CN110054415A - A kind of up-conversion luminescence nano-glass ceramic material and preparation method thereof based on Yb-Mn dimer - Google Patents

A kind of up-conversion luminescence nano-glass ceramic material and preparation method thereof based on Yb-Mn dimer Download PDF

Info

Publication number
CN110054415A
CN110054415A CN201910232253.4A CN201910232253A CN110054415A CN 110054415 A CN110054415 A CN 110054415A CN 201910232253 A CN201910232253 A CN 201910232253A CN 110054415 A CN110054415 A CN 110054415A
Authority
CN
China
Prior art keywords
glass
dimer
ceramic material
conversion luminescence
glass ceramic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910232253.4A
Other languages
Chinese (zh)
Inventor
刘雪云
程翠梅
曾娜
焦清
林常规
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ningbo University
Original Assignee
Ningbo University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ningbo University filed Critical Ningbo University
Priority to CN201910232253.4A priority Critical patent/CN110054415A/en
Publication of CN110054415A publication Critical patent/CN110054415A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00Annealing glass products
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00Thermal 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
    • C03B32/02Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C10/00Devitrified 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
    • C03C10/16Halogen containing crystalline phase
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C4/00Compositions for glass with special properties
    • C03C4/12Compositions for glass with special properties for luminescent glass; for fluorescent glass
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C2214/00Nature of the non-vitreous component
    • C03C2214/20Glass-ceramics matrix
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C2214/00Nature of the non-vitreous component
    • C03C2214/30Methods of making the composites

Abstract

The invention discloses a kind of up-conversion luminescence nano-glass ceramic material and preparation method thereof based on Yb-Mn dimer, feature are that its molar percentage composition includes: SiO240%, Al2O320%, Ga2O310%, LiF 15%, YF315%, molar concentration of the dopant containing manganese compound is 0 ~ 1.5%, and the molar concentration containing ytterbium compound is that 0 ~ 1%, SnO doping molar concentration is 0.5%, preparation method prepares Yb using twin crystal phase nano-glass ceramics as host material, using melting-quenching-annealing-heat treating process3+‑Mn2+Dimer up-conversion luminescence biphase glass ceramic material, advantage are by changing Mn2+Doping content and heat treatment temperature, it can be achieved that the broad emission band of 450 nm to 750 nm emits, while the material has very higher mechanical strength, good chemical stability and higher transparency.

