CN109678348A - A kind of fluorine oxygen ceramic-vitreous material and preparation method thereof - Google Patents
A kind of fluorine oxygen ceramic-vitreous material and preparation method thereof Download PDFInfo
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- CN109678348A CN109678348A CN201910143982.2A CN201910143982A CN109678348A CN 109678348 A CN109678348 A CN 109678348A CN 201910143982 A CN201910143982 A CN 201910143982A CN 109678348 A CN109678348 A CN 109678348A
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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
Abstract
The invention discloses a kind of fluorine oxygen ceramic-vitreous materials and preparation method thereof, and raw material includes: GeO210-20mol%, SiO220-40mol%, Al2O310-20mol%, B2O31-10mol%, Li2O 1-10mol%, BaF225-40mol%, Yb2O30.6-3mol% and TmF30.2-0.5mol%.The logical fluorin-oxygen glass ceramic material luminescent properties obtained of the present invention are superior, luminous efficiency is high, mechanical strength is good, enrich application of the fluorin-oxygen glass material system on material of infrared window.
Description
Technical field
The present invention relates to technical field of glass materials, and in particular to a kind of fluorine oxygen ceramic-vitreous material and preparation method thereof.
Background technique
Fluorine oxide material system converts luminous efficiency because not only having the characteristics that on the height of fluoride, but also has oxide material
The characteristics of chemical stability of material is good, high mechanical strength, and have broad application prospects.Fluorin-oxygen glass has low phonon energy
Characteristic, and chemical stability and mechanical strength properties are good, attract wide attention in luminous and photon field, are incandescnet particles
Good host material.
Currently, adulterating various incandescnet particles for fluorin-oxygen glass has many reports, including doping with rare-earth ions, heavy metal from
Son and transition metal ions, but the research in terms of material of infrared window is less, and existing fluorin-oxygen glass Integral luminous performance, machine
It still needs further improvement for tool intensity, and heavy metal ion is gradually abandoned making and using due to its contamination hazard.
Summary of the invention
The object of the present invention is to provide a kind of fluorine oxygen ceramic-vitreous materials and preparation method thereof, to solve existing fluorin-oxygen glass
Host material luminous efficiency as incandescnet particle doping is low, luminous intensity is low and mechanical strength is not high problem, provides one
The material of infrared window that kind luminous efficiency is high, luminous intensity is high, mechanical strength is good.
The technical scheme to solve the above technical problems is that
A kind of fluorine oxygen ceramic-vitreous material, including raw material: GeO210-20mol%, SiO220-40mol%, Al2O3
10-20mol%, B2O31-10mol%, Li2O 1-10mol%, BaF225-40mol%, Yb2O30.6-3mol% and TmF3
0.2-0.5mol%.
Further, in preferred embodiments of the present invention, above-mentioned fluorine oxygen ceramic-vitreous material is obtained by following methods: will
It is obtained after heating melting, annealing, for the first time heat treatment and the second heat treatment after above-mentioned raw materials mixing.
Further, in preferred embodiments of the present invention, the temperature of heating melting is 1300-1500 DEG C, heating time
For 45-60min；Annealing temperature is 350-480 DEG C, annealing time 2-3h；The temperature of heat treatment is 550-700 DEG C for the first time,
Soaking time is 2-4h；The temperature of second of heat treatment is 900-1000 DEG C, soaking time 1-2h, and is carrying out the second heat
When processing also apply electric field strength be 8500-9500V/cm, the frequency conversion high voltage electric field that frequency is 20-40Hz.
Further, in preferred embodiments of the present invention, above-mentioned fluorine oxygen ceramic-vitreous material includes raw material: GeO2 12-
16mol%, SiO225-35mol%, Al2O312-16mol%, B2O32-6mol%, Li2O 2-6mol%, BaF2 25-
35mol%, Yb2O31-2.4mol% and TmF30.3-0.4mol%.
