CN106082677A - Mix ultraviolet cut-on height Aluminous Silicate Glass-Ceramics of cerium, titanium and preparation method thereof - Google Patents
Mix ultraviolet cut-on height Aluminous Silicate Glass-Ceramics of cerium, titanium and preparation method thereof Download PDFInfo
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- CN106082677A CN106082677A CN201610394546.9A CN201610394546A CN106082677A CN 106082677 A CN106082677 A CN 106082677A CN 201610394546 A CN201610394546 A CN 201610394546A CN 106082677 A CN106082677 A CN 106082677A
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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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- 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
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
-
- 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
- C03C2201/00—Glass compositions
- C03C2201/06—Doped silica-based glasses
- C03C2201/30—Doped silica-based glasses containing metals
- C03C2201/34—Doped silica-based glasses containing metals containing rare earth metals
- C03C2201/3423—Cerium
-
- 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
- C03C2201/00—Glass compositions
- C03C2201/06—Doped silica-based glasses
- C03C2201/30—Doped silica-based glasses containing metals
- C03C2201/40—Doped silica-based glasses containing metals containing transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn
- C03C2201/42—Doped silica-based glasses containing metals containing transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn containing titanium
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Ceramic Engineering (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Glass Compositions (AREA)
Abstract
A kind of ultraviolet cut-on height Aluminous Silicate Glass-Ceramics mixing cerium, titanium, this optical filtering pipe glass molar percentage compositing range is SiO2: 40～50mol%, Al2O3: 25～35mol%, MgO:5～10mol%, ZnO:0～5mol%；Li2O:0 5mol%, TiO2: 5～10mol%, ZrO2: 0～5mol%, CeO2: 3～8mol%.Made glass heat conductance is between 1.0 1.2W/MK, and thermal expansion is 50 60 × 10‑7Between/K.After prepared glass is by grinding, polishing, crystallite heat treatment, the tunable cut-off to xenon lamp spectrum 200 600nm scope can be realized, the present invention can reduce xenon lamp transition heat efficiency and reach more than 50%, reduce neodymium glass thermal distoftion more than 60% in the case of xenon flash lamp pumping, and then the repeated work frequency of raising neodymium glass laser, it is expected to be used in hectowatt repetition high-energy neodymium glass laser system from now on.
Description
Technical field
The invention belongs to inorganic non-metallic class optoelectronic information and field of functional materials, relate to one and be applicable to repetition high-energy
Neodymium glass laser system, and there is cut-off wave band in the range of scalable xenon lamp spectrum 200-600nm, mix the high aluminum silicate of cerium, titanium
Salt devitrified glass and preparation method thereof.
Background technology
Repetition high-energy neodymium glass laser suffers from being widely applied in laser impact intensified, Ti∶Sapphire laser pumping source field
Demand.But the thermomechanical property that neodymium glass is poor, on the one hand makes it cannot bear the highest heat accumulation, on the other hand can cause tight
The optical thermal distortion of weight.It is then desired to study suitable pump technology to the thermal accumlation reducing in neodymium glass, and then realize neodymium
The repetition work of amorphous laser.
At present, xenon lamp is most widely used pump light source in neodymium glass laser.Analyze xenon lamp emission spectrum and neodymium
The absorption spectrum of glass is learnt, the main output spectrum scope of xenon lamp is 400-1000nm, and the major absorbance peak of neodymium glass is
About 350nm, 530nm, 580nm, 750nm, 800nm and 870nm.Owing to the laser output wavelength of neodymium glass is 1053nm, no
With absorption band by different for the Excited state produced, and then the contribution to nd glass laser efficiency and heat accumulation efficiency is the most different.
At 350nm, the absorption band of 530nm, 580nm, the pump energy having more than 50% is converted into heat.
For meeting repetition high light beam quality laser demand, optional different filter glass material realizes xenon lamp spectrum
Regulation.It is applied to the filter in high power neodymium glass laser system at present and predominantly mixes the quartz ampoule of cerium, can only end
200-380nm ultraviolet light (CN 103466942 B, yellow ultraviolet-transmitquartz quartz glass plate and preparation method thereof；CN
104609729 A, navy blue filter ultraviolet quartz tube and preparation method thereof)；And other ultraviolet cut-on filter glasses are also only limitted to
200-400nm wave band (CN 87105349 A, fluorescent glass absorbing UV and IFR)；Repetition high light beam quality neodymium glass can not be met
The xenon lamp spectrum regulatory demand of glass laser instrument.In addition, xenon lamp can produce the energy of Kilojoule magnitude in 400-600nm scope
Amount, therefore filter glass not only has spectral modulation function, should also have sufficiently high thermal shock resistance.
Summary of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, it is provided that a kind of mix cerium, titanium high aluminosilicate micro-
Crystal glass and preparation method thereof, on the one hand realizes the tunable absorption in 200-600nm scope, on the other hand increases substantially glass
The surface strength of glass, final acquisition can meet the optical filtering microcrystal glass tube or micro-used in repetition high-energy neodymium glass laser system
Crystal glass sheet, it is achieved neodymium glass thermal distoftion under xenon flash lamp pumping is greatly lowered.
