CN110228948B - Novel photoluminescence transparent glass ceramic and preparation method thereof - Google Patents

Novel photoluminescence transparent glass ceramic and preparation method thereof Download PDF

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CN110228948B
CN110228948B CN201910402146.1A CN201910402146A CN110228948B CN 110228948 B CN110228948 B CN 110228948B CN 201910402146 A CN201910402146 A CN 201910402146A CN 110228948 B CN110228948 B CN 110228948B
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江莎
付绍珂
胡潇月
陈明月
王传婷
罗小霞
周贤菊
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Chongqing University of Post and Telecommunications
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • 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
    • 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 a novel photoluminescence transparent glass ceramic and a preparation method thereof, belonging to the technical field of optical temperature measurement of rare earth doped phosphate nanocrystal-containing transparent glass ceramic. The glass ceramic with the rare earth doped nanocrystalline is obtained by mixing raw materials, melting the raw materials, quenching and forming, annealing a sample, cutting the sample and performing heat treatment. Transparent glass-ceramics have some of the advantages of both crystals and glass: (1) compared with glass, the transparent glass ceramic improves the luminous efficiency of the rare earth luminous center to a certain extent, and greatly improves the chemical stability and the mechanical property; (2) compared with crystals, the glass ceramic has compact structure, no air holes, low preparation cost, short synthesis period and easy realization of mass production. The transparent glass ceramic disclosed by the invention is simple and easy to obtain in ingredients, and has the advantages of low preparation cost, high luminous efficiency, high transmittance, high stability, high mechanical property, adjustable luminous band and the like.

Description

Novel photoluminescence transparent glass ceramic and preparation method thereof
Technical Field
The invention relates to a transparent glass ceramic for optical temperature measurement and a preparation method thereof, in particular to a glass ceramic containing novel crystals and a preparation method thereof.
Background
The temperature is a physical quantity indicating the degree of cooling and heating of the object, and is the most measured physical quantity so far. The accurate measurement of the temperature has very important practical significance and research value in the fields of science and technology, military, industrial production and the like. For traditional contact thermometers, such as glass liquid thermometers and gas thermometers based on the thermal expansion effect of materials, thermocouple thermometers based on the seebeck effect, etc., they have the advantages of convenient use, wide measurement range, accurate measurement, easy analysis of data, etc., but with the rapid development of scientific technology, the traditional thermometers face a lot of difficulties and challenges in temperature measurement, and cannot meet a lot of complex special environments, such as microelectronic circuits, biological cell growth, strong corrosiveness, strong electric fields, strong magnetic fields, etc., or moving objects. Therefore, there is a need to develop and explore a new non-contact optical temperature detection technology with fast response, high accuracy and miniaturization to solve some of the disadvantages of the conventional temperature sensor.
In recent years, a series of luminescent materials for measuring temperature by using an optical method have been rapidly developed in the aspect of temperature sensing test due to the outstanding advantages of non-contact type, quick response and the like, and various optical temperature measurement technologies including near infrared temperature measurement, raman scattering temperature measurement, fluorescence temperature measurement and the like are realized. The near-infrared temperature measurement technology is used for realizing temperature measurement based on the blackbody radiation principle, is a common industrial object surface temperature measurement mode, has the defects of low surface emission and spatial resolution and is difficult to be used for micro equipment; raman scattering temperature measurement is realized by analyzing Raman vibration modes at different temperatures, and the method is only used for measuring the temperature of an object with obvious Raman effect; fluorescence temperature measurement is realized based on the fluorescence temperature-sensitive characteristic of rare earth ions, and the rare earth ions have good luminescence property due to 4f-4f transition, thereby showing great advantages in the aspect of optical temperature sensors and having important significance in the aspect of temperature sensing. Therefore, the temperature measurement method based on the fluorescence temperature-sensitive property has received extensive attention and research from researchers. The materials used for fluorescence temperature measurement are commonly powder, thin films, glass ceramic materials and the like, when a powder sample is used as a temperature measurement material, the transparency is poor, only the surface part of the sample can be effectively excited, excitation and emitted light cannot permeate into the sample, and energy can be lost through energy transfer at the deep inside; when the film sample is used as a temperature measuring material, the mechanical strength and the mechanical property are poor, and the film sample can be fixed only by being evaporated on a substrate; the transparent microcrystalline glass material has volume effect, greatly improved optical characteristic and high chemical and mechanical stability, and thus has great significance in optical performance and practical application.