The preparation method of above-mentioned fluorine oxygen ceramic-vitreous material, comprising:
(1) after above-mentioned raw materials being mixed at 1300-1500 DEG C heating melting 45-60min, at 1320-1360 DEG C go out
Material, is then poured into compression moulding in mold, obtains prefabricated sample；
(2) prefabricated sample is made annealing treatment into 2-3h at 350-480 DEG C, obtains forerunner's glass；
(3) forerunner's glass is successively carried out being heat-treated for the first time and second is heat-treated；
Wherein, the process being heat-treated for the first time are as follows: forerunner's glass is warming up to 550-700 with the rate of 10-15 DEG C/min
DEG C heat preservation 2-4h；
The process of second of heat treatment are as follows: by forerunner's glass after first time is heat-treated with the rate of 5-10 DEG C/min
It is warming up to 900-1000 DEG C and keeps the temperature 1-2h under frequency conversion high voltage electric field, be cooled to room temperature, fluorine oxygen ceramic-vitreous material is made；Its
In, the electric field strength of frequency conversion high voltage electric field is 8500-9500V/cm, frequency 20-40Hz.
Further, in preferred embodiments of the present invention, in step (1), the melting temperature of raw material components is 1350-
1450℃。
Further, in preferred embodiments of the present invention, in step (2), annealing temperature is 400-450 DEG C, when annealing
Between be 2-2.5h.
Further, in preferred embodiments of the present invention, in step (3), the temperature of heat treatment is 600-660 for the first time
DEG C, soaking time 3.5-4h.
Further, in preferred embodiments of the present invention, in step (3), the temperature of second of heat treatment is 950-980
DEG C, soaking time 1-1.5h.
Further, in preferred embodiments of the present invention, in step (3), the electric field strength of frequency conversion high voltage electric field is
8800-9300V/cm, frequency 25-35Hz.
The invention has the following advantages:
The present invention combines specific work by improving host glass component and content and the suitable rare earth ion of addition
Skill Parameter Conditions obtain the fluorin-oxygen glass ceramic material that luminescent properties are superior, luminous efficiency is high, mechanical strength is good, enrich fluorine oxygen
Application of the glass material system on material of infrared window.
The present invention added in glass matrix germanium ion obtain glass matrix category germanate glass, germanate glass have compared with
Low phonon energy, good glass forming ability can both make up germanate simultaneously because introducing fluoride in matrix components
The defect that water content is big in glass, fusion temperature is high, viscosity is big, and the controlled micro crystallization (ceramic) of glass, Jin Ergai may be implemented
It is apt to the optical property of entire glass system, and the rare earth ion adulterated: Yb3+And Tm3+Solubility is compared to common glassy silicate
Glass is improved largely.In terms of choosing rare earth ion, the present invention is with Yb3+And Tm3+Codope is carried out, with Yb3+As sensitization from
Son, Tm3+As the centre of luminescence, Yb3+Transfer energy to active ions Tm3+, it is allowed to from ground state transition to excitation state, in sharp
Excited-state Absorption occurs again and continues up generation transition for the ion of hair state, to form certain population cloth in higher energy level
It occupies, to improve luminous efficiency and luminous intensity.In addition, alkali metal Li+Introducing advantageously reduced fluorescent quenching concentration, have
Conducive to further increasing luminescent properties.
In terms of preparation process, the present invention adjusts to control out to be melted suitable for the heating of glass-ceramic substrate component of the present invention
Melt, anneal and heat treatment process parameter, and when carrying out second and being heat-treated, by increasing high-pressure frequency-conversion electric field, so that former
Expect that the ion in component can promote (direction of an electric field is identical as ionic charge) or inhibit (electricity in displacement under electric field action
Field direction is opposite with ionic charge) diffusion and migration of ion, microcrystalline growth is realized and is controlled, nucleus is avoided to reunite.
Specific embodiment
Principles and features of the present invention are described with reference to embodiments, the given examples are served only to explain the present invention,
It is not intended to limit the scope of the present invention.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer suggests
Condition carries out.Reagents or instruments used without specified manufacturer is the conventional products that can be obtained by commercially available purchase.
Embodiment 1:
The fluorine oxygen ceramic-vitreous material of the present embodiment, raw material includes: GeO215mol%, SiO230mol%, Al2O3
15mol%, B2O36mol%, Li2O 2mol%, BaF230mol%, Yb2O31.6mol% and TmF30.4mol%.
