CN106946462A - A kind of transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass and preparation method thereof - Google Patents

A kind of transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass and preparation method thereof Download PDF

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CN106946462A
CN106946462A CN201710296209.0A CN201710296209A CN106946462A CN 106946462 A CN106946462 A CN 106946462A CN 201710296209 A CN201710296209 A CN 201710296209A CN 106946462 A CN106946462 A CN 106946462A
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glass
rare earth
earth ion
sio
sides
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韩建军
刘亚丽
刘超
赵志永
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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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
    • C03C10/16—Halogen containing crystalline phase
    • 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

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Materials Engineering (AREA)
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  • Ceramic Engineering (AREA)
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Abstract

The present invention provides a kind of transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass and preparation method thereof.The glass is constituted：SiO2:50~70mol%, Al2O3:3~12mol%, Na2O:15~20mol%, NaF:5~12mol%, YF3:5~12mol%, above-mentioned composition sum is 100%；The glass composition also includes the ErF for accounting for 0.1~1mol% of above-mentioned composition sum3, wherein SiO2：Al2O3Molar content ratio be more than 6.5.Compared to silicate glass, six side's yttrium fluoride natrium fluorine oxygen devitrified glasses have the relatively low phonon energy (can as little as 230cm‑1), the multi-phonon non-radiative relaxation speed of rare earth ion is reduced, so that up-conversion luminescence efficiency of the rare earth ion in devitrified glass is improved significantly.

