CN102241480A - Elemental silver-doped rare earth ion luminescent glass and its preparation method - Google Patents

Elemental silver-doped rare earth ion luminescent glass and its preparation method Download PDF

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CN102241480A
CN102241480A CN2010101688167A CN201010168816A CN102241480A CN 102241480 A CN102241480 A CN 102241480A CN 2010101688167 A CN2010101688167 A CN 2010101688167A CN 201010168816 A CN201010168816 A CN 201010168816A CN 102241480 A CN102241480 A CN 102241480A
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glass
rare earth
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simple substance
substance silver
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CN102241480B (en
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周明杰
马文波
翁方轶
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention discloses elemental silver-doped rare earth ion luminescent glass and its preparation method, wherein the luminescent glass is a substance whose chemical formula is as follows: aSiO2.bAl2O3.cCaO.dNaF.eCaF2.xEuF3.yAg2O. The preparation method provided by the invention comprises the following steps of: using SiO2, Al2O3, CaCO3, NaF, CaF2, EuF3 and AgNO3 as raw materials, melting the raw materials at the temperature of 1200-1500 DEG C for 0.5-3 hours, pouring the melt into a die for moulding; staying warm under reducing atmosphere at the temperature of 300-550 DEG C for 0.5-5 hours; removing the reducing atmosphere, heating up to the temperature of 550-800 DEG C, followed by insulation for 1-5 hours, and finally cooling to room temperature to obtain the luminescent glass. The luminescent glass provided by the invention has high luminescent intensity and high luminescent efficiency. The preparation method provided by the invention has simple process, and is convenient to operate and easy to control; the product prepared by the preparation method has high luminescent intensity and high luminescent efficiency.

Description

Rare earth luminescence glass of doping simple substance silver and preparation method thereof
Technical field
The invention belongs to the luminescent material technical field, relate to a kind of fluorescent glass and preparation method thereof, relate in particular to rare earth luminescence glass of a kind of simple substance silver that mixes and preparation method thereof.
Background technology
Along with the development of semiconductor lighting technology (LED), be the daily life that the new light sources of representative has been come into us gradually with third generation semiconductor material gan.Under equal brightness, semiconductor illuminating light source current consumption only is 1/10 of ordinary incandescent lamp, and the life-span can reach more than 100,000 hours.As novel lighting engineering, plurality of advantages such as that LED has is energy-conservation, environmental protection, applying flexible can be widely used in fields such as various indications, demonstration, decoration, backlight and general lighting.Present business-like most of White-light LED illumination device adopts is that blue-light LED chip cooperates and is subjected to blue-light excitedly can send gold-tinted or fluorescent material green, orange light.This class fluorescent material has higher luminous efficiency, and preparation method's maturation.But the light source device that this method is made has following defective: the Resins, epoxy that (1) is used to encapsulate is easily aging, and reduce device lifetime; (2) complex process, cost is higher; (3) chromaticity coordinates instability, the easy drift of white light etc.
Than powder body material, can realize that under the royal purple optical excitation luminous glass then has significant advantage: (1) has good light transmittance; (2) good chemical stability and thermostability; (3) preparation technology is simple, and is with low cost; (4) make bulk and different shapes easily; (5) can the displaced loop epoxy resins, because these characteristics can realize that the luminous glass of high-performance is suitable as the luminescence medium material of LED lighting field very much.But because the network structure compactness of glass, the solid solubility of rare earth ion in glass network is lower; The phonon energy of glass is higher in addition, causes the radiationless recombination probability of Doped Rare Earth ionic very big, greatly reduces the radiative recombination probability of rare earth ion, thereby has caused rare earth ion luminous intensity in glass very weak, even not luminous.
Summary of the invention
The technical problem to be solved in the present invention is, has defective a little less than the luminous intensity at existing fluorescent glass in the prior art, and the rare earth luminescence glass of a kind of luminous intensity height, doping simple substance silver that luminous efficiency is high is provided.
The technical problem that the present invention further will solve is, provides a kind of technology product simple, easy to operate, easy to control, that prepare to have the rare earth luminescence glass of the doping simple substance silver of higher luminous intensity and higher luminous efficiency.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of rare earth luminescence glass of the simple substance silver that mixes is the material of following chemical formula: aSiO 2BAl 2O 3CCaOd NaFeCaF 2XEuF 3YAg 2O, wherein a, b, c, d, e, x, y are molfraction, their span is respectively: a is 25～50, b is 15～30, c is 0～10, d is 0～15, e is 5～30, x is 0.01～1, y is 0.01～1.