The purpose of the present invention, is achieved by the following technical solution:
A kind of ultraviolet cut-on height Aluminous Silicate Glass-Ceramics mixing cerium, titanium, is characterised by the molar percentage group of this glass
Become:
SiO2: 40～50mol%, Al2O3: 25～35mol%, MgO:5～10mol%, ZnO:0～5mol%；Li2O:
0-5mol%, TiO2: 5～10mol%, ZrO2: 0～5mol%, CeO2: 3～8mol%.
The preparation method of a kind of ultraviolet cut-on height Aluminous Silicate Glass-Ceramics mixing cerium, titanium, comprises the following steps:
1. calculate the percentage by weight of glass by the molar percentage of host glass composition, then weigh raw material, mixing
Uniformly, compound is formed；
2. described compound is put in crucible, be placed in the silicon molybdenum rod furnace of 1500～1600 DEG C and melt, molten
The change time is 2～8 hours；
3. annealing: glass pouring is put into warmed up to the Muffle furnace of glass transformation temperature after going out, after being incubated 3 hours, with 5～
The rate of temperature fall of 10 DEG C/h is down to 200 DEG C, then cools to room temperature with the furnace；
4. the host glass after annealing is warming up to 750～850 DEG C, is incubated 8～16 hours, then proceedes to be warming up to 900
～1050 DEG C, it is incubated 2～8 hours, it is thus achieved that nano crystalline glass.
This devitrified glass has the tunable cut-off to xenon lamp spectrum 200-600nm scope, it is adaptable to repetition high-energy neodymium
Optical filtering components and parts in glass laser system.
The technique effect of the present invention:
The present invention is by adding substantial amounts of cerium oxide and titanium oxide, by the uv absorption of glass in high alumina silicate glass
Wave band extends to 500nm；By titanium oxide with zirconic be simultaneously introduced, increase the overall crystallization property of glass, on the one hand will
The uv absorption wave band of devitrified glass extends to 600nm, is on the other hand obviously improved the thermal shock resistance of glass.
The present invention prepare for having the devitrified glass filter that xenon lamp spectrum is carried out ultraviolet cut-on, it is right to realize
The tunable cut-off of xenon lamp spectrum 400-600nm scope；
The present invention is prepared glass and can be processed by ion exchange, controlled micro crystallization, increases substantially the thermal shock resistance of glass,
Significantly extend the service life of devitrified glass filtering device and use operating frequency.
Accompanying drawing explanation
Fig. 1 is the H103 resin after this system embodiment 1 glass and controlled micro crystallization process at visible-range；
Fig. 2 is the optical filtering pipe made of embodiment 1 glass and commonly mix cerium quartz ampoule at repetition high-energy neodymium glass laser
In the impact of the thermal efficiency is contrasted.
Specific implementation method
Embodiment 1
A kind of devitrified glass filter that xenon lamp spectrum carries out ultraviolet cut-on, this glass has xenon lamp spectrum 400-
The tunable cut-off of 600nm scope.
One. preparation technology:
The first step: formula is (by mole meter):
Second step:
By the first step given formula dispensing, raw material is sufficiently mixed uniformly；,
3rd step: at 1500 DEG C, divides compound 4～6 times and joins quartz crucible/corundum crucible, platinum earthenware
In crucible, found 4 hours with fusion method；
4th step: at 1550 DEG C, vitreous humour is clarified 6 hours；
6th step: carry out mechanical agitation 9 hours；
7th step: prepared vitreous humour is poured in graphite or cast iron die sizing；
8th step: after being incubated 4 hours at 750 DEG C in Muffle furnace, carry out conventional annealing process；
9th step: to obtain glass cut, fine grinding, after polishing, carry out soda acid combination process 3.5 hours；
Tenth step: at 800 DEG C, glass sample is incubated 24 hours, is warmed up to 950 DEG C and is incubated 10 hours.
Embodiment 2
Testing and apply same as Example 1, simply preparation technology is different, as follows:
Preparation technology:
The first step: formula is (by mole meter):
Second step:
By the first step given formula dispensing, raw material is sufficiently mixed uniformly；,
3rd step: at 1550 DEG C, divides compound 4～6 times and joins quartz crucible/corundum crucible, platinum earthenware
In crucible, found 4 hours with fusion method；
4th step: at 1580 DEG C, vitreous humour is clarified 6 hours；
6th step: carry out mechanical agitation 9 hours；
7th step: prepared vitreous humour is poured in graphite or cast iron die sizing；
8th step: after being incubated 4 hours at 800 DEG C in Muffle furnace, carry out conventional annealing process；
9th step: to obtain glass cut, fine grinding, after polishing, carry out soda acid combination process 3.5 hours；；
Tenth step: at 850 DEG C, glass sample is incubated 24 hours, is warmed up to 1050 DEG C and is incubated 10 hours.
Other implementations are all identical with embodiment 1,2, and simply the formula in preparation technology is different.It is listed below
Component.