Description

A kind of transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass and its system Preparation Method
Technical field
The present invention relates to field of light emitting materials, more particularly to a kind of transparent rare earth ion doped β-NaYF4Fluorine oxygen crystallite Glass and preparation method thereof.
Background technology
Rear-earth-doped up-conversion luminescent material is because of extensive concern of its unique luminescent properties by each field.However, by Up-conversion phosphor made from the synthetic methods such as water/solvent-thermal method, liquid-phase coprecipitation, thermal decomposition method, because of its high scattering and not The transparency, and application in terms of Solid State Laser has limitation, limits its practical ranges, thus it is desirable that energy It is made with higher clarity, preferably chemistry and the block up-conversion of mechanical stability.
The indexs such as chemical stability, the mechanical strength of oxide glass have an obvious superiority, but oxide glass Phonon energy it is too high, the efficiency that result in rare earth ion doped oxide glass up-conversion luminescence is very undesirable.Fluoride Glass can mix the features such as concentration is high, phonon energy is low, radiationless transition probability is small due to its rare earth ion, for rare earth ion Relatively good matrix, but fluoride glass preparation condition is harsh, expensive, hold corrosion-vulnerable and unstable etc., these because Element all limits their practical application.Rear-earth-doped fluorine oxygen devitrified glass has had the advantage of the two concurrently：In fluorine oxygen devitrified glass In, fluoride microcrystal is small to tens or even more than ten nanometers, it is ensured that the transparency of height；It is rare earth ion doped to arrive crystal of fluoride In, it is ensured that high doping concentration and the environment of low phonon energy；Crystal of fluoride is oxidized thing and surrounded again, it is ensured that good Mechanical performance.The material of the low phonon energy of fluoride and the mechanical performance of oxide is so combined, is necessarily had greatly Potential using value.
The luminescent properties of rear-earth-doped fluorine oxygen devitrified glass are directly related with fluoride nano crystal.NaYF4With phonon energy The features such as radiationless relaxation of low, multi-phonon is low, luminous efficiency is high is measured, it there are two kinds of crystal structures：Emission in Cubic α-NaYF4With six sides Phase β-NaYF4。β-NaYF4It is considered as to change host material on current efficiency highest Infrared-Visible, it has very low Phonon energy, minimum can reach 230cm-1.However, for the rear-earth-doped fluorin-oxygen glass of general component, Low Temperature Heat Treatment is only α-NaYF can be obtained4, and β-NaYF4Often it can just be obtained by higher heat treatment temperature, now nanocrystalline crystallization size mistake Greatly, silicate phase is separated out, and causes glass devitrification, and that obtain is α-NaYF4With β-NaYF4Mixed phase, thus real hair Wave β-NaYF4Advantage in up-conversion luminescence, it is impossible to meet the requirement of practical application.To realize β-NaYF4Truly Using preparing transparent rare-earth doped beta-NaYF4Fluorine oxygen devitrified glass is imperative.
The content of the invention
The present invention provides a kind of transparent rare earth ion doped β-NaYF to solve above-mentioned technical problem4Fluorine oxygen devitrified glass And preparation method thereof.The devitrified glass not only has good chemical stability and mechanical performance, and is lighted with good Performance.
To achieve these goals, the technical scheme is that：
A kind of transparent rare earth ion doped β-NaYF4Fluorine oxygen devitrified glass, the glass, which is constituted, is：SiO2:50~ 70mol%, Al2O3:3~12mol%, Na2O:15~20mol%, NaF:5~12mol%, YF3:5~12mol%, above-mentioned group / and be 100%；The glass composition also includes the ErF for accounting for 0.1~1mol% of above-mentioned composition sum3, wherein SiO2： Al2O3Molar content ratio be more than 6.5.
In such scheme, SiO in the glass composition2Content is more than 55mol%.
In such scheme, Al in the glass composition2O3Content is not more than 10mol%.
In such scheme, the glass composition is：SiO2:60mol%, Al2O3:9mol%, Na2O:16mol%, NaF: 7mol%, YF3:8mol%, ErF3:0.5mol%.
In such scheme, the glass composition is：SiO2:60mol%, Al2O3:7mol%, Na2O:18mol%, NaF: 7mol%, YF3:8mol%, ErF3:0.5mol%.
In such scheme, the glass composition is：SiO2:60mol%, Al2O3:5mol%, Na2O:18mol%, NaF: 7mol%, YF3:10mol%, ErF3:0.5mol%.
Described transparent rare earth ion doped β-NaYF4The preparation method of fluorine oxygen devitrified glass, this method be first by Molar percentage weighed and be sufficiently mixed uniformly with ball milling sample mixing machine after each component raw material, in the corundum crucible for being placed in densification, Founded at a temperature of 1450~1550 DEG C 1~2 hour；Then gained glass melt is poured on metal copper mold and be pressed into rapidly Type, anneal 3h at 350 DEG C, obtains transparent forerunner's glass；Forerunner's glass is heat-treated again, transparent rare earth ion is obtained and mixes Miscellaneous β-NaYF4Fluorine oxygen devitrified glass.
In such scheme, the heat treating regime is to be incubated 1~3 hour at a temperature of 550~700 DEG C.