Description

A kind of up-conversion luminescence nano-glass ceramic material based on Yb-Mn dimer and its Preparation method
Technical field
The present invention relates to a kind of nano-glass ceramic composites, are formed more particularly, to one kind based on aggregation coupling Yb-Mn dimer up-conversion luminescence nano-glass ceramic material and preparation method thereof.
Background technique
In recent years, up-conversion luminescent material is due in solar battery, biological fluorescent labelling, Three-dimensional Display and the neck such as anti-fake Domain shows wide application prospect, it has also become one of the forward position of current illumination field and hot spot.Swashing in such current material Center living depends on rare earth ion.However, the intrinsic narrow emission of rare earth ion, emission peak are fixed and multi-peak emission is special Property limits the development for mixing rare earth up-conversion luminescent material to a certain extent.Find the novel efficient upper conversion material without rare earth Material is particularly important.Compared with rare earth ion, transition metal ions has wideband adjustable emission characteristics.Wherein bivalent manganese from Sub- Mn2+All the time because its luminous advantage outstanding is even more to be widely used in illumination and display field.Utilize Yb3+/Mn2+ Being co-doped with and obtaining the visible up-conversion luminescence of room temperature in same material is a kind of new up-conversion luminescence phenomenon reported in recent years. South China Science & Engineering University Zhang Qinyuan professor is in " perovskite KZnF within 20133:Yb3+/Mn2+The adjustable up-conversion luminescence of temperature-independent " (Temperature-tunable upconversion luminescence of perovskite nanocrystals KZnF3:Yb3+/Mn2+, Advanced Optical Materials. 2013;1:4209-4215) reported for the first time in a text Mn2+Converted wideband shines on 585 nm, and proposes the Mn in the system2+With Yb3+Certain is formd by assembling coupling The special centre of luminescence --- the Yb of kind3+-Mn2+Dimer.This centre of luminescence can either efficiently absorb 980 nm LD of commercialization Pump light, while Mn can be presented again2+Characteristic emission, finally obtain broadband, the room temperature up-conversion luminescence that peak position is tunable, be expected to The spectrum for making up rare earth ion is insufficient, widens the application range of up-conversion luminescent material.However, can be realized Yb at present3+-Mn2+ The system of dimer room temperature up-conversion luminescence is not much and nearly all concentrates in powder or nano material, in other materials, such as Research in transparent optical material rarely has development, it is necessary to expand its matrix species.
Glass ceramics, also known as devitrified glass are obtained by control parent glass nucleation and crystallization by nanometer crystal phase With a kind of composite material of glass phase composition.This kind of material had not only had nanocrystal close or even superior luminescent properties, but also There are the good mechanical strength and chemical stability similar to glass phase.With transparent single crystal and ceramic phase ratio, technology of preparing is simple, It is low in cost, easy to process, and adulterate light emitting ionic can priority enrichment in nanometer crystal phase, reduce radiationless relaxation probability, To improve luminous efficiency.In addition, compared to nano-powder material, transparent glass ceramics possesses high temperature resistant, wet-heat resisting, firm resistance to With, good light stability and the advantage outstanding such as more environmentally friendly.Therefore, transparent glass ceramics future very likely substitutes traditional glass The materials such as glass, powder, ceramics become the host material that first entering light functional area most has application value.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to be able to achieve Yb3+-Mn2+In the room temperature for assembling coupling Converted wideband, tunable luminous up-conversion luminescence nano-glass ceramic material and preparation method thereof, preparation method collection simplicity, Efficiently and energy conservation is in one.
The technical scheme of the invention to solve the technical problem is: a kind of upper conversion based on Yb-Mn dimer Illuminant nanometer glass ceramic material, glass ceramic substrate molar percentage composition includes: SiO240%, Al2O320%, Ga2O3 10%, LiF 15%, YF315%, molar concentration of the dopant containing manganese compound is 0 ~ 1.5%, and the molar concentration containing ytterbium compound is The molar concentration of 0 ~ 1%, antioxidant SnO are 0.5%.SnO is for preventing Mn in melting process2+Oxidation.
Preferably, described is MnCO containing manganese compound3, described is YbF containing ytterbium compound3。MnCO3It is a kind of dry It is stable in dry air to contain manganese compound, it is decomposed when heated, energy needed for the manganese oxide compounds than melting equivalent is less.Cause This preferred MnCO containing manganese compound3;Similarly, Yb is compared2O3, the fluoride YbF of introducing3Fusing point is lower, and melting effect is more preferable, institute The melting energy needed is less;For adding the glass of LiF component, LiF can reduce glass melting temperature as fluxing agent.Therefore This programme has good energy-saving effect.In addition the SnO for introducing 0.5% prevents divalent manganesetion in melting process to be oxidized to height Valence manganese ion (such as Mn3+、Mn5+、 Mn7+) lose its fluorescent characteristic.
The preparation method of the above-mentioned up-conversion luminescence nano-glass ceramic material based on Yb-Mn dimer, including following step It is rapid:
(1) raw material preparation: raw material proportioning according to claim 1 or 2 weighs various raw materials and grinds in the agate mortar 20g mixture uniformly is obtained, is carefully transferred to corundum crucible;
(2) melting and quenching: corundum crucible being placed in chamber type electric resistance furnace and be melted, and melting temperature is 1450 DEG C, and the melting time is 60 minutes, then fusant is poured on the preheated stainless steel plate to 300 DEG C, and is quickly suppressed with another block of preheating steel plate To complete During Quenching, solid block glass is obtained;
(3) it anneals: solid block glass being put into annealing furnace and is annealed, annealing temperature is 550 DEG C, and annealing time is 3 small When, 30 DEG C finally are down to 25 ~ 35 DEG C/h of rate of temperature fall, has obtained eliminating internal stress machining property good Presoma glass;