Glass prepared by above-described embodiment has in the tunable cut-off of 200-600nm spectral region, and xenon lamp can be suppressed to exist
The inefficient pumping to neodymium glass rod of the 200-600nm scope, and then reduce the thermal distoftion in gain media.As shown in Figure 2, exist
Neodymium-doped laser glass laser instrument increases devitrified glass prepared by embodiment 1 filter pipe, reduce the thermal efficiency 50% of xenon lamp with
On；Additionally by titanium oxide with zirconic be simultaneously introduced, increase the overall crystallization property of glass, and then be obviously improved glass
Thermal shock resistance, under 1700 Joule energy pumpings, the pipe that filters bursts.
The present invention prepare for having the crystallite filter glass in the tunable cut-off of 200-600nm spectral region, can be big
Thermal distoftion in amplitude reduction gain media；
The present invention is prepared glass and can be processed by controlled micro crystallization, increases substantially the thermal shock resistance of glass, extends crystallite
The service life of glass filter part and use operating frequency.
Claims (3)
1. mix a ultraviolet cut-on height Aluminous Silicate Glass-Ceramics for cerium, titanium, be characterised by the molar percentage composition of this glass
For: SiO2: 40～50mol%, Al2O3: 25～35mol%, MgO:5～10mol%, ZnO:0～5mol%；Li2O:0-
5mol%, TiO2: 5～10mol%, ZrO2: 0～5mol%, CeO2: 3～8mol%.
2. the preparation method of the ultraviolet cut-on height Aluminous Silicate Glass-Ceramics mixing cerium, titanium described in claim 1, it is characterised in that
Comprise the following steps:
1. calculate the percentage by weight of glass by the molar percentage of host glass composition, then weigh raw material, mix homogeneously,
Form compound；
2. described compound is put in crucible, be placed in the silicon molybdenum rod furnace of 1500～1600 DEG C and melt, during fusing
Between be 2～8 hours；
3. annealing: glass pouring is put into warmed up to the Muffle furnace of glass transformation temperature after going out, after being incubated 3 hours, with 5～10
DEG C/h rate of temperature fall be down to 200 DEG C, then cool to room temperature with the furnace；
4. the host glass after annealing is warming up to 750～850 DEG C, is incubated 8～16 hours, then proceed to be warming up to 900～
1050 DEG C, it is incubated 2～8 hours, it is thus achieved that nano crystalline glass.
The ultraviolet cut-on height Aluminous Silicate Glass-Ceramics mixing cerium, titanium the most according to claim 1, it is characterised in that it is right to have
The tunable cut-off of xenon lamp spectrum 200-600nm scope, it is adaptable to the optical filtering unit device in repetition high-energy neodymium glass laser system
Part.
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| CN201610394546.9A CN106082677B (en) | 2016-06-06 | 2016-06-06 | Mix cerium, the high Aluminous Silicate Glass-Ceramics of the ultraviolet cut-on of titanium and preparation method thereof |
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| CN201610394546.9A CN106082677B (en) | 2016-06-06 | 2016-06-06 | Mix cerium, the high Aluminous Silicate Glass-Ceramics of the ultraviolet cut-on of titanium and preparation method thereof |
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| CN106082677B CN106082677B (en) | 2018-04-13 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107171168A (en) * | 2017-07-25 | 2017-09-15 | 秦树军 | It is a kind of to improve the spectrum body of laser photoelectricity conversion efficiency and optical quality |
| CN110698061A (en) * | 2019-11-07 | 2020-01-17 | 成都为光科技有限公司 | Samarium and cerium doped infrared absorption low-expansion aluminum borate glass and preparation method thereof |
| CN112038468A (en) * | 2020-09-17 | 2020-12-04 | 有研稀土新材料股份有限公司 | Red LED optical device |
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| RU2374190C1 (en) * | 2008-04-22 | 2009-11-27 | Федеральное государственное унитарное предприятие "Обнинское научно-производственное предприятие "Технология" | Glass-ceramic material |
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2016
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Patent Citations (4)
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| US4162921A (en) * | 1977-01-05 | 1979-07-31 | Firsov Vitaly M | Glass-crystalline material and method of producing same |
| JP2000313639A (en) * | 1999-02-25 | 2000-11-14 | Nippon Sheet Glass Co Ltd | Crystallized glass and method for producing the same, and substrate using the same and used for information recording medium, information recording medium and information recording device |
| RU2374190C1 (en) * | 2008-04-22 | 2009-11-27 | Федеральное государственное унитарное предприятие "Обнинское научно-производственное предприятие "Технология" | Glass-ceramic material |
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Non-Patent Citations (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107171168A (en) * | 2017-07-25 | 2017-09-15 | 秦树军 | It is a kind of to improve the spectrum body of laser photoelectricity conversion efficiency and optical quality |
| CN110698061A (en) * | 2019-11-07 | 2020-01-17 | 成都为光科技有限公司 | Samarium and cerium doped infrared absorption low-expansion aluminum borate glass and preparation method thereof |
| CN112038468A (en) * | 2020-09-17 | 2020-12-04 | 有研稀土新材料股份有限公司 | Red LED optical device |
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| CN106082677B (en) | 2018-04-13 |
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