CN112028479B - High-density high-Abbe number near-infrared luminescent glass - Google Patents

High-density high-Abbe number near-infrared luminescent glass Download PDF

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CN112028479B
CN112028479B CN202010805419.XA CN202010805419A CN112028479B CN 112028479 B CN112028479 B CN 112028479B CN 202010805419 A CN202010805419 A CN 202010805419A CN 112028479 B CN112028479 B CN 112028479B
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luminescent glass
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infrared luminescent
abbe number
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CN112028479A (en
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张明辉
刘希曼
刘学超
潘秀红
陈锟
邓伟杰
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Shanghai Institute of Ceramics of CAS
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • 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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Abstract

The invention discloses near-infrared luminescent glass with high density and high Abbe number. The near-infrared luminescent glass is rare earth ion doped heavy metal oxide luminescent glass and comprises the following components: in mole percent, La2O325-35% of Yb2O3Less than 10% of Er2O32-5% of Nb2O520-40% of Ga2O3Accounting for 30-50%.

Description

High-density high-Abbe number near-infrared luminescent glass
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to high-density high-Abbe number near-infrared luminescent glass.
Background
In recent years, rare earth ion doped luminescent glass attracts people's attention. Rare earth ion doped luminescent glasses have potential uses in infrared converters and upconversion short wavelength solid state lasers due to their upconversion properties from infrared to visible wavelengths. In addition, the application fields of the rare earth ion doped luminescent glass also relate to the aspects of high-density optical storage, optical fiber communication, three-dimensional display, food analysis, agricultural product analysis, pharmaceutical analysis, biomedicine and the like, wherein the advantages of the rare earth ion doped luminescent glass in the aspect of petrochemical industry are particularly obvious.
Er3+Besides excellent infrared amplification and laser emission performances, the energy level of the material is rich and uniformly distributed, single-beam pumping is facilitated, and the material has high quenching concentration. Such as using commercial 980nm and 808nm pump excitation4I15/2→4I11/2And4I15/2→4I9/2possibility of transition, so that Er3+Applications that convert from visible up-conversion to infrared luminescence are very attractive. To realize Er3+Most critical is the search for suitable host materials. In the studies reported so far, silicate glass, tellurate glass, chalcogenide glass and fluoride glass are mostly used as the matrix material. The maximum phonon energy of silicate glass is higher, which is not beneficial to improving the luminescence property of the glass. Tellurate glass has relatively low phonon energy, high refractive index and relatively high RE ion solubility, but relatively low stability and relatively high material cost. Chalcogenide glass has a large refractive index and a high infrared transmission limit, but the solubility of rare earth ions is low, and the requirement on the purity of raw materials is high. The fluoride glass has low phonon energy, good rare earth ion dissolving capacity and low OH-Absorption, but the preparation process is complicated, the chemical stability is poor, the mechanical property is poor, and the thermal conductivity is low, which brings great challenges for expanding the commercial production application of fluoride glass.
In terms of the preparation method, the raw material components of tellurate glass, silicate glass and chalcogenide glass have strong glass forming capability, so that the tellurate glass, the silicate glass and the chalcogenide glass can be prepared by adopting a traditional quenching annealing mode. However, heavy metal oxide glasses are less formable and therefore the quench annealing method is not suitable for making heavy metal oxide based glasses.
Disclosure of Invention
The invention mainly aims to provide the high-density high-Abbe number near-infrared luminescent glass which effectively solves the problems of poor stability, large dispersion, low cost and the like of the traditional infrared luminescent glass,Low density, poor machinability, low maximum phonon energy, compact structure and high Er concentration3+And the doped glass also has stronger machinability and thermal stability, which lays a foundation for the practical application of the glass.
In a first aspect, the present invention provides a high-density high-abbe-number near-infrared luminescent glass. The near-infrared luminescent glass is rare earth ion doped heavy metal oxide luminescent glass and comprises the following components: in mole percent, La2O325-35% of Yb2O3Less than 10% of Er2O32-5% of Nb2O520-40% of Ga2O3Accounting for 30-50%. Wherein, La2O3、Nb2O5And Ga2O3As a host of luminescent glass, Er2O3And Yb2O3As a light-emitting functional component of the luminescent glass.
Luminescent glass (may also be referred to as "LNG glass" or "La") of the present invention2O3-Nb2O5-Ga2O3Heavy metal glass ") using heavy metal oxide La2O3、Nb2O5And Ga2O3As a matrix, the glass matrix has lower phonon energy, and the nonradiative transition of excitons can be reduced. Selecting La2O3、Nb2O5And Ga2O3The three oxides are taken as matrixes, so that the luminescent glass of the invention not only has La-like2O3-Ga2O3Lower maximum phonon energy of glass, and also has La-like2O3-Nb2O5High refractive index of glass. In addition, the present invention is characterized by adding Yb to the above-mentioned heavy metal matrix material2O3The refractive index of the glass can be improved, and the near-infrared luminescence property of the rare earth doped glass can be optimized. The size, electronic structure and the like of the rare earth oxide of the matrix material are similar to those of the rare earth luminescent ions, and a suitable environment can be provided for the rare earth luminescent ions, so that the matrix material can provide a suitable environment for the rare earth luminescent ionsThe luminous intensity is improved.