(4) it is heat-treated: glass precursor being cut into the good glass sample of shape, size and is heat-treated, heat treatment temperature is 750 ~ 770 DEG C, heat treatment time is 2 hours, is finally down to 30 DEG C with 40 ~ 55 DEG C/h of rate of temperature fall to get to both containingγ-Ga2O3Contain againβ-YF3Biphase glass ceramic material, finally nano-glass ceramics are processed by shot blasting to obtain shape Shape, size it is unified based on Yb3+-Mn2+The up-conversion luminescence nano-glass ceramic material of dimer.
Compared with the prior art, the advantages of the present invention are as follows: the present invention is a kind of to be based on Yb3+-Mn2+The upper conversion of dimer Illuminant nanometer glass ceramic material and preparation method thereof is successfully precipitated two kinds by control glass ingredient in devitrified glass The nanocrystal (as shown in TEM, there are big overlappings between two kinds of nanocrystals) of close proximity, this makes in Yb3+-Mn2+Altogether It mixes in two-phase devitrified glass to form Yb3+-Mn2+A possibility that dimer centre of luminescence, shines to form upper converted wideband. It is analyzed by spectrum test, it was confirmed that form Yb in two-phase devitrified glass3+-Mn2+The dimer centre of luminescence.And pass through It is preferred that the gallium oxide that spinel structure in glass matrix while is precipitated may be implemented in glass ingredient and control heat treatment temperature (γ-Ga2O3) and orthohormbic structure yttrium fluoride (β-YF3) nanocrystalline.Y3+Ionic radius and Yb3+The radius of ion is very close, Therefore having preferable solid solubility to this rare earth ion, (ionic radius is close, and ion is easily accessible in the crystal phase, crystalline environment Effect is improved to ionoluminescence).It is rich in materialγ-Ga2O3Withβ-YF3It is transient metal Mn that two kinds nanocrystalline2+It provides Lower phonon energy environment, advantageously reduces radiationless transition probability, to improve luminous efficiency.Moreover, Mn2+Glow peak It is strongly depend on locating surrounding's local environment, by adjusting Mn2+Crystalline field environment can realize the regulation to its spectrum.
In conclusion a kind of up-conversion luminescence nano-glass ceramic material and its system based on Yb-Mn dimer of the present invention Preparation Method prepares Yb using melting-quenching-annealing-heat treating process using twin crystal phase nano-glass ceramics as host material3+- Mn2+Dimer up-conversion luminescence biphase glass ceramic material, the glass precursor that this method is prepared have good processing Performance;Energy quick crystallization when crystallization and thermal treatment, andγ-Ga2O3Withβ-YF3The low phonon energy environment of biphase nanocrystalline can mention High Mn2+Up-conversion luminescence efficiency.The great advantage of this method is can to continue to use the forming method of any glass, is such as rolled, Compacting is blown, and is drawn, and casting etc. is more suitable for automatic operation and prepares complex-shaped, accurate in size product, is a kind of collection Easy, the efficient and energy saving preparation method in one.Yb of the present invention3+-Mn2+Dimer up-conversion luminescence biphase glass pottery Ceramic material, not only mechanical strength with higher, good chemical stability and higher transparency etc., while also showing face The adjustable wide spectrum up-conversion luminescence of color.Test result shows by adjusting Mn2+Doping concentration and heat treatment temperature, can be with The relative intensity for changing double transmitting broadbands centered on ~ 515 and ~ 605nm, realizes Yb3+-Mn2+Dimer biphase glass The Color tunable up-conversion luminescence of ceramics, the broad-band illumination light source of Color tunable can be used for illuminating, show, is anti-fake, tunable The fields such as laser.
Detailed description of the invention
Fig. 1 be embodiment 1-9 XRD spectrum andγ-Ga2O3Withβ-YF3Nanocrystalline standard diffraction card, standard are spread out Penetrate the vertical bar shape pattern that card refers to bottom end in XRD diagram;
(a) is that the TEM of embodiment 5 schemes in Fig. 2, is (b) (a) corresponding SEAD figure, (c) isγ-Ga2O3Withβ-YF3Nanocrystalline HRTEM figure is (d) the UV-NIR absorption spectrum of glass precursor and glass ceramics, is (e) photo under corresponding fluorescent lamp;
(a) is the up-conversion luminescence spectrum of the sample for preparing under 980 nm excitation at a temperature of different heat treatment in Fig. 3, (b) is Different Mn2+Up-conversion luminescence spectrum of the sample prepared under ion doping concentration under 980 nm excitation;
Fig. 4 be up-conversion luminescence nano-glass ceramic material excitation and emission spectra, wherein (a) be GC760-M, (b) be GC760-YM1.5 (c) is GC760-Y;
Fig. 5 is Yb3+-Mn2+The upconversion luminescence mechanism figure of dimer biphase glass ceramic material.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
One, specific embodiment
A kind of up-conversion luminescence nano-glass ceramic material based on Yb-Mn dimer, glass ceramic substrate molar percentage Composition includes: SiO240%, Al2O320%, Ga2O310%, LiF 15%, YF315%, dopant is mole dense containing manganese compound Degree is 0 ~ 1.5%, and the molar concentration containing ytterbium compound is 0 ~ 1%, and the molar concentration of antioxidant SnO is 0.5%, wherein containing manganese Conjunction object is MnCO3, it is YbF containing ytterbium compound3, preparation method includes the following steps:
1) raw material preparation: getting out various raw materials according to raw material proportioning and be uniformly mixed, wherein difference Mn2+Ions dosage and Heat treatment temperature is shown in Table 1;
2) melting, quenching are from annealing: by uniformly mixed various different Mn2+The raw material of ion doping concentration carries out high temperature respectively Melting, melting temperature are 1500 DEG C, and the melting time is 60 minutes, and fusant is then poured into preheated 300 DEG C of stainless steel plate Above and quickly with another piece of preheating steel plate compacting to complete During Quenching, the solid glass is put into annealing furnace carries out later Annealing, annealing temperature are 550 DEG C, and annealing time is 3 hours, are down to room temperature with 25 ~ 35 DEG C/h of rate of temperature fall, obtain Eliminate the presoma glass of internal stress;