In the rare earth luminescence glass of described doping simple substance silver, the span of described a, b, c, d, e, x, y is respectively that a is 35～50, b is 20～30, c is 0～5, d is 5～10, e is 10～20, x is 0.1～1, y is 0.1～1.
The preparation method of the rare earth luminescence glass of doping simple substance silver may further comprise the steps:
(1), with SiO 2, Al 2O 3, CaCO 3, NaF, CaF 2, EuF 3And AgNO 3Be raw material, according to chemical formula aSiO 2BAl 2O 3CCaOd NaFeCaF 2XEuF 3YAg 2Molar ratio among the O between each element takes by weighing raw material, mix, wherein a, b, c, d, f, x, y are molfraction, and their span is respectively: a is 25～50, b is 15～30, c is 0～10, d is 0～15, e is 5～30, x is 0.01～1, y is 0.01～1;
(2), the raw material after will mixing is 1200～1500 ℃ of insulation fusings 0.5～3 hours down, the glass melt after the fusing is poured mould molding into;
(3), the glass after the moulding under reducing atmosphere, be heated to 300～550 ℃ of insulations and carried out the anneal first time in 0.5～5 hour;
(4), then remove reducing atmosphere and be warming up to 550～800 ℃ of insulations again and handle and to carry out anneal second time in 1～10 hour, cool to room temperature can be prepared fluorescent glass at last.
The preparation method of the rare earth luminescence glass of described doping simple substance silver, in the described step (1), the span of described a, b, c, d, e, x, y is respectively that a is 35～50, b is 20～30, c is 0～5, d is 5～10, e is 10～20, x is 0.1～1, y is 0.01～1.
The preparation method of the rare earth luminescence glass of described doping simple substance silver, in the described step (2), raw material after mixing is poured in corundum crucible or the platinum crucible, to install then and put into high temperature box furnace after the corundum crucible of material or platinum crucible are added a cover 1300～1400 ℃ of insulation fusings 1～2 hours down, the glass melt after the fusing is poured moulding on the pig mold into.
The preparation method of the rare earth luminescence glass of described doping simple substance silver, in the described step (3), the glass after the moulding is heated to 400～500 ℃ of insulations and carried out the anneal first time in 1～4 hour under reducing atmosphere.
The preparation method of the rare earth luminescence glass of described doping simple substance silver, in the described step (4), after first time anneal, remove reducing atmosphere and be warming up to 600～700 ℃ of insulations again and handle and carried out the anneal second time in 2～4 hours, last cool to room temperature can be prepared fluorescent glass.
The preparation method of the rare earth luminescence glass of described doping simple substance silver, described reducing atmosphere is the mixed gas of hydrogen, hydrogen and nitrogen, the atmosphere that carbon monoxide forms.
The preparation method of the rare earth luminescence glass of described doping simple substance silver, the purity of described raw material all is not less than analytical pure.
The rare earth luminescence glass of doping simple substance silver of the present invention has been owing to introduced Ag simple substance in rare earth luminescence glass, make rare earth ion effect in Ag simple substance and the glass, improved the luminous efficiency and the luminous intensity of fluorescent glass greatly.With respect to the rare earth luminescence glass of not introduced Ag simple substance, luminous efficiency of the present invention can improve more than 80%.
Among the preparation method of the rare earth luminescence glass of doping simple substance silver of the present invention, at first directly add Ag at the first step frit +Ion is by introducing Ag in glass in the process of founding +Ion, and then the glass of moulding carried out first anneal in reducing atmosphere, make the Ag that is entrained in the glass +Be reduced into metal A g simple substance particle, at last by the pattern and the size of suitable second annealing treating process control Ag simple substance particle, make it and rare earth ion between interact, thereby make the luminous enhancing of rare earth ion.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples, in the accompanying drawing:
Fig. 1 is embodiment 5 doping Ag +The emmission spectrum and the Ag that do not mix of fluorescent glass +The comparison diagram of emmission spectrum of fluorescent glass;
Fig. 2 is embodiment 6 doping Ag +The emmission spectrum and the Ag that do not mix of fluorescent glass +The comparison diagram of emmission spectrum of fluorescent glass.