When white light enters a transparent material, a dispersion phenomenon occurs. For optical material applications, it is often desirable for the material to have a low dispersion coefficient. However, the larger the refractive index value of the material, the larger the dispersion coefficient tends to be, and these two optical properties of the material are contradictory and restrictive. The abbe number can be used to characterize the degree of dispersion of the optical glass. The larger the Abbe number, the smaller the dispersion ability. The near-infrared luminescent glass has high refractive index, ndThe value is not less than 2.02, the Abbe number is between 27 and 60, and the optical material is an excellent optical material.
In addition, the near-infrared luminescent glass also has excellent mechanical properties, and the density is 5.2504-5.817g/cm3The micro Vickers hardness is not less than 8.42 GPa. The high density of glass makes it possible to enhance the radiation resistance, which is very effective in reducing the radiation loss of the detector and thus in extending the lifetime and in enabling its application in high-energy physics.
The thermal property of the near-infrared luminescent glass is good. In some embodiments, the glass transition temperature of the near-infrared luminescent glass is 790-800 ℃, and the crystallization starting temperature is 860-930 ℃.
Preferably, the transmittance of the near-infrared luminescent glass in an infrared region is more than 60%.
In a second aspect, the present invention provides a method for preparing the above luminescent glass with high density and high abbe number, comprising the following steps:
(1) with La2O3、Yb2O3、Er2O3、Nb2O5And Ga2O3Weighing raw materials according to the composition of the near-infrared luminescent glass and mixing to form a mixture;
(2) forming the mixture to obtain a prefabricated body;
(3) the method comprises the following steps of (1) enabling a prefabricated body to be in a container-free suspension state by using a gas suspension method, and melting the prefabricated body into a uniform and stable melt by using laser;
(4) and after the laser melting is finished, turning off the laser to cool and solidify the melt so as to form the solid near-infrared luminescent glass with high density and high Abbe number.
Preferably, the pre-sintering and heat preservation are carried out for 8-10 hours at the temperature of 900-1000 ℃ before the molding.
Preferably, the molding is followed by sintering and heat preservation at 1100-1200 ℃ for 11-12 hours to obtain a preform.
Preferably, the molding is tablet molding. Preferably, the tablet forming is performed under an air atmosphere. The pressure of the tablet can be 4-8 MPa.
Preferably, the power of the laser is 40-85W, and the holding time is 3-4 min.
The preparation method has the characteristics of low cost, no need of subsequent processing, novel preparation method, simple and convenient operation flow, contribution to large-scale production and the like. The high-density high-Abbe number near-infrared luminescent glass obtained by the preparation method not only has high Abbe number and higher transmittance, but also has good mechanical strength, thermal stability and lower phonon energy, has unique advantages in the aspects of food analysis, agricultural product analysis, pharmaceutical analysis, biomedicine and the like, is widely applied, and has particularly remarkable advantages in the aspect of petrochemical industry. In addition, the preparation process can be used for developing novel inorganic functional materials and metastable phase structures, such as magnetic functional materials, high dielectric constant materials and the like.
In a third aspect, the present invention provides a substrate formulation suitable for use in a near-infrared luminescent glass, comprising: in mole percent, La2O325-35% of Nb2O520-40% of Ga2O3Accounting for 30-50%. The abbe number of the blank glass obtained by the formula can reach 85.
Drawings
FIG. 1 is a pictorial representation of a near infrared luminescent glass prepared in examples 1-5;
FIG. 2 is a graph of refractive index of near-infrared luminescent glasses prepared in examples 1 to 5;
FIG. 3 is a DTA curve of the near-infrared luminescent glasses prepared in examples 1-5;
FIG. 4 is a graph showing the transmittance in the infrared region as a function of incident wavelength for near-infrared luminescent glasses prepared in examples 1 to 5;
FIG. 5 shows the near-infrared emission spectra of the near-infrared luminescent glasses prepared in examples 2 to 5 under the excitation of laser light at 980 nm.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative of, and not restrictive on, the present invention.
The following is an exemplary description of the method for preparing the high-density high-abbe-number near-infrared luminescent glass according to the present invention.
The components of the near-infrared luminescent glass are weighed according to mole percentage. The near-infrared luminescent glass is rare earth ion doped heavy metal oxide luminescent glass, and comprises the following components: in mole percent, La2O325-35% of Yb2O3Less than 10% of Er2O32-5% of Nb2O520-40% of Ga2O3Accounting for 30-50%. In the above composition, La in the lanthanoid rare earth ion3+Does not emit light and is suitable for use as a host material. Ga2O3Is a component with low phonon energy and high thermal stability, and is beneficial to improving the luminescent property of the material. Tests prove that the composition is designed to be the proportion of the luminescent glass components with stable performance and preparation process. When Ga is2O3Too high a proportion, the melt is very unstable when the sample is prepared and glass formation is not possible. Preferably Yb2O3Less than 7.5% of Er2O35% by weight of Nb2O520% of Ga2O3Accounting for 40 percent.
As a most preferred embodiment, the luminescent glass has the formula: in mole percent, xYb2O3-5Er2O3-(35-x)La2O3-20Nb2O5-40Ga2O3. Wherein x is more than or equal to 0 and less than or equal to 15. Preferably 0. ltoreq. x.ltoreq.10.