Disclosure of Invention
The invention mainly aims to overcome the defects of the existing optical temperature measuring material, and provides a novel optical glass ceramic and a preparation method thereof, which improve the testing performance, reduce the cost and are more suitable for the practical application of optical temperature measurement.
In order to achieve the purpose, the invention adopts the scheme that: a novel photoluminescence transparent glass ceramic is prepared by mixing raw materials, melting the raw materials, quenching and forming, annealing a sample, cutting the sample and performing heat treatment on the raw materials to obtain the glass ceramic with rare earth doped nanocrystals, wherein the raw materials comprise the following components in percentage by mol: na (Na)2CO3 15-25％，CaO 20-30％，P2O5 5-10％，H3BO330-50%, rare earth ion 0.5-5%, ZrO2As a crystal nucleus agent, 1% of the total weight of the above ingredients was weighed. The rare earth ions are selected from rare earth oxide Eu2O3、Sm2O3、Tb4O7And Nd2O3One or more of (a).
According to the raw materials, the preparation method of the photoluminescent transparent glass ceramic is mainly completed by the following steps:
step one, proportioning and weighing: the raw materials required for preparing the transparent glass ceramic are calculated and weighed according to the proportion of the raw materials.
Step two, mixing the ingredients: and (3) putting the raw materials weighed in the step one into a ceramic mortar cleaned in advance, fully grinding for one hour to uniformly mix the raw materials to obtain a batch, and placing the batch in a ceramic crucible cleaned in advance.
Step three, melting the ingredients: and (3) melting the batch materials in the step (II) in a high-temperature lifting furnace at 1350 ℃ and 1450 ℃ for 60-120min to obtain homogenized and clarified glass liquid in an air atmosphere.
Step four, quench forming: and (4) quickly pouring the molten glass liquid in the third step onto a preheated copper plate, and quickly pressing and forming.
Step five, DSC test: the sample is subjected to Differential thermal analysis by Differential Scanning Calorimetry (DSC for short) to find out the glass transition temperature, crystallization peak, melting temperature, and the like.
Step six, annealing the sample: and setting the temperature of the annealing furnace to be 400-450 ℃ according to the data result of the step five, carrying out annealing treatment on the sample, preserving the heat at the temperature of 400-450 ℃ for 100-180min, and obtaining the glass precursor sample after the temperature in the furnace is naturally reduced to the normal temperature.
Step seven, cutting a sample: and cutting the glass precursor sample obtained in the step six on a cutting machine to obtain glass sheets with uniform sizes.
Step eight, heat treatment: and (3) carrying out two-step heat treatment on the glass precursor sample obtained in the step seven, wherein in the first step, the crystal nucleation temperature is firstly adjusted, the glass precursor sample is placed in a muffle furnace, the heating temperature is 500-560 ℃, and the heat preservation time is 80-180 min. In order to better control the crystallization conditions of the glass, the glass is gradually explored within the range of 500-560 ℃ to obtain the proper nucleation temperature of the glass.
Step nine, in the step eight, further crystal growth treatment is carried out according to the optimal nucleation temperature, the heating temperature is 600-.
Step ten, polishing a sample: and (4) grinding and polishing the glass ceramic obtained in the step nine to obtain the final transparent glass ceramic.
The size of the nano crystal grain of the glass ceramic prepared by the invention is within the range of 10-20 nm.
By the technical scheme, the photoluminescent transparent glass ceramic and the preparation process thereof have the following advantages:
the rare earth doped transparent glass ceramic takes phosphate as a glass matrix, so that the preparation cost is obviously reduced. The glass ceramic obtained by heat treatment crystallization has the advantages of glass and crystal, has good mechanical strength, improves the chemical stability and thermal stability of phosphate glass, forms a stable rare earth ion luminescence center and enhances the luminescence performance. The preparation process of the invention adopts a high-temperature melting quenching method, the preparation process is simple, the cost is low, the thermal stability is good, the luminous efficiency is high, the transmittance is high, the luminous wave band is adjustable, and the like, and the prepared glass ceramic has a novel nano crystal phase.