Above-mentioned luminescent spectrum is to be that the detector analysis draws with Tianjin, island RF-5301PC spectrograph.
Embodiment
The rare earth luminescence glass of embodiment 1, doping simple substance silver is the material of following chemical formula: 25SiO 230Al 2O 310CaO15NaF20CaF 20.01EuF 31Ag 2O
Preparation method: take by weighing silicon-dioxide (SiO respectively 2) 6.15g, aluminum oxide (Al 2O 3) 12.54g, lime carbonate (CaCO 3) 4.1g, Sodium Fluoride (NaF) 2.58g, Calcium Fluoride (Fluorspan) (CaF 2) 6.4g, europium (EuF 3) 0.006g and Silver Nitrate (AgNO 3) 1.39g.With load weighted raw material in mortar ground and mixed evenly after, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1200 ℃ of fusings of high temperature box furnace, be incubated and after 3 hours glass melt poured on the pig mold, be pressed into transparent glass, again glass is placed annealing furnace, 95%N 2+ 5%H 2Be warmed up to 550 ℃ under the reducing atmosphere, be incubated after 5 hours, turn off 95%N 2+ 5%H 2Gas is warmed up to 700 ℃ of insulations then and turned off stove in 2 hours, cools to room temperature with the furnace, can prepare component and be: 25SiO 230Al 2O 310CaO15NaF20CaF 20.01EuF 31Ag 2The fluorescent glass of O.
The rare earth luminescence glass of embodiment 2, doping simple substance silver is the material of following chemical formula:
50SiO 2·15Al 2O 3·15NaF·20CaF 2·1EuF 3·0.01Ag 2O
Preparation method: take by weighing silicon-dioxide (SiO respectively 2) 13.38g, aluminum oxide (Al 2O 3) 6.81g, Sodium Fluoride (NaF) 2.8g, Calcium Fluoride (Fluorspan) (CaF 2) 6.95g, europium (EuF 3) 0.8g and Silver Nitrate (AgNO 3) 0.015g.With load weighted raw material in mortar ground and mixed evenly after, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1300 ℃ of fusings of high temperature box furnace, be incubated and after 2 hours glass melt poured on the pig mold, be pressed into transparent glass, again glass is placed annealing furnace, H 2Be warmed up to 300 ℃ under the reducing atmosphere, be incubated after 5 hours, turn off H 2Gas is warmed up to 550 ℃ of insulations then and turned off stove in 4 hours, cools to room temperature with the furnace, can prepare component and be: 50SiO 215Al 2O 315NaF20CaF 21EuF 30.01Ag 2The fluorescent glass of O.
The rare earth luminescence glass of embodiment 3, doping simple substance silver is the material of following chemical formula:
50SiO 2·30Al 2O 3·10CaO·10CaF 2·0.1EuF 3·0.5Ag 2O
Preparation method: take by weighing silicon-dioxide (SiO respectively 2) 12.15g, aluminum oxide (Al 2O 3) 12.37g, lime carbonate (CaCO 3) 4.04g, Calcium Fluoride (Fluorspan) (CaF 2) 3.15g, europium (EuF 3) 0.08g and Silver Nitrate (AgNO 3) 0.69g.With load weighted raw material in mortar ground and mixed evenly after, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1500 ℃ of fusings of high temperature box furnace, be incubated and after 0.5 hour glass melt poured on the pig mold, be pressed into transparent glass, again glass is placed annealing furnace, 95%N 2+ 5%H 2Be warmed up to 400 ℃ under the reducing atmosphere, be incubated after 4 hours, turn off 95%N 2+ 5%H 2Gas is warmed up to 800 ℃ of insulations then and turned off stove in 1 hour, cools to room temperature with the furnace, can prepare component and be: 50SiO 230Al 2O 310CaO10CaF 20.1EuF 30.5Ag 2The fluorescent glass of O.
