was then down to room with 12 hours
Temperature.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109320092A (en) * | 2018-10-24 | 2019-02-12 | 宁波大学 | A kind of compound chalcogenide glass ceramic material of lead halide crystallite and preparation method thereof |
CN111253058A (en) * | 2020-01-22 | 2020-06-09 | 中国科学院西安光学精密机械研究所 | Device and method for preparing anhydrous infrared glass optical fiber preform |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103864297A (en) * | 2014-03-26 | 2014-06-18 | 南京信息工程大学 | Intermediate infrared optical glass for fine molding and molding |
CN106477882A (en) * | 2016-09-27 | 2017-03-08 | 中国科学院西安光学精密机械研究所 | A kind of diamagnetism sulfur system magnetic rotation glass and preparation method thereof |
-
2017
- 2017-04-07 CN CN201710224787.3A patent/CN107010830B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103864297A (en) * | 2014-03-26 | 2014-06-18 | 南京信息工程大学 | Intermediate infrared optical glass for fine molding and molding |
CN106477882A (en) * | 2016-09-27 | 2017-03-08 | 中国科学院西安光学精密机械研究所 | A kind of diamagnetism sulfur system magnetic rotation glass and preparation method thereof |
Non-Patent Citations (1)
Title |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109320092A (en) * | 2018-10-24 | 2019-02-12 | 宁波大学 | A kind of compound chalcogenide glass ceramic material of lead halide crystallite and preparation method thereof |
CN111253058A (en) * | 2020-01-22 | 2020-06-09 | 中国科学院西安光学精密机械研究所 | Device and method for preparing anhydrous infrared glass optical fiber preform |
CN111253058B (en) * | 2020-01-22 | 2021-09-14 | 中国科学院西安光学精密机械研究所 | Device and method for preparing anhydrous infrared glass optical fiber preform |
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