The light-emitting band of the invention is adjustable, (1) the light-emitting band can be adjusted by singly doping different rare earth elements, and (2) the light-emitting band can be adjusted by codoping two or more different rare earth elements and changing the concentration ratio of rare earth doping. The rare earth doped photoluminescent material can realize luminescence from visible to infrared bands.
The nano-scale crystals are embedded in the glass, so that the transparency of the glass ceramic is greatly influenced, the size of the nano-crystalline grains is within the range of 10-20nm, and the size of the crystalline grains of the glass ceramic is much smaller than the wavelength of visible light, so that the glass ceramic can achieve high transparency.
Drawings
FIG. 1 is a flow chart of the preparation of the novel photoluminescent glass-ceramic of the present invention.
FIG. 2 is a DSC graph, T, of the photoluminescent glass-ceramic of the present invention containing nanocrystalsgIs the glass transition temperature, Tc1Is the first crystallization peak, Tc2Is the second crystallization peak, TmThe endothermic peak of the glass melting.
FIG. 3 shows that Ca is contained in the present invention8Eu2(PO4)6O2，Ca8Sm2(PO4)6O2，Ca8Tb2(PO4)6O2，Ca8Eu2(PO4)6O2:Nd3 +The X-ray diffraction patterns of the photoluminescence Glass Ceramic (GC) and the corresponding glass (PG) of the nanocrystalline are that the nucleation temperature of the first heat treatment is 550 ℃, and the crystal growth temperature of the second heat treatment is a certain temperature between 610 ℃ and 650 ℃.
FIG. 4 shows that Ca is contained in the present invention8Eu2(PO4)6O2Nanocrystalline photoluminescent glass-ceramicsAs shown in FIG. 4(a), the interplanar spacing of (1) is 0.27nm, which corresponds to the lattice plane Ca of (202)8Eu2(PO4)6O2A crystal; as can be seen from fig. 4(b), the diffraction spot of the nanocrystal particle corresponds to the (202) lattice plane, as can be seen from fig. 4(c), the size of the nanocrystal particle is less than 20nm, and as can be seen from fig. 4(d), the nanocrystal particle has only one main crystal phase, consistent with the XRD test results.
FIG. 5 is a photograph of a photoluminescent Glass Ceramic (GC) and glass of the present invention in real-life under natural light and under an ultraviolet lamp.
Detailed Description
In order to further illustrate the technical means adopted by the invention, the specific implementation and efficacy of the novel photoluminescent glass-ceramic and the preparation process thereof provided by the invention are described in detail as follows:
example 1
The novel photoluminescence Ca proposed by the present invention was prepared according to the experimental scheme shown in FIG. 18Eu2(PO4)6O2The glass-ceramic is a mixture of glass-ceramic,
step one, proportioning and weighing: the raw materials required for preparing the transparent glass ceramic are calculated and weighed according to the following proportion. The mol percentage is as follows: na (Na)2CO3 25％，CaO 23％，P2O5 6％，H3BO3 44％，Eu2O3 2％，ZrO2As a nucleating agent, 1% by weight of the total amount of the formulation was weighed out.
Step two, mixing the ingredients: and (3) putting the raw materials weighed in the step one into a ceramic mortar cleaned in advance, fully grinding for 1 hour to uniformly mix the raw materials to obtain a batch, and placing the batch in a ceramic crucible cleaned in advance.
Step three, melting the ingredients: melting the batch materials in the step two in a high-temperature lifting furnace, wherein the melting temperature is 1400 ℃, keeping the temperature for 100min, and obtaining glass liquid in an air atmosphere;
step four, quench forming: and 4, quickly pouring the molten glass liquid in the third step onto a preheated copper plate, and quickly covering the copper plate for pressing and forming.
Step five, DSC test: differential thermal analysis is carried out on the sample through differential scanning calorimetry, the glass transition temperature, the crystallization peak, the melting temperature and the like are found, the test range is 25-1200 ℃, and the heating rate is 20 ℃/min.
Step six, annealing the sample: and D, according to the data result of the step five, annealing the sample, setting the annealing temperature to be 450 ℃, keeping the annealing temperature for 180min, and obtaining a glass precursor sample after the temperature in the furnace is naturally reduced to the normal temperature.