The rare earth luminescence glass of embodiment 4, doping simple substance silver is the material of following chemical formula:
45SiO 2·30Al 2O 3·10CaO·10NaF·5CaF 2·0.1EuF 3·0.5Ag 2O
Preparation method: take by weighing silicon-dioxide (SiO respectively 2) 11.35g, aluminum oxide (Al 2O 3) 12.84g, lime carbonate (CaCO 3) 4.2g, Sodium Fluoride (NaF) 1.76g, Calcium Fluoride (Fluorspan) (CaF 2) 1.63g, europium (EuF 3) 0.4g and Silver Nitrate (AgNO 3) 0.71g.With load weighted raw material in mortar ground and mixed evenly after, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1400 ℃ of fusings of high temperature box furnace, be incubated and after 2 hours glass melt poured on the pig mold, be pressed into transparent glass, again glass is placed annealing furnace, 95%N 2+ 5%H 2Be warmed up to 500 ℃ under the reducing atmosphere, be incubated after 1 hour, turn off 95%N 2+ 5%H 2Gas is warmed up to 700 ℃ of insulations then and turned off stove in 4 hours, cools to room temperature with the furnace, can prepare component and be: 45SiO 230Al 2O 310CaO10NaF5CaF 20.1EuF 30.5Ag 2The fluorescent glass of O.
The rare earth luminescence glass of embodiment 5, doping simple substance silver is the material of following chemical formula:
40SiO 2·30Al 2O 3·5CaO·10NaF·15CaF 2·0.5EuF 3·0.25Ag 2O
Preparation method: take by weighing silicon-dioxide (SiO respectively 2) 9.81g, aluminum oxide (Al 2O 3) 12.49g, lime carbonate (CaCO 3) 2.03g, Sodium Fluoride (NaF) 1.71g, Calcium Fluoride (Fluorspan) (CaF 2) 4.78g, europium (EuF 3) 0.4g and Silver Nitrate (AgNO 3) 0.35g.With load weighted raw material in mortar ground and mixed evenly after, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1500 ℃ of fusings of high temperature box furnace, be incubated and after 1 hour glass melt poured on the pig mold, be pressed into transparent glass, again glass is placed annealing furnace, be warmed up to 550 ℃ under the CO gas reduction atmosphere, be incubated after 1 hour, turning off CO gas is warmed up to 700 ℃ of insulations then and turned off stove in 10 hours, cool to room temperature with the furnace, can prepare component and be: 40SiO 230Al 2O 35CaO10NaF15CaF 20.5EuF 30.25Ag 2The fluorescent glass of O.In order to contrast, we have adopted same forerunner's method for glass preparation and the subsequent heat treatment prepared AgNO that do not mix 3Sample.As shown in Figure 1, be that present embodiment prepares doping 0.25mol%AgNO 3AgNO does not mix 3The fluorescent glass of emission spectrum present embodiment preparation of sample at the emission spectrum down that excites of 394nm, mainly emission peak is at 440nm, 590nm and 610nm, doping AgNO 3The emissive porwer of sample than the AgNO that do not mix 3The integrated intensity of emission of sample improved 83%.
The rare earth luminescence glass of embodiment 6, doping simple substance silver is the material of following chemical formula:
40SiO 2·30Al 2O 3·5CaO·10NaF·15CaF 2·0.5EuF 3·0.2Ag 2O
Preparation method: take by weighing silicon-dioxide (SiO respectively 2) 9.81g, aluminum oxide (Al 2O 3) 12.49g, lime carbonate (CaCO 3) 2.03g, Sodium Fluoride (NaF) 1.71g, Calcium Fluoride (Fluorspan) (CaF 2) 4.78g, europium (EuF 3) 0.4g and Silver Nitrate (AgNO 3) 0.28g.With load weighted raw material in mortar ground and mixed evenly after, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1500 ℃ of fusings of high temperature box furnace, be incubated and after 1 hour glass melt poured on the pig mold, be pressed into transparent glass, again glass is placed annealing furnace, 95%N 2+ 5%H 2Be warmed up to 550 ℃ under the reducing atmosphere, be incubated after 5 hours, turn off 95%N 2+ 5%H 2Gas is warmed up to 700 ℃ of insulations then and turned off stove in 10 hours, cools to room temperature with the furnace, can prepare component and be: 40SiO 230Al 2O 35CaO10NaF15CaF 20.5EuF 30.2Ag 2The fluorescent glass of O.In order to contrast, we adopt to use the same method and have prepared the AgNO that do not mix 3Sample.As shown in Figure 2, be that present embodiment prepares doping 0.2mol%AgNO 3AgNO does not mix 3The fluorescent glass of emission spectrum present embodiment preparation of sample at the emission spectrum down that excites of 394nm, mainly emission peak is at 440nm, 590nm and 610nm, doping AgNO 3The emissive porwer of sample than the AgNO that do not mix 3The integrated intensity of emission of sample improved 108%.
