CN105481250A - Colorless transparent glass-ceramic with long after-glow down-conversion luminescence characteristics and preparation method thereof - Google Patents
Colorless transparent glass-ceramic with long after-glow down-conversion luminescence characteristics and preparation method thereof Download PDFInfo
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Abstract
The invention provides a colorless transparent glass-ceramic with long after-glow down-conversion luminescence characteristics. The glass-ceramic comprises a glass substrate and a dopant. The glass substrate has a molar chemical composition of (20-40) GeO2-(20-40) M2O3-(10-60) ZnO-(5-20) La2O3-(5-20) Li2O, and the total sum of the molar ratio of the compounds is 100%, wherein M represents B or Ga. The dopant is based on the glass substrate and further doped with 0.1-2mol.% of MnO and 0.1-3mol.% of Yb2O3. The glass prepared by the present invention has high transparency, stable physical and chemical properties, and can be used as an upper cover plate of crystalline silicon solar cell; and the preparation process is simple. The invention solves the problem of continuous working of solar cell without sunlight and provides a novel thinking and technique means for improving the usage efficiency of solar cell and photoelectric conversion efficiency.
Description
Technical field
What the present invention relates to is a kind of characteristics of luminescence material with new luminescence phenomenon, the invention still further relates to a kind of preparation method of characteristics of luminescence material.Described characteristics of luminescence material can be used for improving solar cell photoelectric efficiency of conversion.
Background technology
Long-afterglow luminescent glass is the energy-saving environmental protection storage luminescent material of Novel pollution-free, and the energy storage that it obtains under sunlight, luminescent lamp, incandescent light etc. being irradiated in the material, then discharges with the form of luminescence lentamente.Utilize this characteristic to can be used as the lighting source at night and dark place, have significant application value in fields such as building and traffic.The west majority state such as the U.S., Germany is by using novel environment friendly luminous product in relevant legislation regulation building, and European Union member countries also promulgate corresponding industry standard.
Long afterglow glass mainly contains two kinds of preparation means: one, rare earth doped or transient metal doped ion in glass host material.1998, Qiu Jianrong prepared Eu first in reducing atmosphere
2+/ Dy
3+mix CaO-Al altogether
2o
3-B
2o
3and SrO-Al
2o
3-SiO
2green glow long afterglow glass.In the same year, M.Yamazaki reports Tb
3+doping ZnO-B
2o
3-SiO
2the green glow of glass under ultraviolet excitation is long-persistence luminous, and subsequently, they pass through Yb again
3+ion sensitizedly enhance Tb
3+ion long-persistence luminous.Although can obtain long-afterglow luminescent glass, its luminescent properties can't reach practical level.2000, J.Fu was first at Eu
2+/ Dy
3+mix SrO-MgO-CaO-B altogether
2o
3-SiO
2the blue-light-emitting of time of persistence more than 5h is achieved in devitrified glass.Devitrified glass has crystalline material luminous intensity height and glass isotropy, easy feature of processing concurrently, is the extremely potential long-afterglow material of a class.The people such as Soviet Union's clanging or clanking sound are with ZnO-B
2o
3-SiO
2for host glass by mix manganese (II) ion separately or mix manganese (II) altogether, ytterbium (III) ion, antimony (III), samarium (III) ion prepared a series of green, yellow and red long-afterglow luminescent microcrystal glass, and proposition can utilize this material to carry out the memory storage of writings and image.L.Xiao also by thermal treatment at SrO-Al
2o
3-B
2o
3glass surface separates out SrAl
2o
4: Eu
2+, Dy
3+nanometer steady persistence crystal preparation green glow long-afterglow luminescent glass.2005, Qiu built standby first passage thermal treatment at Mn
2+doped with Ge O
2-B
2o
3-ZnO glass surface separates out the Zn with Characteristics of Long Luminosity, micro-meter scale
2geO
4crystal.
Another kind of conventional preparation means is directly mixed in glass matrix by the fluorescent material with Characteristics of Long Luminosity, prepares long-afterglow luminescent glass as CN1397509A discloses by long persistence luminescent powder and glass powder with low melting point being mixed the cooling of melting again; Fluorescent glass powder first made by the long persistence luminescent powder that CN1603265A adopts one or more ion-activated and host glass, then adopts multiple conventional process of glass to make steady persistence visible luminescent glass; CN102464450A discloses commercial SrAl
2o
4: Eu
2+, Dy
3+fluorescent material and sulfate-phosphate glass powder with low melting point mixed sintering prepare green glow long afterglow glass.