Step seven, cutting a sample: and cutting the glass precursor sample obtained in the step six on a cutting machine to obtain the glass sheet with proper and uniform size.
Step eight, heat treatment: and (4) carrying out two-step heat treatment on the glass precursor sample obtained in the step seven, carrying out heat treatment for crystal nucleation in the first step, and keeping the temperature at 520 ℃ for 120min under the condition.
Step nine, carrying out further crystal growth treatment on the basis of the step eight to obtain Ca8Eu2(PO4)6O2The nanocrystalline glass ceramic is subjected to heat preservation for 120min at 630 ℃, and then is naturally cooled to the normal temperature.
Step ten, polishing a sample: grinding and polishing the glass ceramic prepared in the ninth step to finally obtain the product containing Ca8Eu2(PO4)6O2Novel transparent glass-ceramics of nanocrystalline.
Example 2
The novel Ca-containing compositions of the present invention were prepared according to the experimental scheme shown in FIG. 18Sm2(PO4)6O2A photoluminescent glass-ceramic of a nanocrystal,
step one, proportioning and weighing: the raw materials required for preparing the transparent glass ceramic are calculated and weighed according to the following proportion. The mol percentage is as follows: na (Na)2CO3 25％，CaO 23.5％，P2O5 6％，H3BO3 44％，Sm2O3 1.5％，ZrO2As a crystal nucleus agent, weighing the total weight of the ingredients1% of the total.
Step two, mixing the ingredients: and (3) putting the raw materials weighed in the step one into a ceramic mortar cleaned in advance, fully grinding for 1 hour to uniformly mix the raw materials to obtain a batch, and placing the batch in a ceramic crucible cleaned in advance.
Step three, melting the ingredients: and (5) melting the batch materials in the step two in a high-temperature lifting furnace, wherein the melting temperature is 1350 ℃, and keeping the temperature for 80min to obtain glass liquid in an air atmosphere.
Step four, quench forming: and 4, quickly pouring the molten glass liquid in the third step onto a preheated copper plate, and quickly covering the copper plate for pressing and forming.
Step five, DSC test: differential thermal analysis is carried out on the sample through differential scanning calorimetry, the glass transition temperature, the crystallization peak, the melting temperature and the like are found, the test range is 25-1200 ℃, and the heating rate is 20 ℃/min.
Step six, annealing the sample: and D, according to the data result of the step five, annealing the sample, setting the annealing temperature to be 400 ℃, preserving the heat for 100min, and obtaining the glass precursor sample after the temperature in the furnace is naturally reduced to the normal temperature.
Step seven, cutting a sample: and cutting the glass precursor sample obtained in the step six on a cutting machine to obtain the glass sheet with proper and uniform size.
Step eight, heat treatment: and (4) carrying out two-step heat treatment on the glass precursor sample obtained in the step seven, carrying out heat treatment for crystal nucleation in the first step, and keeping the temperature at 500 ℃ for 180min under the condition.
Step nine, carrying out further crystal growth treatment on the basis of the step eight to obtain Ca8Sm2(PO4)6O2The nano-crystalline glass ceramic is subjected to heat preservation for 120min at the temperature of 600 ℃, and then is naturally cooled to the normal temperature.
Step ten, polishing a sample: grinding and polishing the glass ceramic prepared in the ninth step to finally obtain the product containing Ca8Sm2(PO4)6O2Novel transparent glass-ceramics of nanocrystalline.
Example 3
The novel Ca-containing compositions of the present invention were prepared according to the experimental scheme shown in FIG. 18Tb2(PO4)6O2A photoluminescent glass-ceramic of a nanocrystal,
step one, proportioning and weighing: the raw materials required for preparing the transparent glass ceramic are calculated and weighed according to the following proportion. The mol percentage is as follows: na (Na)2CO3 25％，CaO 22％，P2O5 6％，H3BO3 44％，Tb4O7 3％，ZrO2As a nucleating agent, 1% by weight of the total amount of the formulation was weighed out.