The present invention prepares transparent rare earth ion doped β-NaYF using fusion method4Na in fluorine oxygen devitrified glass, its composition2O As fluxing agent, the viscosity and surface tension of glass metal are reduced, promotes clarification and the homogenizing of glass metal.Na2O、NaF、YF3Jointly To form β-NaYF4Element needed for providing.SiO2For glass network former.Al2O3For network intermediate, conduct when content is high Network former, causes glass network structural relaxation；As network outer body when content is low, now only SiO2Formed as network Body, glass network structure is finer and close.For NaYF4Two kinds of structures, hexagonal phase β-NaYF4It is then thermodynamics stable state crystalline phase；Cube Phase α-NaYF4For thermodynamics metastable state crystalline phase, it can spontaneously be changed into hexagonal phase at relatively high temperatures.However, being intended in glass Form hexagonal phase β-NaYF4, only frequently can lead to the decline of glass transparent degree by improving heat treatment temperature.By adjusting glass group Into SiO in rise glass2Content, reduces Al2O3Content, makes glass network compact structure, and its jammed effect causes metastable α-NaYF4Can not exist, so that pure β-NaYF be made in glass4Crystalline phase.This be the present invention with other rare earth ion doped β- NaYF4Fluorine oxygen devitrified glass, compared to maximum advantage, is also its innovation.
The beneficial effects of the present invention are：
The present invention realizes β-NaYF by adjusting fluorin-oxygen glass component, optimization Technology for Heating Processing4It is nanocrystalline in crystallite glass Separated out in glass.Due to rare earth ion Er3+With Y3+Ionic radius is close, and valence state is identical, Er3+Part substitution Y3+Position is so as to enter Enter the β-NaYF to precipitation4In nanometer lattice.Compared to silicate glass (phonon energy 1100cm-1), β-NaYF4With relatively low Phonon energy (can as little as 230cm-1), reduce the multi-phonon non-radiative relaxation speed of rare earth ion so that rare earth from Up-conversion luminescence efficiency of the son in devitrified glass is improved significantly.
Brief description of the drawings
Fig. 1 to Fig. 3 is respectively that embodiment 1 is heat-treated the XRD spectrum of front and rear sample, UV-visible-near infrared absorption And fluorescence spectrum.
Fig. 4 to Fig. 6 is respectively that embodiment 2 is heat-treated the XRD spectrum of front and rear sample, UV-visible-near infrared absorption And fluorescence spectrum.
Fig. 7 to Fig. 9 is respectively that embodiment 3 is heat-treated the XRD spectrum of front and rear sample, UV-visible-near infrared absorption And fluorescence spectrum.
Figure 10 is the XRD spectrum that comparative example 1 is heat-treated front and rear sample.
Figure 11 is the XRD spectrum that comparative example 2 is heat-treated front and rear sample.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention Content is not limited solely to the following examples.
Embodiment 1
The glass of the present embodiment constitutes (S1)：SiO2:60mol%, Al2O3:9mol%, Na2O:16mol%, NaF: 7mol%, YF3:8mol%, ErF3:0.5mol%, the pure SiO of raw material Analysis about Selection2、Al2O3、Na2CO3, NaF and spectroscopic pure YF3With ErF3.Raw material SiO is weighed by above-mentioned molar percentage2:13.5529g,Al2O3:3.4498g,Na2CO3:6.3753g, NaF:1.1050g,YF3:4.3880g,ErF3:0.4215g, is sufficiently mixed uniformly with ball milling sample mixing machine, is placed in the corundum earthenware of densification In crucible, founded at a temperature of 1500 DEG C 1.5 hours；Then gained glass melt is poured on metal copper mold and be pressed into rapidly Type, anneal 3h at 350 DEG C, obtains transparent forerunner's glass；Forerunner's glass is heat-treated 2 hours at 650 DEG C again, obtains transparent Rare earth ion doped β-NaYF4Fluorine oxygen devitrified glass.Fig. 1 is the X ray diffracting spectrum of devitrified glass after sample S1 is heat-treated, PDF cards are compareed, crystalline phase is β-NaYF4；β-NaYF in the devitrified glass sample are can be calculated using Scherrer formula4It is average Particle size is 46.2nm.Fig. 2 is the UV-visible-near infrared absorption figure before and after sample S1 is heat-treated, and can therefrom be seen Arrive, devitrified glass sample the splitting at peak occurs at~1530nm after heat treatment, illustrates Er3+Enter β-NaYF4It is nanocrystalline, β- NaYF4Many case characteristics cause absorption spectrum to cleave.To carrying out luminescent properties test (Fig. 3) before and after sample S1 heat treatments, 980nm pumpings are observed that green glow (525nm, the 545nm) transmitting of devitrified glass sample after heat treatment is very strong；Compared to heat Before processing sample, its green emission integrated intensity improves two orders of magnitude.
Embodiment 2