In sum, within having reported that long-afterglow luminescent glass emission wavelength is all positioned at visible ray 400-700nm scope, the report of any near-infrared band (>1000nm) long-afterglow luminescent glass has not yet been had.1000nm near infrared light is positioned at crystal silicon solar batteries optimal response wave band, can, by crystal silicon battery efficient absorption, be conducive to improving cell photoelectric efficiency of conversion.Meanwhile, because high-energy regions in solar spectrum (UV-light) easily causes solar cell to cross thermal losses, thus conversion luminescence under ultraviolet-near infrared, both converted UV-light near infrared light, was a kind of means of efficiency utilization sun power.Being mixed altogether by rare earth ion to realize transforming under ultraviolet (visible)-near infrared luminous, and its theoretical quantum luminous efficiency is 200%.Qiu Jianrong etc. report series of rare earth ion (as Eu
2+/ Yb
3+) mix lower conversion fluorescent glass altogether.The old large people such as grade that admires separates out fluorochemical (CaF in oxyfluoride glass
2, CeF
3deng) nanocrystal have studied conversion luminescence characteristic under rare earth ion.But, report that the quantum-cutting near-infrared luminous life-span is Microsecond grade to the maximum, do not reach steady persistence rank (a few hours or tens of hours) far away, thus cannot by energy storage at sunshine on daytime, night twilight sunset release can mode solar cell is carried out 24 hours uninterrupted " charging ".
Summary of the invention
The object of the present invention is to provide a kind of can solve crystal silicon solar batteries also can the water white transparency devitrified glass with conversion luminescence characteristic under steady persistence of problem of continuous firing under without sun exposure condition.The present invention also aims to provide a kind of preparation method with the water white transparency devitrified glass of conversion luminescence characteristic under steady persistence.
Of the present invention have the water white transparency devitrified glass of conversion luminescence characteristic under steady persistence and comprise glass matrix and hotchpotch, and the Mole percent proportioning chemical constitution of described glass matrix is (20-40) GeO
2-(20-40) M
2o
3-(10-60) ZnO-(5-20) La
2o
3-(5-20) Li
2o, the Mole percent proportioning summation of each composition compound is 100%, wherein M=B or Ga; Described hotchpotch is 0.1-2mol.%MnO and 0.1-3mol.%Yb that adulterate again on the basis of glass matrix
2o
3.
The preparation method with the water white transparency devitrified glass of conversion luminescence characteristic under steady persistence of the present invention comprises the following steps:
(1) be (20-40) GeO according to the Mole percent proportioning chemical constitution of glass matrix
2-(20-40) M
2o
3-(10-60) ZnO-(5-20) La
2o
3-(5-20) Li
2o, the Mole percent proportioning summation that glass matrix respectively forms compound is 100%, then 0.1-2mol.%MnO and 0.1-3mol.%Yb that adulterate on the basis of glass matrix
2o
3ratio by raw material Homogeneous phase mixing 30-120 minute in ball mill, put into platinum crucible, pre-burning 0.5-2 hour at 600-900 DEG C in weak reducing atmosphere stove;
(2) after the raw material after pre-burning being naturally cooled to room temperature, secondary mixing 30-120 minute is carried out in ball mill, put into weak reducing atmosphere stove subsequently and carry out melting system, temperature 1200-1650 DEG C, soaking time 1-2 hour, subsequently fused solution is carried out quenching on copper coin heated in advance, finally at 400-600 DEG C of annealing 2-6 hour;
(3) prepared glass is put into weakly reducing atmosphere stove, thermal treatment 0.5-24 hour at 600-800 DEG C.
Described weak reducing atmosphere is volume ratio is 95% nitrogen and 5% hydrogen gas mixture.
M=B or Ga.
Be different from steady persistence and up-conversion luminescence being combined of people's report such as Hyppanen and realize steady persistence is changed visible luminescent, the present invention is intended to steady persistence and lower conversion luminescence to combine, namely in glass matrix, the crystal with long afterglow property is separated out by micritization, conversion luminescence effect under cooperation between recycling dopant ion, realize transforming under ultraviolet (visible)-near infrared (1000nm) steady persistence luminous, thus solve crystal silicon solar batteries also can the problem of continuous firing under without sun exposure condition.