Step two, mixing the ingredients: putting the raw materials weighed in the step one into a ceramic mortar which is cleaned in advance, fully grinding for 1h to uniformly mix the raw materials to obtain a batch, and placing the batch in a ceramic crucible which is cleaned in advance;
step three, melting the ingredients: melting the batch materials in the step two in a high-temperature lifting furnace at 1450 ℃ for 60min to obtain molten glass in an air atmosphere;
step four, quench forming: quickly pouring molten glass liquid in the third step onto a preheated copper plate, and quickly covering the copper plate for compression molding;
step five, DSC test: carrying out differential thermal analysis on the sample by differential scanning calorimetry to find out the glass transition temperature, crystallization peak, melting temperature and the like, wherein the test range is 25-1200 ℃, and the heating rate is 20 ℃/min;
step six, annealing the sample: and D, according to the data result of the step five, annealing the sample, setting the annealing temperature to be 420 ℃, preserving the heat for 150min, and obtaining a glass precursor sample after the temperature in the furnace is naturally reduced to the normal temperature.
Step seven, cutting a sample: and cutting the glass precursor sample obtained in the step six on a cutting machine to obtain the glass sheet with proper and uniform size.
Step eight, heat treatment: and (4) carrying out two-step heat treatment on the glass precursor sample obtained in the step seven, carrying out heat treatment for crystal nucleation in the first step, and keeping the temperature at 550 ℃ for 100min under the condition.
And step nine, performing further crystal growth treatment on the basis of the step eight to obtain the glass ceramic with the nanocrystalline, wherein the temperature is kept at 670 ℃ for 80min, and then the temperature is naturally reduced to the normal temperature.
Step ten, polishing a sample: grinding and polishing the glass ceramic prepared in the ninth step to finally obtain the product containing Ca8Tb2(PO4)6O2Novel transparent glass-ceramics of nanocrystalline.
Example 4
The novel Ca-containing compositions of the present invention were prepared according to the experimental scheme shown in FIG. 18Eu2(PO4)6O2:Nd3+A photoluminescent glass-ceramic of a nanocrystal,
step one, proportioning and weighing: the raw materials required for preparing the transparent glass ceramic are calculated and weighed according to the following proportion. The mol percentage is as follows: na (Na)2CO3 25％，CaO 22％，P2O5 6％，H3BO3 44％，Eu2O3 2.5％，Nd2O3 0.5％,ZrO2As a nucleating agent, 1% by weight of the total amount of the formulation was weighed out.
Step two, mixing the ingredients: putting the raw materials weighed in the step one into a ceramic mortar which is cleaned in advance, fully grinding for 1h to uniformly mix the raw materials to obtain a batch, and placing the batch in a ceramic crucible which is cleaned in advance;
step three, melting the ingredients: melting the batch materials in the step two in a high-temperature lifting furnace, wherein the melting temperature is 1400 ℃, keeping the temperature for 100min, and obtaining glass liquid in an air atmosphere;
step four, quench forming: quickly pouring molten glass liquid in the third step onto a preheated copper plate, and quickly covering the copper plate for compression molding;
step five, DSC test: carrying out differential thermal analysis on the sample by differential scanning calorimetry to find out the glass transition temperature, crystallization peak, melting temperature and the like, wherein the test range is 25-1200 ℃, and the heating rate is 20 ℃/min;
step six, annealing the sample: and D, according to the data result of the step five, annealing the sample, setting the annealing temperature to be 450 ℃, preserving the heat for 180min, and obtaining a glass precursor sample after the temperature in the furnace is naturally reduced to the normal temperature.
Step seven, cutting a sample: and cutting the glass precursor sample obtained in the step six on a cutting machine to obtain the glass sheet with proper and uniform size.
Step eight, heat treatment: and (4) carrying out two-step heat treatment on the glass precursor sample obtained in the step seven, carrying out heat treatment for crystal nucleation in the first step, and keeping the temperature at 560 ℃ for 80min under the condition.
And step nine, performing further crystal growth treatment on the basis of the step eight to obtain the glass ceramic with the nanocrystalline crystal phase, wherein the temperature is maintained at 645 ℃ for 100min, and then, the temperature is naturally reduced to the normal temperature.
Step ten, polishing a sample: grinding and polishing the glass ceramic prepared in the ninth step to finally obtain the product containing Ca8Eu2(PO4)6O2:Nd3+Novel transparent glass-ceramics of nanocrystalline.