The preparation method of the fluorine oxygen ceramic-vitreous material of the present embodiment, comprising:
(1) at 1400 DEG C then heating melting 45min is poured into 1350 DEG C of bottom discharges after mixing above-mentioned raw materials
Compression moulding in mold obtains prefabricated sample；
(2) prefabricated sample is made annealing treatment into 3h at 450 DEG C, obtains forerunner's glass；
(3) forerunner's glass is successively carried out being heat-treated for the first time and second is heat-treated；
Wherein, the process being heat-treated for the first time are as follows: forerunner's glass is warming up to 600 DEG C of heat preservations with the rate of 12 DEG C/min
3h；
The process of second of heat treatment are as follows: by forerunner's glass after first time is heat-treated with the rate liter of 10 DEG C/min
Temperature keeps the temperature 1.5h to 900 DEG C and under frequency conversion high voltage electric field, is cooled to room temperature, and fluorine oxygen ceramic-vitreous material is made；Wherein, frequency conversion
The electric field strength of high voltage electric field is 9000V/cm, frequency 30Hz.
Fluorine oxygen glass-ceramic sample obtained above is passed through into surface polishing treatment, highest transmitance can in visible range
Up to 89%, the fluorescence lifetime of upper laser level is 314 μ s, fluorescence quantum efficiency is up to 57.5%, and bend resistance intensity is 191MPa.
Embodiment 2:
The fluorine oxygen ceramic-vitreous material of the present embodiment, raw material includes: GeO210mol%, SiO240mol%, Al2O3
10mol%, B2O310mol%, Li2O 2mol%, BaF225mol%, Yb2O32.8mol% and TmF30.2mol%.
The preparation method of the fluorine oxygen ceramic-vitreous material of the present embodiment, comprising:
(1) at 1300 DEG C then heating melting 60min is poured into 1320 DEG C of bottom discharges after mixing above-mentioned raw materials
Compression moulding in mold obtains prefabricated sample；
(2) prefabricated sample is made annealing treatment into 3h at 350 DEG C, obtains forerunner's glass；
(3) forerunner's glass is successively carried out being heat-treated for the first time and second is heat-treated；
Wherein, the process being heat-treated for the first time are as follows: forerunner's glass is warming up to 550 DEG C of heat preservations with the rate of 10 DEG C/min
4h；
The process of second of heat treatment are as follows: by forerunner's glass after first time is heat-treated with the rate liter of 5 DEG C/min
Temperature keeps the temperature 2h to 900 DEG C and under frequency conversion high voltage electric field, is cooled to room temperature, and fluorine oxygen ceramic-vitreous material is made；Wherein, frequency conversion is high
The electric field strength of piezoelectric field is 8500V/cm, frequency 20Hz.
Fluorine oxygen glass-ceramic sample obtained above is passed through into surface polishing treatment, highest transmitance can in visible range
Up to 85%, the fluorescence lifetime of upper laser level is 302 μ s, fluorescence quantum efficiency is up to 56%, and bend resistance intensity is 185MPa.
Embodiment 3:
The fluorine oxygen ceramic-vitreous material of the present embodiment, raw material includes: GeO220mol%, SiO220mol%, Al2O3
10mol%, B2O31mol%, Li2O 6mol%, BaF240mol%, Yb2O32.7mol% and TmF30.3mol%.
The preparation method of the fluorine oxygen ceramic-vitreous material of the present embodiment, comprising:
(1) at 1500 DEG C then heating melting 45min is poured into 1360 DEG C of bottom discharges after mixing above-mentioned raw materials
Compression moulding in mold obtains prefabricated sample；
(2) prefabricated sample is made annealing treatment into 2h at 480 DEG C, obtains forerunner's glass；
(3) forerunner's glass is successively carried out being heat-treated for the first time and second is heat-treated；
Wherein, the process being heat-treated for the first time are as follows: forerunner's glass is warming up to 690 DEG C of heat preservations with the rate of 15 DEG C/min
2.5h；
The process of second of heat treatment are as follows: by forerunner's glass after first time is heat-treated with the rate liter of 10 DEG C/min
Temperature keeps the temperature 1h to 1000 DEG C and under frequency conversion high voltage electric field, is cooled to room temperature, and fluorine oxygen ceramic-vitreous material is made；Wherein, frequency conversion
The electric field strength of high voltage electric field is 9500V/cm, frequency 40Hz.
Fluorine oxygen glass-ceramic sample obtained above is passed through into surface polishing treatment, highest transmitance can in visible range
Up to 86.3%, the fluorescence lifetime of upper laser level is 308 μ s, fluorescence quantum efficiency is up to 57.8%, and bend resistance intensity is 188MPa.