First the method cooled by melting at a certain temperature prepares the bulk glass of high optical quality; The crystal with Characteristics of Long Luminosity is separated out subsequently in glass by thermal treatment; Finally by the glass sample of preparation at 240-320nm ultraviolet light irradiation after 10-30 minute, can observe glow peak, to be positioned at 1000nm long-persistence luminous, time of persistence 0.5-3 hour.Glass transparent degree prepared by the present invention is high, physical and chemical performance stable and preparation technology is simple, can be used as crystal silicon solar batteries upper cover plate glass, solving also can the problem of continuous firing without solar cell under sun exposure condition, for raising solar cell service efficiency and photoelectric transformation efficiency provide a kind of new approaches and technique means.
Accompanying drawing explanation
Fluorescent glass pictorial diagram photo is transformed, from the pictorial diagram photo being respectively embodiment 1 from left to right, embodiment 2, embodiment 3, embodiment 4 obtain under the steady persistence that Fig. 1 obtains for the present invention.
Fig. 2 transforms illuminated diagram under fluorescent glass burst of ultraviolel under steady persistence of the present invention.
Fig. 3 transforms fluorescent glass uv irradiation decay of afterglow figure after 20 minutes under steady persistence of the present invention.
Embodiment
Illustrate below and the present invention is described in more detail.
Embodiment 1:25GeO
2-25Ga
2o
3-40ZnO-3La
2o
3-7Li
2o:0.5MnO, 1Yb
2o
3.
In above-mentioned glass formula, before classes of compounds, numerical value represents molar percentage (mol.%), represents MnO and Yb adulterated in glass after colon
2o
3molar content.Preparation method: take zinc carbonate (ZnCO respectively
3), gallium oxide (Ga
2o
3), germanium oxide (GeO
2), lanthanum trioxide (La
2o
3), Quilonum Retard (Li
2cO
3), manganous carbonate (MnCO
3), ytterbium oxide (Yb
2o
3), above-mentioned raw materials is put into ball mill and stir 1 hour, put into platinum crucible subsequently, (95% nitrogen and 5% hydrogen gas mixture) pre-burning 2 hours in 900 DEG C of weak reducing atmosphere stoves.After raw material after pre-burning naturally cools to room temperature, secondary stirs 1 hour in ball mill, to put at 1400 DEG C, weak reducing atmosphere stove (95% nitrogen and 5% hydrogen gas mixture) melting subsequently 2 hours.Glass metal is cooled on the copper coin of 200 DEG C of preheatings, and be placed in the retort furnace of 400 DEG C anneal 2 hours.Finally the bulk glass prepared thermal treatment in 650 DEG C of weak reducing atmosphere stoves is obtained final devitrified glass sample for 2 hours.Carry out Performance Detection to the sample after polishing, acquired results is shown in accompanying drawing, and wherein, Fig. 1 is the devitrified glass pictorial diagram of preparation; Fig. 2 is the fluorescence spectrum of this sample under 290nm burst of ultraviolel; Fig. 3 is 290nm uv irradiation after 20 minutes, 1000nm luminous intensity decay pattern in time.
Embodiment 2:25GeO
2-25Ga
2o
3-40ZnO-3La
2o
3-7Li
2o:0.25MnO, 1Yb
2o
3.
In above-mentioned glass formula, before classes of compounds, numerical value represents molar percentage (mol.%), represents MnO and Yb adulterated in glass after colon
2o
3molar content.Preparation method: take zinc carbonate (ZnCO respectively
3), gallium oxide (Ga
2o
3), germanium oxide (GeO
2), lanthanum trioxide (La
2o
3), Quilonum Retard (Li
2cO
3), manganous carbonate (MnCO
3), ytterbium oxide (Yb
2o
3), above-mentioned raw materials is put into ball mill and stir 1 hour, put into platinum crucible subsequently, (95% nitrogen and 5% hydrogen gas mixture) pre-burning 2 hours in 900 DEG C of weak reducing atmosphere stoves.After raw material after pre-burning naturally cools to room temperature, secondary stirs 1 hour in ball mill, to put at 1400 DEG C, weak reducing atmosphere stove (95% nitrogen and 5% hydrogen gas mixture) melting subsequently 2 hours.Glass metal is cooled on the copper coin of 200 DEG C of preheatings, and be placed in the retort furnace of 400 DEG C anneal 2 hours.Finally the bulk glass prepared thermal treatment in the weak reducing atmosphere stove of 650 DEG C is obtained final devitrified glass sample for 1 hour.Carry out Performance Detection to the sample after polishing, acquired results is shown in accompanying drawing, and wherein, Fig. 1 is the devitrified glass pictorial diagram of preparation; Fig. 2 is the fluorescence spectrum of this sample under 290nm burst of ultraviolel; Fig. 3 is 290nm uv irradiation after 20 minutes, 1000nm luminous intensity decay pattern in time.