3) it is heat-treated: the glass precursor after annealing is heat-treated, heat treatment temperature is 750 DEG C ~ 770 DEG C, heat treatment time It is 2 hours, room temperature is finally down to 40 ~ 55 DEG C/h of rate of temperature fall to get each embodiment Yb is arrived3+-Mn2+Turn on dimer Change light biphase glass ceramic material, the specific heat treatment temperature of embodiment 1 ~ 9 and time and Mn2+And Yb3+Ion is mixed Miscellaneous concentration is shown in Table 1.
The 04/16 type chamber type electric resistance furnace of LHT that above-mentioned melting plant used is manufactured by German Na Bore company.It uses For raw material respectively from Aladdin and traditional Chinese medicines company, purity is 99.99%.Annealing and heat treatment are all made of German Na Bore company The LT 5/11/P330 type annealing furnace of manufacture.
Title, raw material and proportion, the heat treatment temperature/time of 1 each sample of table
Two, analysis of experimental results
Yb-Mn dimer up-conversion luminescence biphase glass ceramics prepared in the above embodiments is tested for the property, Fig. 1 is The XRD spectrum of above-described embodiment andγ-Ga2O3Withβ-YF3Nanocrystalline standard diffraction card.By carefully comparing discovery institute Each diffraction maximum of the sample of preparation respectively withγ-Ga2O3Withβ-YF3Standard card it is corresponding, illustrate prepared embodiment 2 ~ 5 and embodiment 7 ~ 9 be to have bothγ-Ga2O3Withβ-YF3Nanocrystalline target substance --- biphase glass ceramics.Embodiment 1 is simple glass, and embodiment 6 is to compare other embodiments compared with low heat-treatment temperature (750 degree), which does not analyse simultaneously Out two kinds it is nanocrystalline.
(a) is that the TEM of embodiment 5 schemes in Fig. 2, is (b) (a) corresponding SEAD figure, (c) isγ-Ga2O3Withβ-YF3Nanometer Brilliant HRTEM figure is (d) the UV-NIR absorption spectrum of glass precursor and glass ceramics, is (e) photo under corresponding fluorescent lamp. By Fig. 2 a it is found that two kinds of nanocrystals coexist in glass matrix, it is consistent with Fig. 1 result.The selective electron diffraction (SAED) of Fig. 2 b Pattern shows discrete polycrystalline diffraction ring, it was confirmed that has crystal precipitation in glass matrix.Fig. 2 c givesγ-Ga2O3Withβ- YF3Nanocrystalline high resolution transmission electron microscopy (HRTEM) image, two kinds of nanocrystalline spacing and crystal growth direction difference Indicated by red line and yellow line, lattice fringe spacing measures respectively 0.174nm and 0.208nm, by contrast, discovery withβ-YF3's (212) face andγ-Ga2O3(400) face be well matched with.This further explanation is successfully prepared biphase glass ceramics.Figure 2d shows the optical absorption spectra of UV-NIR.Observe that typical absorption peak, this attribution occur at ~ 980nm in all samples In Yb3+:2F7/22F5/2Transition, and Yb3+Absorption peak do not show significant changes after heat treatment.This is because Yb3+ 'sf-fTransition is by outer-shell electron5s 2 p 6 Shielding.In addition, the increase of heat treatment temperature will lead to the increase of nanocrystalline content. It is worth noting that, nanocrystalline changes of contents directly affects transparency of the glass material in visible-range.Therefore, embodiment 7 keep good transparency unlike other embodiments, such as the photo institute of sample under the illustration and Fig. 2 e fluorescent lamp in Fig. 2 d Show.
The up-conversion luminescence spectrum of (a) for product obtained at a temperature of different heat treatment under 980 nm excitation in Fig. 3, It (b) is different Mn2+The up-conversion luminescence spectrum of product obtained under 980 nm excitation under ion doping concentration.As seen from the figure, Embodiment 2 ~ 7 is made of 450 to the 750nm transmitting broadband centered on ~ 515 or ~ 605nm, and this phenomenon is attributed to Yb3 +-Mn2+Dimer |2F7/2,4T1(4G)>→| 2F7/2,6A1(6S) > transition is located at tetrahedron and octahedral ligand ring Border, an only wide orange emission band in embodiment 1.Orange emission gradually increases with the raising of heat treatment temperature in Fig. 3 a By force, this is because the nanocrystalline content being precipitated increases, non-radiative probability is reduced, orange luminescence enhancing.Orange emission is strong in Fig. 3 b Degree is with Mn2+Concentration increase shows monotone increasing, and green emitted intensity is in Mn2+Concentration value be 1.5mol% before it is aobvious Show monotone increasing.With Mn2+Concentration reach 1.5mol%, due to concentration quenching effect, green emitted is slightly reduced.It can infuse It anticipates and arrives, in Mn2+The lower situation of concentration under, green emitted is dominant.This shows by controlling Mn2+Concentration can be with Adjust up-conversion luminescence color.Importantly, the up-conversion luminescence obtained is quite strong, even if in low-down pump power laser It can also be observed by the naked eye under excitation (0.5W).
(a) is excitation and the transmitting map of embodiment 8 in Fig. 4, is (b) excitation of embodiment 5 and transmitting map, (c) is The excitation of embodiment 9 and transmitting map.As shown in fig. 4 a, under 445 nm excitation, the visible emission band of embodiment 8 is very similar Switching emission band thereon.Therefore, further confirm that Up-conversion emission band is originated from Yb3+-Mn2+Dimer is located at tetrahedron With octahedral ligand environment |2F7/2,4T1(4G)>→| 2F7/2,6A1(6S) > transition.In fig. 4b, embodiment 5 is shown Two additional near infrared emission bands, this is attributed to Yb3+:2F7/22F5/2Transition, referring to fig. 4 c.What is monitored at 976nm swashs Luminous spectrum is similar to the excitation spectrum (see Fig. 4 a) of embodiment 8, shows in Yb3+-Mn2+Dimer up-conversion luminescence biphase In glass ceramic material, by exciting Mn2+Yb can be excited indirectly3+.The process belongs to from Mn2+To Yb3+Height non-resonance energy Amount transmitting, because of Mn2+With Yb3+Between without spectra overlapping.According to the above analysis, Yb as shown in Figure 5 is given3+-Mn2+Dimerization The upconversion luminescence mechanism figure of body biphase glass ceramic material.
Above description is not limitation of the present invention, and the present invention is also not limited to the example above.The art it is common Within the essential scope of the present invention, the variations, modifications, additions or substitutions made also should belong to protection of the invention to technical staff Range.