Embodiment 4:
The fluorine oxygen ceramic-vitreous material of the present embodiment, raw material includes: GeO212mol%, SiO235mol%, Al2O3
16mol%, B2O33mol%, Li2O 6mol%, BaF225mol%, Yb2O32.5mol% and TmF30.5mol%.
The preparation method of the fluorine oxygen ceramic-vitreous material of the present embodiment, comprising:
(1) at 1350 DEG C then heating melting 50min is poured into 1350 DEG C of bottom discharges after mixing above-mentioned raw materials
Compression moulding in mold obtains prefabricated sample；
(2) prefabricated sample is made annealing treatment into 2.5h at 400 DEG C, obtains forerunner's glass；
(3) forerunner's glass is successively carried out being heat-treated for the first time and second is heat-treated；
Wherein, the process being heat-treated for the first time are as follows: forerunner's glass is warming up to 700 DEG C of heat preservations with the rate of 10 DEG C/min
2h；
The process of second of heat treatment are as follows: by forerunner's glass after first time is heat-treated with the rate liter of 6 DEG C/min
Temperature keeps the temperature 2h to 900 DEG C and under frequency conversion high voltage electric field, is cooled to room temperature, and fluorine oxygen ceramic-vitreous material is made；Wherein, frequency conversion is high
The electric field strength of piezoelectric field is 9000V/cm, frequency 30Hz.
Fluorine oxygen glass-ceramic sample obtained above is passed through into surface polishing treatment, highest transmitance can in visible range
Up to 85.5%, the fluorescence lifetime of upper laser level is 305 μ s, fluorescence quantum efficiency is up to 57.1%, and bend resistance intensity is 187MPa.
Embodiment 5:
The fluorine oxygen ceramic-vitreous material of the present embodiment, raw material includes: GeO212mol%, SiO235mol%, Al2O3
12mol%, B2O32mol%, Li2O 2mol%, BaF235mol%, Yb2O31.5mol% and TmF30.5mol%.
The preparation method of the fluorine oxygen ceramic-vitreous material of the present embodiment, comprising:
(1) at 1450 DEG C then heating melting 45min is poured into 1320 DEG C of bottom discharges after mixing above-mentioned raw materials
Compression moulding in mold obtains prefabricated sample；
(2) prefabricated sample is made annealing treatment into 2.3h at 450 DEG C, obtains forerunner's glass；
(3) forerunner's glass is successively carried out being heat-treated for the first time and second is heat-treated；
Wherein, the process being heat-treated for the first time are as follows: forerunner's glass is warming up to 650 DEG C of heat preservations with the rate of 10 DEG C/min
3h；
The process of second of heat treatment are as follows: by forerunner's glass after first time is heat-treated with the rate liter of 10 DEG C/min
Temperature keeps the temperature 1.5h to 980 DEG C and under frequency conversion high voltage electric field, is cooled to room temperature, and fluorine oxygen ceramic-vitreous material is made；Wherein, frequency conversion
The electric field strength of high voltage electric field is 8800V/cm, frequency 25Hz.
Fluorine oxygen glass-ceramic sample obtained above is passed through into surface polishing treatment, highest transmitance can in visible range
Up to 84.6%, the fluorescence lifetime of upper laser level is 311 μ s, fluorescence quantum efficiency is up to 57.3%, and bend resistance intensity is 186MPa.
Embodiment 6:
The fluorine oxygen ceramic-vitreous material of the present embodiment, raw material includes: GeO215mol%, SiO225mol%, Al2O3
16mol%, B2O36mol%, Li2O 3mol%, BaF232.25mol%, Yb2O32.4mol% and TmF30.35mol%.
The preparation method of the fluorine oxygen ceramic-vitreous material of the present embodiment, comprising:
(1) at 1400 DEG C then heating melting 50min inclines in 1320-1360 DEG C of bottom discharge after mixing above-mentioned raw materials
The compression moulding in mold obtains prefabricated sample；
(2) prefabricated sample is made annealing treatment into 2-3h at 350-480 DEG C, obtains forerunner's glass；
(3) forerunner's glass is successively carried out being heat-treated for the first time and second is heat-treated；
Wherein, the process being heat-treated for the first time are as follows: forerunner's glass is warming up to 660 DEG C of heat preservations with the rate of 10 DEG C/min
4h；
The process of second of heat treatment are as follows: by forerunner's glass after first time is heat-treated with the rate liter of 10 DEG C/min
Temperature keeps the temperature 2h to 960 DEG C and under frequency conversion high voltage electric field, is cooled to room temperature, and fluorine oxygen ceramic-vitreous material is made；Wherein, frequency conversion is high
The electric field strength of piezoelectric field is 9300V/cm, frequency 30Hz.