The rare earth luminescence glass of embodiment 7, doping simple substance silver is the material of following chemical formula: 35SiO 220Al 2O 310CaO5NaF30CaF 20.01EuF 30.1Ag 2O
Preparation method: take by weighing silicon-dioxide (SiO respectively 2) 8.66g, aluminum oxide (Al 2O 3) 8.40g, lime carbonate (CaCO 3) 4.12g, Sodium Fluoride (NaF) 0.86g, Calcium Fluoride (Fluorspan) (CaF 2) 9.65g, europium (EuF 3) 0.006g and Silver Nitrate (AgNO 3) 0.13g.With load weighted raw material in mortar ground and mixed evenly after, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1500 ℃ of fusings of high temperature box furnace, be incubated and after 1 hour glass melt poured on the pig mold, be pressed into transparent glass, again glass is placed annealing furnace, 95%N 2+ 5%H 2Be warmed up to 550 ℃ under the reducing atmosphere, be incubated after 0.5 hour, turn off 95%N 2+ 5%H 2Gas is warmed up to 700 ℃ of insulations then and turned off stove in 2 hours, cools to room temperature with the furnace, can prepare component and be: 35SiO 220Al 2O 310CaO5NaF30CaF 20.01EuF 30.1Ag 2The fluorescent glass of O.

Claims (9)

1. the rare earth luminescence glass of the simple substance silver that mixes is characterized in that, is the material of following chemical formula: aSiO 2BAl 2O 3CCaOd NaFeCaF 2XEuF 3YAg 2O, wherein a, b, c, d, e, x, y are molfraction, their span is respectively: a is 25～50, b is 15～30, c is 0～10, d is 0～15, e is 5～30, x is 0.01～1, y is 0.01～1.
2. the rare earth luminescence glass of doping simple substance silver according to claim 1, it is characterized in that the span of described a, b, c, d, e, x, y is respectively: a is 35～50, b is 20～30, c is 0～5, d is 5～10, e is 10～20, x is 0.1～1, y is 0.1～1.
3. the preparation method of the rare earth luminescence glass of doping simple substance silver is characterized in that, may further comprise the steps:
(1), with SiO 2, Al 2O 3, CaCO 3, NaF, CaF 2, EuF 3And AgNO 3Be raw material, according to chemical formula aSiO 2BAl 2O 3CCaOd NaFeCaF 2XEuF 3YAg 2Molar ratio among the O between each element takes by weighing raw material, mix, wherein a, b, c, d, f, x, y are molfraction, and their span is respectively: a is 25～50, b is 15～30, c is 0～10, d is 0～15, e is 5～30, x is 0.01～1, y is 0.01～1;
(2), the raw material after will mixing is 1200～1500 ℃ of insulation fusings 0.5～3 hours down, the glass melt after the fusing is poured mould molding into;
(3), the glass after the moulding under reducing atmosphere, be heated to 300～550 ℃ of insulations and carried out the anneal first time in 0.5～5 hour;
(4), then remove reducing atmosphere and be warming up to 550～800 ℃ of insulations again and handle and to carry out anneal second time in 1～10 hour, cool to room temperature can be prepared fluorescent glass at last.
4. the preparation method of the rare earth luminescence glass of doping simple substance silver according to claim 3, it is characterized in that, in the described step (1), the span of described a, b, c, d, e, x, y is respectively that a is 35～50, b is 20～30, c is 0～5, d is 5～10, e is 10～20, x is 0.1～1, y is 0.1～1.
5. the preparation method of the rare earth luminescence glass of doping simple substance silver according to claim 3, it is characterized in that, in the described step (2), raw material after mixing is poured in corundum crucible or the platinum crucible, to install then and put into high temperature box furnace after the corundum crucible of material or platinum crucible are added a cover 1300～1400 ℃ of insulation fusings 1～2 hours down, the glass melt after the fusing is poured moulding on the pig mold into.