Claims (3)

1. a kind of up-conversion luminescence nano-glass ceramic material based on Yb-Mn dimer, it is characterised in that its glass ceramics base Matter molar percentage composition includes: SiO240%, Al2O320%, Ga2O310%, LiF 15% and YF315%, dopant contains manganese The molar concentration for closing object is 0 ~ 1.5%, and the molar concentration containing ytterbium compound is 0 ~ 1%, and the molar concentration of antioxidant SnO is 0.5%。
2. a kind of up-conversion luminescence nano-glass ceramic material based on Yb-Mn dimer according to claim 1, special Sign is: described is MnCO containing manganese compound3, described is YbF containing ytterbium compound3
3. a kind of preparation of the up-conversion luminescence nano-glass ceramic material of any of claims 1 or 2 based on Yb-Mn dimer Method, it is characterised in that the following steps are included:
(1) raw material preparation: raw material proportioning according to claim 1 or 2 weighs various raw materials and grinds in the agate mortar 20g mixture uniformly is obtained, is carefully transferred to corundum crucible;
(2) melting and quenching: corundum crucible being placed in chamber type electric resistance furnace and be melted, and melting temperature is 1500 DEG C, and the melting time is 60 minutes, then fusant is poured on the preheated stainless steel plate to 300 DEG C, and is quickly suppressed with another block of preheating steel plate To complete During Quenching, solid block glass is obtained;
(3) it anneals: solid block glass being put into annealing furnace and is annealed, annealing temperature is 550 DEG C, and annealing time is 3 small When, 30 DEG C finally are down to 25 ~ 35 DEG C/h of rate of temperature fall, has obtained eliminating internal stress machining property good Presoma glass;
(4) it is heat-treated: glass precursor being cut into the good glass sample of shape, size and is heat-treated, heat treatment temperature is 750 ~ 770 DEG C, heat treatment time is 2 hours, is finally down to 30 DEG C with 40 ~ 55 DEG C/h of rate of temperature fall to get to both containingγ-Ga2O3Contain againβ-YF3Biphase glass ceramic material, finally nano-glass ceramics are processed by shot blasting to be based on The up-conversion luminescence nano-glass ceramic material of Yb-Mn dimer.
CN201910232253.4A 2019-03-26 2019-03-26 A kind of up-conversion luminescence nano-glass ceramic material and preparation method thereof based on Yb-Mn dimer Pending CN110054415A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910232253.4A CN110054415A (en) 2019-03-26 2019-03-26 A kind of up-conversion luminescence nano-glass ceramic material and preparation method thereof based on Yb-Mn dimer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910232253.4A CN110054415A (en) 2019-03-26 2019-03-26 A kind of up-conversion luminescence nano-glass ceramic material and preparation method thereof based on Yb-Mn dimer