Fluorine oxygen glass-ceramic sample obtained above is passed through into surface polishing treatment, highest transmitance can in visible range
Up to 84.2%, the fluorescence lifetime of upper laser level is 308 μ s, fluorescence quantum efficiency is up to 55.7%, and bend resistance intensity is 181MPa.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of fluorine oxygen ceramic-vitreous material, which is characterized in that including raw material: GeO210-20mol%, SiO2 20-
40mol%, Al2O310-20mol%, B2O31-10mol%, Li2O 1-10mol%, BaF225-40mol%, Yb2O3
0.6-3mol% and TmF30.2-0.5mol%.
2. fluorine oxygen ceramic-vitreous material according to claim 1, which is characterized in that the fluorine oxygen ceramic-vitreous material by with
Lower method obtains: obtaining after heating melting, annealing, for the first time heat treatment and the second heat treatment after above-mentioned raw materials are mixed.
3. fluorine oxygen ceramic-vitreous material according to claim 1, which is characterized in that the temperature of heating melting is 1300-
1500 DEG C, heating time 45-60min；Annealing temperature is 350-480 DEG C, annealing time 2-3h；The temperature of heat treatment for the first time
Degree is 550-700 DEG C, soaking time 2-4h；The temperature of second of heat treatment is 900-1000 DEG C, soaking time 1-2h, and
And carry out second be heat-treated when also apply electric field strength be 8500-9500V/cm, the frequency conversion high-voltage electricity that frequency is 20-40Hz
?.
4. fluorine oxygen ceramic-vitreous material according to claim 1, which is characterized in that including raw material: GeO212-16mol%,
SiO225-35mol%, Al2O312-16mol%, B2O32-6mol%, Li2O 2-6mol%, BaF225-35mol%,
Yb2O31-2.4mol% and TmF30.3-0.4mol%.
5. the preparation method of the described in any item fluorine oxygen ceramic-vitreous materials of claim 1-4 characterized by comprising
(1) after above-mentioned raw materials being mixed at 1300-1500 DEG C heating melting 45-60min, in 1320-1360 DEG C of bottom discharge, so
After be poured into compression moulding in mold, obtain prefabricated sample；
(2) the prefabricated sample is made annealing treatment into 2-3h at 350-480 DEG C, obtains forerunner's glass；
(3) forerunner's glass is successively carried out being heat-treated for the first time and second is heat-treated；
Wherein, the process of the first time heat treatment are as follows: forerunner's glass is warming up to 550-700 with the rate of 10-15 DEG C/min
DEG C heat preservation 2-4h；
The process of second of the heat treatment are as follows: by forerunner's glass after first time is heat-treated with the rate of 5-10 DEG C/min
It is warming up to 900-1000 DEG C and keeps the temperature 1-2h under frequency conversion high voltage electric field, be cooled to room temperature, fluorine oxygen ceramic-vitreous material is made；Its
In, the electric field strength of the frequency conversion high voltage electric field is 8500-9500V/cm, frequency 20-40Hz.
6. preparation method according to claim 5, which is characterized in that in step (1), the melting temperature of raw material components is
1350-1450℃。
7. preparation method according to claim 5, which is characterized in that in step (2), annealing temperature is 400-450 DEG C, is moved back
The fiery time is 2-2.5h.
8. preparation method according to claim 5, which is characterized in that in step (3), the temperature of heat treatment is for the first time
600-660 DEG C, soaking time 3.5-4h.
9. preparation method according to claim 5, which is characterized in that in step (3), the temperature of second of heat treatment is
950-980 DEG C, soaking time 1-1.5h.
10. preparation method according to claim 5, which is characterized in that in step (3), the electric-field strength of frequency conversion high voltage electric field
Degree is 8800-9300V/cm, frequency 25-35Hz.
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