The glass of the present embodiment constitutes (S2)：SiO2:60mol%, Al2O3:7mol%, Na2O:18mol%, NaF: 7mol%, YF3:8mol%, ErF3:0.5mol%, the pure SiO of raw material Analysis about Selection2、Al2O3、Na2CO3, NaF and spectroscopic pure YF3With ErF3.Raw material SiO is weighed by above-mentioned molar percentage2:13.5529g,Al2O3:2.6832g,Na2CO3:7.1722g, NaF:1.1050g,YF3:4.3880g,ErF3:0.4215g, is sufficiently mixed uniformly with ball milling sample mixing machine, is placed in the corundum earthenware of densification In crucible, founded at a temperature of 1500 DEG C 1.5 hours；Then gained glass melt is poured on metal copper mold and be pressed into rapidly Type, anneal 3h at 350 DEG C, obtains transparent forerunner's glass；Forerunner's glass is heat-treated 2 hours at 650 DEG C again, obtains transparent Rare earth ion doped β-NaYF4Fluorine oxygen devitrified glass.Fig. 4 is the X-ray diffraction of devitrified glass sample after sample S2 is heat-treated Collection of illustrative plates, compares PDF cards, and crystalline phase is β-NaYF4；β-NaYF in the devitrified glass sample are can be calculated using Scherrer formula4 Average particle size particle size is 51.4nm.Fig. 5 is the UV-visible-near infrared absorption figure before and after sample S2 is heat-treated, Cong Zhongke To see, there is the splitting at peak at~1530nm in devitrified glass sample after heat treatment, illustrates Er3+Enter β-NaYF4Nanometer Crystalline substance, β-NaYF4Many case characteristics cause absorption spectrum to cleave.To carrying out luminescent properties test (figure before and after sample S2 heat treatments 6), green glow (525nm, the 545nm) transmitting of devitrified glass sample is very strong after 980nm pumpings are observed that heat treatment；Phase Compared with sample before heat treatment, its green emission integrated intensity improves two orders of magnitude.
Embodiment 3
The glass of the present embodiment constitutes (S3)：SiO2:60mol%, Al2O3:5mol%, Na2O:18mol%, NaF: 7mol%, YF3:10mol%, ErF3:0.5mol%, the pure SiO of raw material Analysis about Selection2、Al2O3、Na2CO3, NaF and spectrum Pure YF3With ErF3.Raw material SiO is weighed by above-mentioned molar percentage2:13.5529g,Al2O3:1.9166g,Na2CO3: 7.1722g,NaF:1.1050g,YF3:5.4850g,ErF3:0.4215g, is sufficiently mixed uniformly with ball milling sample mixing machine, is placed in densification Corundum crucible in, founded at a temperature of 1500 DEG C 1.5 hours；Then gained glass melt is poured on metal copper mold rapidly Compressing, anneal 3h at 350 DEG C, obtains transparent forerunner's glass；Forerunner's glass is heat-treated 3 hours at 650 DEG C again, obtained To transparent rare earth ion doped β-NaYF4Fluorine oxygen devitrified glass.Fig. 7 is that the X of devitrified glass sample after sample S3 is heat-treated is penetrated Ray diffraction diagram is composed, and compares PDF cards, and crystalline phase is β-NaYF4；It is can be calculated using Scherrer formula in the devitrified glass sample β-NaYF4Average particle size particle size is 55.7nm.Fig. 8 is the UV-visible-near infrared absorption before and after sample S3 is heat-treated Figure, therefrom it can be seen that, there is the splitting at peak at~1530nm in devitrified glass sample after heat treatment, illustrates Er3+Enter β- NaYF4It is nanocrystalline, β-NaYF4Many case characteristics cause absorption spectrum to cleave.To carrying out luminescent properties before and after sample S3 heat treatments Test (Fig. 9), green glow (525nm, the 545nm) transmitting of devitrified glass sample is non-after 980nm pumpings are observed that heat treatment Chang Qiang；Compared to sample before heat treatment, its green emission integrated intensity improves two orders of magnitude.
Comparative example 1
The glass of the present embodiment constitutes (R1)：SiO2:50mol%, Al2O3:15mol%, Na2O:18mol%, NaF: 7mol%, YF3:10mol%, ErF3:0.5mol%, the pure SiO of raw material Analysis about Selection2、Al2O3、Na2CO3, NaF and spectrum Pure YF3With ErF3.Raw material SiO is weighed by above-mentioned molar percentage2:11.2941g,Al2O3:5.7497g,Na2CO3: 7.1722g,NaF:1.1050g,YF3:5.4850g,ErF3:0.4215g, is sufficiently mixed uniformly with ball milling sample mixing machine, is placed in densification Corundum crucible in, founded at a temperature of 1500 DEG C 1.5 hours；Then gained glass melt is poured on metal copper mold rapidly Compressing, anneal 3h at 350 DEG C, obtains transparent forerunner's glass；Forerunner's glass is heat-treated 3 hours at 650 DEG C again, obtained To transparent devitrified glass.Figure 10 is the X ray diffracting spectrum of devitrified glass sample after sample R1 is heat-treated, and compares PDF cards, Crystalline phase is α-NaYF4, and non-beta-NaYF4.Due to SiO in R1 glass composition2：Al2O3Molar content ratio be less than 6.5, therefore glass In not separate out target nanocrystalline.
Comparative example 2
The glass of the present embodiment constitutes (R2)：SiO2:66mol%, Al2O3:7mol%, Na2O:12mol%, NaF: 7mol%, YF38mol%, ErF3:0.5mol%, the pure SiO of raw material Analysis about Selection2、Al2O3、Na2CO3, NaF and spectroscopic pure YF3With ErF3.Raw material SiO is weighed by above-mentioned molar percentage2:14.9082g,Al2O3:2.6832g,Na2CO3:4.7815g, NaF:1.1050g,YF3:4.3880g,ErF3:0.4215g, is sufficiently mixed uniformly with ball milling sample mixing machine, is placed in the corundum earthenware of densification In crucible, founded at a temperature of 1500 DEG C 1.5 hours；Then gained glass melt is poured on metal copper mold and be pressed into rapidly Type, anneal 3h at 350 DEG C, obtains transparent forerunner's glass；Forerunner's glass is heat-treated 3 hours at 650 DEG C again, obtains transparent Devitrified glass.Figure 11 is the X ray diffracting spectrum of devitrified glass sample after sample R2 is heat-treated, and compares PDF cards, and crystalline phase is α-NaYF4, and non-beta-NaYF4.Na in R2 glass composition2O is less than 15mol%, therefore it is nanocrystalline not separate out target in glass.
In summary, it is necessary to while meeting the SiO in the present invention2：Al2O3Molar content ratio be more than 6.5 and Na2O rubs You are more than 15mol% at content, and the transparent rare earth ion doped β-NaYF of excellent performance of the present invention could be successfully made4Fluorine oxygen is micro- Crystal glass.