Publications (1)

Publication Number Publication Date
CN110054415A true CN110054415A (en) 2019-07-26

Family

ID=67315965

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910232253.4A Pending CN110054415A (en) 2019-03-26 2019-03-26 A kind of up-conversion luminescence nano-glass ceramic material and preparation method thereof based on Yb-Mn dimer

Country Status (1)

Country Link
CN (1) CN110054415A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110590162A (en) * 2019-10-23 2019-12-20 中国科学院福建物质结构研究所 Nanocrystalline transparent glass ceramic for multidimensional optical storage and preparation method thereof
CN113087397A (en) * 2021-04-13 2021-07-09 泰山学院 Double-phase transparent glass ceramic with ultra-wideband fluorescence emission characteristic and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006062448A1 (en) * 2006-12-28 2008-07-10 Schott Ag Photovoltaic module with thin electrode- and silicon layers, for solar energy collection, includes high-refraction glass or glass-ceramic converter plate containing specified dopants
CN103922584A (en) * 2014-03-20 2014-07-16 华东理工大学 Transition metal ion co-doped ultraviolet-excited adjustable luminescent glass and preparation method thereof
CN105481250A (en) * 2015-12-04 2016-04-13 哈尔滨工程大学 Colorless transparent glass-ceramic with long after-glow down-conversion luminescence characteristics and preparation method thereof
CN106947483A (en) * 2017-04-11 2017-07-14 武汉理工大学 A kind of additive Mn lithium yttrium fluoride upconverting fluorescent material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006062448A1 (en) * 2006-12-28 2008-07-10 Schott Ag Photovoltaic module with thin electrode- and silicon layers, for solar energy collection, includes high-refraction glass or glass-ceramic converter plate containing specified dopants
CN103922584A (en) * 2014-03-20 2014-07-16 华东理工大学 Transition metal ion co-doped ultraviolet-excited adjustable luminescent glass and preparation method thereof
CN105481250A (en) * 2015-12-04 2016-04-13 哈尔滨工程大学 Colorless transparent glass-ceramic with long after-glow down-conversion luminescence characteristics and preparation method thereof
CN106947483A (en) * 2017-04-11 2017-07-14 武汉理工大学 A kind of additive Mn lithium yttrium fluoride upconverting fluorescent material and preparation method thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
HANG LIN ET AL.: "Tuning of multicolor emissions in glass ceramics containing γ-Ga2O3 and β-YF3 nanocrystals", 《JOURNAL OF MATERIALS CHEMISTRY C》 *
XUEYUN LIU ET AL.: "Color-tunable Upconversion Luminescence in Yb3+/Mn2+ Codoped Dual-phase Glass Ceramics", 《第十届中国功能玻璃学术研讨会暨新型光电子材料国际论坛会议摘要集 工程科技I辑》 *
徐叙瑢主编: "《发光材料与显示技术》", 31 January 2003, 化学工业出版社 *
田英良等: "《新编玻璃工艺学》", 30 June 2009, 中国轻工业出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110590162A (en) * 2019-10-23 2019-12-20 中国科学院福建物质结构研究所 Nanocrystalline transparent glass ceramic for multidimensional optical storage and preparation method thereof
CN110590162B (en) * 2019-10-23 2022-04-19 中国科学院福建物质结构研究所 Nanocrystalline transparent glass ceramic for multidimensional optical storage and preparation method thereof
CN113087397A (en) * 2021-04-13 2021-07-09 泰山学院 Double-phase transparent glass ceramic with ultra-wideband fluorescence emission characteristic and preparation method thereof