Embodiment 3:25GeO
2-25B
2o
3-40ZnO-3La
2o
3-7Li
2o:0.5MnO, 1Yb
2o
3.
In above-mentioned glass formula, before classes of compounds, numerical value represents molar percentage (mol.%), represents MnO and Yb adulterated in glass after colon
2o
3molar content.Preparation method: take zinc carbonate (ZnCO respectively
3), boric acid (H
3bO
3), germanium oxide (GeO
2), lanthanum trioxide (La
2o
3), Quilonum Retard (Li
2cO
3), manganous carbonate (MnCO
3), ytterbium oxide (Yb
2o
3), above-mentioned raw materials is put into ball mill and stir 1 hour, put into platinum crucible subsequently, (95% nitrogen and 5% hydrogen gas mixture) pre-burning 2 hours in 900 DEG C of weak reducing atmosphere stoves.After raw material after pre-burning naturally cools to room temperature, secondary stirs 1 hour in ball mill, to put at 1400 DEG C, weak reducing atmosphere stove (95% nitrogen and 5% hydrogen gas mixture) melting subsequently 2 hours.Glass metal is cooled on the copper coin of 200 DEG C of preheatings, and be placed in the retort furnace of 400 DEG C anneal 2 hours.Finally the bulk glass prepared thermal treatment in the weak reducing atmosphere stove of 650 DEG C is obtained final devitrified glass sample for 1 hour.Carry out Performance Detection to the sample after polishing, acquired results is shown in accompanying drawing, and wherein, Fig. 1 is the devitrified glass pictorial diagram of preparation; Fig. 2 is the fluorescence spectrum of this sample under 290nm burst of ultraviolel; Fig. 3 is 290nm uv irradiation after 20 minutes, 1000nm luminous intensity decay pattern in time.
Embodiment 4:25GeO
2-25B
2o
3-40ZnO-3La
2o
3-7Li
2o:0.25MnO, 1Yb
2o
3.
In above-mentioned glass formula, before classes of compounds, numerical value represents molar percentage (mol.%), represents MnO and Yb adulterated in glass after colon
2o
3molar content.Preparation method: take zinc carbonate (ZnCO respectively
3), boric acid (H
3bO
3), germanium oxide (GeO
2), lanthanum trioxide (La
2o
3), Quilonum Retard (Li
2cO
3), manganous carbonate (MnCO
3), ytterbium oxide (Yb
2o
3), above-mentioned raw materials is put into ball mill and stir 1 hour, put into platinum crucible subsequently, (95% nitrogen and 5% hydrogen gas mixture) pre-burning 2 hours in 900 DEG C of weak reducing atmosphere stoves.After raw material after pre-burning naturally cools to room temperature, secondary stirs 1 hour in ball mill, to put at 1400 DEG C, weak reducing atmosphere stove (95% nitrogen and 5% hydrogen gas mixture) melting subsequently 2 hours.Glass metal is cooled on the copper coin of 200 DEG C of preheatings, and be placed in the retort furnace of 400 DEG C anneal 2 hours.Finally the bulk glass prepared thermal treatment in the weak reducing atmosphere stove of 650 DEG C is obtained final devitrified glass sample for 1 hour.Carry out Performance Detection to the sample after polishing, acquired results is shown in accompanying drawing, and wherein, Fig. 1 is the devitrified glass pictorial diagram of preparation; Fig. 2 is the fluorescence spectrum of this sample under 290nm burst of ultraviolel; Fig. 3 is 290nm uv irradiation after 20 minutes, 1000nm luminous intensity decay pattern in time.
Claims (4)
1. there is a water white transparency devitrified glass for conversion luminescence characteristic under steady persistence, comprise glass matrix and hotchpotch, it is characterized in that: the Mole percent proportioning chemical constitution of described glass matrix is (20-40) GeO
2-(20-40) M
2o
3-(10-60) ZnO-(5-20) La
2o
3-(5-20) Li
2o, the Mole percent proportioning summation of each composition compound is 100%, wherein M=B or Ga; Described hotchpotch is 0.1-2mol.%MnO and 0.1-3mol.%Yb that adulterate again on the basis of glass matrix
2o
3.