Fig. 5 shows that, by comparing the glass (PG) with the glass ceramic (PG), the transparency of the obtained glass ceramic is not significantly attenuated after crystallization, and the very transparent property is maintained, and the transparent glass ceramic improves the luminous efficiency of the rare earth luminescent center to a certain extent, and greatly improves the chemical stability and mechanical properties.

Claims (8)

1. A novel photoluminescence transparent glass ceramic is characterized in that: the glass ceramic with the rare earth doped nanocrystalline is obtained by mixing raw materials, melting the raw materials, quenching and forming, annealing a sample, cutting the sample and performing heat treatment on the raw materials, wherein the raw materials comprise the following components in percentage by mol: na (Na)2CO3 15-25%，CaO 20-30%，P2O5 5-10%，H3BO3 30-50%, rare earth ion 0.5-5%, ZrO2As a crystal nucleus agent, the above ingredients are weighed1% of the total weight, the rare earth ions being selected from rare earth oxide Eu2O3、Sm2O3、Tb4O7And Nd2O3One or more of (a).
2. A novel photoluminescent transparent glass-ceramic according to claim 1, characterized in that: the purity of the rare earth oxide is 99.99%.
3. A novel photoluminescent transparent glass-ceramic according to claim 1 or 2, characterized in that: the glass-ceramic has a nanocrystalline grain size in the range of 10-20 nm.
4. A preparation method of a novel photoluminescence transparent glass ceramic is characterized by comprising the following steps:
step one, proportioning and weighing: the raw materials required for preparing the transparent glass ceramic are calculated and weighed according to the following proportion by mol percent: na (Na)2CO3 15-25%，CaO 20-30%，P2O5 5-10%，H3BO3 30-50% of ZrO, 0.5% -5% of rare earth ions2Taking ZrO with the total weight of 1 percent of the ingredients as a crystal nucleating agent2(ii) a The rare earth ions are selected from rare earth oxide Eu2O3、Sm2O3、Tb4O7And Nd2O3One or more of;
step two, mixing the ingredients: putting the raw materials weighed in the step one into a ceramic mortar cleaned in advance, fully grinding and uniformly mixing to obtain a batch, and putting the batch into a ceramic crucible cleaned in advance;
step three, melting the ingredients: melting the batch materials in the step two in a high-temperature lifting furnace to obtain homogenized and clarified molten glass;
step four, quench forming: quickly pouring the molten glass in the third step onto a preheated copper plate, and pressing and forming;
step five, DSC detection: carrying out differential thermal analysis on the sample by differential scanning calorimetry to find out the glass transition temperature, the crystallization peak and the melting temperature;
step six, annealing the sample: according to the data result of the step five, annealing the sample to obtain a glass precursor;
step seven, cutting a sample: cutting the glass precursor sample obtained in the step six on a cutting machine to obtain glass sheets with uniform sizes;
step eight, heat treatment: performing two-step heat treatment on the glass precursor obtained in the step seven, wherein in the first step, the crystal nucleation temperature is adjusted; and secondly, carrying out crystal growth treatment in one step according to the optimal nucleation temperature to obtain the glass ceramic with the rare earth doped nanocrystalline.
5. The method for preparing a novel photoluminescent transparent glass-ceramic according to claim 4, wherein: and step eight, grinding and polishing the glass ceramic to obtain the final transparent glass ceramic.
6. The method for preparing a novel photoluminescent transparent glass-ceramic according to claim 4 or 5, characterized in that: and the melting treatment in the third step is carried out, wherein the heating temperature is 1350-.
7. The method for preparing a novel photoluminescent transparent glass-ceramic according to claim 4 or 5, characterized in that: and step six, annealing treatment, namely putting the sample into a muffle furnace, heating at the temperature of 400-450 ℃, and keeping the temperature for 180 min.
8. The method for preparing a novel photoluminescent transparent glass-ceramic according to claim 4 or 5, characterized in that: the two-step heat treatment in the step eight, wherein in the first step of heat treatment, the mixture is placed into a muffle furnace, the heating temperature is 500-560 ℃, and the heat preservation time is 80-180 min; in the second step of heat treatment, the heating temperature is 600-670 ℃, and the heat preservation time is 80-120 min.
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