Claims (8)

1. a kind of transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass, it is characterised in that the glass composition For：SiO2:50~70mol%, Al2O3:3~12mol%, Na2O:15~20mol%, NaF:5~12mol%, YF3:5~ 12mol%, above-mentioned composition sum is 100%；The glass composition also includes the 0.1~1mol%'s for accounting for above-mentioned composition sum ErF3, wherein SiO2：Al2O3Molar content ratio be more than 6.5.
2. transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass as claimed in claim 1, it is characterised in that SiO in the glass composition2Content is more than 55mol%.
3. transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass as claimed in claim 1, it is characterised in that Al in the glass composition2O3Content is not more than 10mol%.
4. transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass as claimed in claim 1, it is characterised in that The glass is constituted：SiO2:60mol%, Al2O3:9mol%, Na2O:16mol%, NaF:7mol%, YF3:8mol%, ErF3:0.5mol%.
5. transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass as claimed in claim 1, it is characterised in that The glass is constituted：SiO2:60mol%, Al2O3:7mol%, Na2O:18mol%, NaF:7mol%, YF3:8mol%, ErF3:0.5mol%.
6. transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass as claimed in claim 1, it is characterised in that The glass is constituted：SiO2:60mol%, Al2O3:5mol%, Na2O:18mol%, NaF:7mol%, YF3:10mol%, ErF3:0.5mol%.
7. the preparation method of transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass as claimed in claim 1, Characterized in that, this method is be sufficiently mixed uniformly with ball milling sample mixing machine by mole to weigh first after each component raw material, In the corundum crucible for being placed in densification, founded at a temperature of 1450~1550 DEG C 1~2 hour；Then gained glass melt is toppled over Rapid compressing on metal copper mold, anneal 3h at 350 DEG C, obtains transparent forerunner's glass；Hot place is carried out to forerunner's glass again Reason, obtains transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass.
8. preparation method as claimed in claim 7, it is characterised in that the heat treating regime is at a temperature of 550~700 DEG C Insulation 1~3 hour.
CN201710296209.0A 2017-04-28 2017-04-28 A kind of transparent rare earth ion doped six sides yttrium fluoride natrium fluorine oxygen devitrified glass and preparation method thereof Pending CN106946462A (en)