2. there is a preparation method for the water white transparency devitrified glass of conversion luminescence characteristic under steady persistence, it is characterized in that comprising the following steps:
(1) be (20-40) GeO according to the Mole percent proportioning chemical constitution of glass matrix
2-(20-40) M
2o
3-(10-60) ZnO-(5-20) La
2o
3-(5-20) Li
2o, the Mole percent proportioning summation that glass matrix respectively forms compound is 100%, then 0.1-2mol.%MnO and 0.1-3mol.%Yb that adulterate on the basis of glass matrix
2o
3ratio by raw material Homogeneous phase mixing 30-120 minute in ball mill, put into platinum crucible, pre-burning 0.5-2 hour at 600-900 DEG C in weak reducing atmosphere stove;
(2) after the raw material after pre-burning being naturally cooled to room temperature, secondary mixing 30-120 minute is carried out in ball mill, put into weak reducing atmosphere stove subsequently and carry out melting system, temperature 1200-1650 DEG C, soaking time 1-2 hour, subsequently fused solution is carried out quenching on copper coin heated in advance, finally at 400-600 DEG C of annealing 2-6 hour;
(3) prepared glass is put into weakly reducing atmosphere stove, thermal treatment 0.5-24 hour at 600-800 DEG C.
3. the preparation method with the water white transparency devitrified glass of conversion luminescence characteristic under steady persistence according to claim 2, is characterized in that: described weak reducing atmosphere is volume ratio is 95% nitrogen and 5% hydrogen gas mixture.
4. the preparation method with the water white transparency devitrified glass of conversion luminescence characteristic under steady persistence according to Claims 2 or 3, is characterized in that: M=B or Ga.
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Cited By (6)
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| CN106927685A (en) * | 2017-03-24 | 2017-07-07 | 苏州凯文堡尼光电科技有限公司 | It is a kind of with long-persistence luminous microcrystalline glass optical fiber and preparation method thereof |
| CN106977094A (en) * | 2017-04-18 | 2017-07-25 | 杭州余杭振华日化玻璃有限公司 | Crystal glass and preparation method thereof |
| CN109250918A (en) * | 2018-09-01 | 2019-01-22 | 哈尔滨工程大学 | A kind of preparation method of the transparent glass-ceramics under room temperature environment with broadband Upconversion luminescence |
| CN110054415A (en) * | 2019-03-26 | 2019-07-26 | 宁波大学 | A kind of up-conversion luminescence nano-glass ceramic material and preparation method thereof based on Yb-Mn dimer |
| CN113105113A (en) * | 2021-04-09 | 2021-07-13 | 泰山学院 | Special optical glass with pure red light luminescence characteristic and preparation method and application thereof |
| CN114380505A (en) * | 2022-02-25 | 2022-04-22 | 中国计量大学 | Sunlight-excited ultra-long afterglow microcrystalline glass and preparation method thereof |
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| CN106927685A (en) * | 2017-03-24 | 2017-07-07 | 苏州凯文堡尼光电科技有限公司 | It is a kind of with long-persistence luminous microcrystalline glass optical fiber and preparation method thereof |
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| CN106977094A (en) * | 2017-04-18 | 2017-07-25 | 杭州余杭振华日化玻璃有限公司 | Crystal glass and preparation method thereof |
| CN106977094B (en) * | 2017-04-18 | 2019-05-21 | 杭州余杭振华日化玻璃有限公司 | Crystal glass and preparation method thereof |
| CN109250918A (en) * | 2018-09-01 | 2019-01-22 | 哈尔滨工程大学 | A kind of preparation method of the transparent glass-ceramics under room temperature environment with broadband Upconversion luminescence |
| CN110054415A (en) * | 2019-03-26 | 2019-07-26 | 宁波大学 | A kind of up-conversion luminescence nano-glass ceramic material and preparation method thereof based on Yb-Mn dimer |
| CN113105113A (en) * | 2021-04-09 | 2021-07-13 | 泰山学院 | Special optical glass with pure red light luminescence characteristic and preparation method and application thereof |
| CN114380505A (en) * | 2022-02-25 | 2022-04-22 | 中国计量大学 | Sunlight-excited ultra-long afterglow microcrystalline glass and preparation method thereof |
| CN114380505B (en) * | 2022-02-25 | 2023-03-07 | 中国计量大学 | Sunlight-excited ultra-long afterglow microcrystalline glass and preparation method thereof |
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