Specifically, La2O3、Yb2O3、Er2O3、Nb2O5And Ga2O3Weighing the materials according to the molar ratio, and fully mixing to form a mixture. Mixing may be performed by wet milling using alcohol as a dispersion medium.
The mix is prefired to remove some of the organic impurities. For example, the pre-sintering and heat preservation are carried out at 900-1000 ℃ for 8-10 hours.
And molding the pre-sintered material to obtain a preform. The shaping may be carried out under an air atmosphere. In some embodiments, the pressure may be 4 to 8 MPa. For example, by pressing into a cylindrical material using a tablet press.
And sintering the prefabricated body. For example, sintering at 1100-1200 deg.C for 11-12 hours.
And carrying out laser melting on the sintered preform by using a gas suspension technology. The gravity of the prefabricated body is counteracted through the buoyancy of the airflow, so that the prefabricated body is in a suspension state without a container, and meanwhile, the object is heated by utilizing laser to be melted. For example, the sintered preform is placed in a laser suspension furnace for laser melting. The laser power can be 40-85W, and the heat preservation time can be 3-4 min. The throat diameter of the nozzle is 0.5-3 mm. The laser is then turned off rapidly so that the melt resulting from the melting cools rapidly to form a solid glass. The solid glass may be in the shape of an ellipsoid or a sphere.
In the preparation process of the luminescent glass, the gas suspension technology can be used for avoiding the pollution of foreign impurities to the maximum extent, inhibiting heterogeneous nucleation and enabling the melt to be deeply overcooled so as to realize rapid solidification. Therefore, the heavy metal-based luminescent glass which has uniform components, high purity, less impurities and compact structure and cannot be obtained by the traditional method can be prepared.
In conclusion, the invention utilizes the gas suspension container-free technology to prepare Er3+/Yb3+The co-doped heavy metal glass has innovativeness and feasibility, and the prepared luminescent glass has the advantages of high refractive index, high thermal stability, excellent mechanical strength, high density, high Abbe number and the like.
The present invention is further illustrated by, but is not limited to, the following examples.
Example 1
Firstly according to the formula xYb2O3-5Er2O3-(35-x)La2O3-20Nb2O5-40Ga2O3Weighing the corresponding oxides, mixing, and wet-milling twice by using alcohol to obtain mixed powder. Presintering the mixed powder at 1000 ℃ for 10h in the air atmosphere, cooling along with a furnace, and tabletting to obtain a columnar body. Wherein the pressure for tablet forming is about 8 MPa. And then placing the columnar body in a high-temperature furnace, heating to 1200 ℃, and preserving heat for 12 hours to obtain a prefabricated body. And placing the preform in a laser suspension furnace, wherein the atmosphere is oxygen, and the laser power is about 75W, so that the preform is melted. And after the preform is completely melted to form a uniform and stable melt, closing the laser to solidify the melt under the condition of no container, thereby obtaining the ellipsoidal or spherical glass.
Table 1 test table for performance of luminescent glass of example 1
Figure BDA0002628945890000051
The composition of the blank glass is: in mole percent, 40La2O3-20Nb2O5-40Ga2O3. As can be seen from Table 1, Er was not doped3+And Yb3+The density of the blank glass sample is only 5.2504g/cm3(La2O3And Yb2O3Respectively has a density of 6.52g/cm3And 9.21g/cm3). The Abbe number of the blank LNG glass can reach 85, namely the LNG glass has a lower dispersion coefficient.
As can be seen from FIG. 1, Er is used in the present invention2O3And Yb2O3The high-density high-Abbe number near-infrared luminescent glass is prepared for luminescent functional components.
FIG. 2 is a graph showing the refractive index of the high-density high-Abbe number near-infrared luminescent glass prepared in examples 1 to 5 as a function of the incident wavelength. It can be seen that the refractive index values n at the helium yellow line (587.56nm) for examples 1-5dThe values are all larger than 2 and are higher than the refractive index of ZBLAN glass which is a traditional near-infrared luminescent fluoride material. The prepared near-infrared luminescent glass has the characteristic of high refractive index.
FIG. 3 is a DTA curve of the high density high Abbe number near infrared luminescent glasses prepared in examples 1-5. The DTA curve shows that the glass transition temperature of the sample is about 800 ℃, the crystallization starting temperature is 860 ℃ and 930 ℃, and the glass transition temperature is higher than the corresponding transition temperature of the ZBLAN glass of the traditional near-infrared luminescent fluoride material. This shows that the rare earth doped heavy metal oxide glass prepared by the invention has higher thermal stability.
FIG. 4 is a graph showing the transmittance in the infrared region as a function of incident wavelength for high-density, high-Abbe number near-infrared luminescent glasses prepared in examples 1 to 5. The transmittance curve shows that the sample is in the infrared region, except for 3500cm at 2000--1Due to OH-The absorption is reduced, and the transmittance is good. The result shows that the high-density high-Abbe number near-infrared luminescent glass prepared by the invention has good infrared transmittance, and the transmittance is more than 60%.
FIG. 5 is a graph showing the NIR emission spectra of high-density high-Abbe number NIR luminescent glasses prepared in examples 2-5 under laser excitation at 980 nm. In the spectrogram, the near infrared emission center is located at 1559nm, corresponding to Er3+Is/are as follows4I13/2→4I15/2And (4) transition.
Comparative example 1
Essentially the same as example 1, except that: the glass comprises the following components: 10% Yb2O3-(2-5％)Er2O3-(10-20％)La2O3-(20-30％)Nb2O5-(60-80％)Ga2O3. The composition produced samples were extremely unstable to the melt and failed to form glass because the composition itself had too little glass forming ability to form glass at the cooling rate of the air suspension process.