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Cited By (6)

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CN108409148A (en) * 2018-03-15 2018-08-17 杭州电子科技大学 The upper conversion NaLuF of infrared incoherent LED excitations4Glass ceramics and preparation method thereof
CN108975714A (en) * 2018-08-29 2018-12-11 华南理工大学 A kind of double-energy light-converting glass and preparation method thereof promoting photosynthesis of plant
CN110204209A (en) * 2019-05-08 2019-09-06 杭州电子科技大学 A kind of upper conversion glass ceramic composite material of the rear-earth-doped scandium base fluorinated nano crystalline substance of selectivity
CN115010371A (en) * 2022-06-07 2022-09-06 宁波大学 High-crystallinity intermediate infrared luminescent nano glass ceramic material and preparation method thereof
CN116730621A (en) * 2023-05-30 2023-09-12 华南理工大学 Rare earth doped fluorine oxygen microcrystalline glass with high crystallinity and transparency and preparation method thereof
CN116730621B (en) * 2023-05-30 2024-05-10 华南理工大学 Rare earth doped fluorine oxygen microcrystalline glass with high crystallinity and transparency and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108409148A (en) * 2018-03-15 2018-08-17 杭州电子科技大学 The upper conversion NaLuF of infrared incoherent LED excitations4Glass ceramics and preparation method thereof
CN108409148B (en) * 2018-03-15 2020-11-06 杭州电子科技大学 Infrared incoherent LED excited upconversion NaLuF4Glass-ceramic and method for producing the same
CN108975714A (en) * 2018-08-29 2018-12-11 华南理工大学 A kind of double-energy light-converting glass and preparation method thereof promoting photosynthesis of plant
CN110204209A (en) * 2019-05-08 2019-09-06 杭州电子科技大学 A kind of upper conversion glass ceramic composite material of the rear-earth-doped scandium base fluorinated nano crystalline substance of selectivity
CN110204209B (en) * 2019-05-08 2022-01-04 杭州电子科技大学 Up-conversion glass ceramic composite material of selective rare earth doped scandium-based fluorinated nanocrystalline
CN115010371A (en) * 2022-06-07 2022-09-06 宁波大学 High-crystallinity intermediate infrared luminescent nano glass ceramic material and preparation method thereof
CN115010371B (en) * 2022-06-07 2023-07-14 宁波大学 High-crystallinity mid-infrared luminous nano glass ceramic material and preparation method thereof
CN116730621A (en) * 2023-05-30 2023-09-12 华南理工大学 Rare earth doped fluorine oxygen microcrystalline glass with high crystallinity and transparency and preparation method thereof
CN116730621B (en) * 2023-05-30 2024-05-10 华南理工大学 Rare earth doped fluorine oxygen microcrystalline glass with high crystallinity and transparency and preparation method thereof

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