6. the preparation method of the rare earth luminescence glass of doping simple substance silver according to claim 3 is characterized in that, in the described step (3), the glass after the moulding is heated to 400～500 ℃ of insulations and carried out the anneal first time in 1～4 hour under reducing atmosphere.
7. the preparation method of the rare earth luminescence glass of doping simple substance silver according to claim 3, it is characterized in that, in the described step (4), after first time anneal, the removal reducing atmosphere is warming up to 600～700 ℃ of insulation processing again and carried out the anneal second time in 2～4 hours, last cool to room temperature can be prepared fluorescent glass.
8. according to the preparation method of the rare earth luminescence glass of any described doping simple substance silver of claim 3～7, it is characterized in that described reducing atmosphere is the mixed gas of hydrogen, hydrogen and nitrogen, the atmosphere that carbon monoxide forms.
9. according to the preparation method of the rare earth luminescence glass of any described doping simple substance silver of claim 3～7, it is characterized in that the purity of described raw material all is not less than analytical pure.
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CN102674693A (en) * 2012-06-06 2012-09-19 大连海事大学 Full-color emission glass phosphor and preparation method thereof
CN103274598A (en) * 2013-06-06 2013-09-04 昆明理工大学 Efficient white light emission glass containing silver nanoparticles, and preparation method thereof
CN103342464A (en) * 2013-07-03 2013-10-09 同济大学 Silver-containing nanocrystal blue light enhanced tellurite glass and preparation method thereof
CN104817268A (en) * 2015-04-21 2015-08-05 同济大学 Preparation method and luminescent glass capable of efficiently extracting size-controllable Ag nano particles under low-concentration AgNO3 doping condition
CN106316373A (en) * 2016-07-29 2017-01-11 江苏罗化新材料有限公司 Preparing method for high power illuminant fluoride florescent and crystalline ceramics
CN109437557A (en) * 2018-12-25 2019-03-08 浙江大学 A kind of cluster doped fluorphosphate glass of green white fluorescence silver content and preparation method thereof based on non-bridging oxygen coordination
CN110304831A (en) * 2019-07-22 2019-10-08 中国科学院上海光学精密机械研究所 Dy-Ag is co-doped with silicate Anti-splash glass sheet and preparation method thereof

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CN1785870A (en) * 2005-10-28 2006-06-14 宁波大学 Rare earth ion doped YAG micro crystalline glass and its preparation method

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CN1785870A (en) * 2005-10-28 2006-06-14 宁波大学 Rare earth ion doped YAG micro crystalline glass and its preparation method

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CN102674693A (en) * 2012-06-06 2012-09-19 大连海事大学 Full-color emission glass phosphor and preparation method thereof
CN103274598A (en) * 2013-06-06 2013-09-04 昆明理工大学 Efficient white light emission glass containing silver nanoparticles, and preparation method thereof
CN103274598B (en) * 2013-06-06 2015-11-11 昆明理工大学 A kind of efficient white light launches glass of silver-containing nanoparticles and preparation method thereof
CN103342464A (en) * 2013-07-03 2013-10-09 同济大学 Silver-containing nanocrystal blue light enhanced tellurite glass and preparation method thereof
CN104817268A (en) * 2015-04-21 2015-08-05 同济大学 Preparation method and luminescent glass capable of efficiently extracting size-controllable Ag nano particles under low-concentration AgNO3 doping condition
CN104817268B (en) * 2015-04-21 2017-07-11 同济大学 Low concentration AgNO3Fluorescent glass of the controllable Ag nano particles of yardstick and preparation method thereof is efficiently separated out under doping condition
CN106316373A (en) * 2016-07-29 2017-01-11 江苏罗化新材料有限公司 Preparing method for high power illuminant fluoride florescent and crystalline ceramics
CN109437557A (en) * 2018-12-25 2019-03-08 浙江大学 A kind of cluster doped fluorphosphate glass of green white fluorescence silver content and preparation method thereof based on non-bridging oxygen coordination
CN110304831A (en) * 2019-07-22 2019-10-08 中国科学院上海光学精密机械研究所 Dy-Ag is co-doped with silicate Anti-splash glass sheet and preparation method thereof
CN110304831B (en) * 2019-07-22 2021-11-30 中国科学院上海光学精密机械研究所 Dy-Ag co-doped silicate anti-sputtering plate glass and preparation method thereof

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