Claims (7)

1. The near-infrared luminescent glass is characterized by being heavy metal oxide luminescent glass doped with rare earth ions, and comprising the following components: in mole percent, La2O325-35% of Yb2O3Less than 10% of Er2O32-5% of Nb2O520-40% of Ga2O3Accounting for 30-50%.
2. The near-infrared luminescent glass according to claim 1, wherein La2O3、Nb2O5And Ga2O3As a host of luminescent glass, Er2O3And Yb2O3As a light-emitting functional component of the luminescent glass.
3. The near-infrared luminescent glass according to claim 1, characterized in that the composition of the near-infrared luminescent glass is: in mole percent, La2O325-35% of Yb2O3Less than 10% of Er2O35% by weight of Nb2O520% of Ga2O3Accounting for 40 percent.
4. The near-infrared luminescent glass according to claim 1, wherein the density of the near-infrared luminescent glass is 5.2504-5.817g/cm3The micro Vickers hardness is more than 8.42 GPa.
5. The near-infrared luminescent glass according to claim 1, wherein the refractive index n of the near-infrared luminescent glassdThe value is above 2.02 and the Abbe number is between 27 and 60.
6. A near-infrared luminescent glass in accordance with claim 1, wherein the near-infrared luminescent glass has a transmittance in the infrared region of 60% or more.
7. The near-infrared luminescent glass as claimed in claim 1, wherein the glass transition temperature of the near-infrared luminescent glass is 790-800 ℃, and the crystallization initiation temperature is 860-930 ℃.
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JP2016088761A (en) * 2014-10-29 2016-05-23 株式会社オハラ Infrared ray transmission glass, optical element and preform
CN108301046A (en) * 2018-03-14 2018-07-20 江苏海林电子新材料科技有限公司 A kind of optical crystal and its growing method of the preparation of large scale doped gallium lanthanum crystal
CN110452698A (en) * 2019-07-08 2019-11-15 惠州学院 A kind of visible light ultra wide band is sensitized near-infrared luminous fluorescent powder and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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JP2016088761A (en) * 2014-10-29 2016-05-23 株式会社オハラ Infrared ray transmission glass, optical element and preform
CN108301046A (en) * 2018-03-14 2018-07-20 江苏海林电子新材料科技有限公司 A kind of optical crystal and its growing method of the preparation of large scale doped gallium lanthanum crystal
CN110452698A (en) * 2019-07-08 2019-11-15 惠州学院 A kind of visible light ultra wide band is sensitized near-infrared luminous fluorescent powder and preparation method thereof

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