Similar Documents

Publication Publication Date Title
Raju et al. The influence of sintering temperature on the photoluminescence properties of oxyapatite Eu3+: Ca2Gd8Si6O26 nanophosphors
Hu et al. Enhanced deep-red emission from Mn 4+/Mg 2+ co-doped CaGdAlO 4 phosphors for plant cultivation
Kaur et al. Color tunable photoluminescence properties in Eu3+ doped calcium bismuth vanadate phosphors for luminescent devices
Singh et al. Preparation and photoluminescence properties of SrAl 2 O 4: Eu 2+, RE 3+ green nanophosphors for display device applications
Bandi et al. Citric based sol-gel synthesis and photoluminescence properties of un-doped and Sm3+ doped Ca3Y2Si3O12 phosphors
Lei et al. Preparation and broadband white emission of Ce3+-doped transparent glass-ceramics containing ZnO nanocrystals for WLEDs applications
CN101418217A (en) Multiple colour infrared up-conversion luminous material and preparing process thereof
de Mayrinck et al. Reassessment of the potential applications of Eu3+-doped Y2O3 photoluminescent material in ceramic powder form
ZHANG et al. Luminescent properties of Ce3+/Tb3+ co-doped glass ceramics containing YPO4 nanocrystals for W-LEDs
Rai et al. Probing a new approach for warm white light generation in lanthanide doped nanophosphors
Hassan et al. Investigation of sintering temperature and Ce3+ concentration in YAG: Ce phosphor powder prepared by microwave combustion for white-light-emitting diode luminance applications
Xiaoxu et al. Synthesis of Y2O3 phosphor by a hydrolysis and oxidation method
CN110054415A (en) A kind of up-conversion luminescence nano-glass ceramic material and preparation method thereof based on Yb-Mn dimer
Leng et al. Impact of pH and urea content on size and luminescence of upconverting Y2O3: Yb, Er nanophosphors
Abd et al. Rapid synthesis of Ce3+: YAG via CO2 laser irradiation combustion method: Influence of Ce doping and thickness of phosphor ceramic on the performance of a white LED device
Zheng et al. Structure and spectroscopic properties of Tb3+/Sm3+ co-doped oxyfluoride glass ceramics containing LiYF4 nanocrystals
Lu et al. Fabrication and characterization of transparent (Y0. 98− xTb0. 02Eux) 2O3 ceramics with color‐tailorable emission
CN112457847A (en) Mn/Cr co-doped Li2MgAO4Near-infrared fluorescent powder and preparation method thereof
Wang et al. Fabrication of highly transparent Er3+, Yb3+: Y2O3 ceramics with La2O3/ZrO2 as sintering additives and the near-infrared and upconversion luminescence properties
Abd et al. Ce-doped YAG single-crystals prepared by continuous wave (CW)–CO2 laser combustion technique with attractive characteristics and moderate white LED performance
Zhang et al. Upconversion luminescence in Er-doped γ-AlON ceramic phosphors
Zhou et al. Concentration-dependent up-converted luminescence of Ho3+–Yb3+ co-doped yttrium-stabilized zirconia phosphors
CN113493688B (en) Near-infrared luminescent material and luminescent device containing same
CN102503139B (en) A kind of up-conversion luminous transparent glass ceramic and preparation method thereof
WO2022252400A1 (en) Near-infrared light-emitting substance and light-emitting device comprising same

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190726