CN101613183B - Long-wave broadband ultraviolet excited multi-functional fluorescent glass and preparation method thereof - Google Patents

Long-wave broadband ultraviolet excited multi-functional fluorescent glass and preparation method thereof Download PDF

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CN101613183B
CN101613183B CN2009100488921A CN200910048892A CN101613183B CN 101613183 B CN101613183 B CN 101613183B CN 2009100488921 A CN2009100488921 A CN 2009100488921A CN 200910048892 A CN200910048892 A CN 200910048892A CN 101613183 B CN101613183 B CN 101613183B
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fluorescent glass
long
preparation
ultraviolel
wave broadband
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CN101613183A (en
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余锡宾
杨绪勇
周永勤
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Shanghai Normal University
University of Shanghai for Science and Technology
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Shanghai Normal University
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Abstract

The present invention relates to a long-wave broadband ultraviolet excited multi-functional fluorescent glass and a preparation method thereof; the glass comprises SiO2-aAl2O3-bB2O3-cRexOy; wherein, x=1 or 2, y=1 or 3, A=0.05 to 5, B=0 to 2.5, C=0.01 to 0.2 and x, y, A, B and C are molar ratio; RexOy is EuO, Eu2O3 or Tb2O3. By using the preparation method of the invention, high transparent multi-functional fluorescent glass can be prepared under a simpler process conditions, the fluorescent glass has very strong 250nm-420nm of ultraviolet light absorption capacity and the emission of red, green, blue and white lights can be realized by regulating the production process. The fluorescent glass can be used as the source of three primary colours in the white light light-emitting diode (LED), the laser diode (LD) and the displays and is likely to be used in ultra large screen color displays.

Description

Multi-functional fluorescent glass of long-wave broadband burst of ultraviolel and preparation method thereof
Technical field
The present invention relates to the luminescent material technical field, specifically multi-functional fluorescent glass of long-wave broadband burst of ultraviolel and preparation method thereof.
Background technology
That glass has is even, transparent, hard, good anti-corrosion and series of characteristics such as electricity, optics, enough multiple shapings of energy and working method are made the goods of different shape and size, can change its character by adjusting chemical constitution, to adapt to different service requirementss.The optoelectronic component of many keys in modern information industry all is to be made by the glass with specific optical functionalities as iatron spare, amplifying device, displaying device etc.In addition, because its special networks structure is a short-range order and long-range is unordered,, luminous very even so the doping dispersiveness of rare earth ion in glass is better relatively.Make first after the novel optical glass that contains lanthanum, thorium, the contour refraction of tantalum, low scattering since Corning Incorporated, rare earth opticglass has obtained very fast development, can make the special glass of different purposes by the doping of rare earth ion.But the synthetic fluorescent glass is mainly rare earth ion doped silicate glass at present, and absorption spectrum is narrower and brightness is not high, has been subjected to very big restriction in application facet.
Summary of the invention
The objective of the invention is to prepare a kind of multi-functional fluorescent glass that the long-wave broadband UV-light is sent red, green, blue and white light that absorbs, its luminous efficiency height, the preparation method is simple, and is with low cost.
The invention provides a kind of multi-functional fluorescent glass of long-wave broadband burst of ultraviolel, its composition is represented by following general formula: SiO 2AAl 2O 3BB 2O 3CRe xO y, wherein, a=0.05～0.5, b=0～2.5, c=0.01～0.2 is mol ratio; Re xO yBe EuO, Eu 2O 3Or Tb 2O 3
In fluorescent glass of the present invention, with zeolite as base starting material, utilize the sodium ion in europium ion, inferior europium ion or the terbium ion replacement mesoporous zeolite, europium element or terbium element can send red, green, blue and white light as luminescent activator under the long-wave broadband burst of ultraviolel.
To achieve the above object of the invention, the present invention is achieved by following concrete grammar:
(1) mesoporous zeolite and europium salt or terbium salt solution mix is even, the mol ratio of sodium element in the mesoporous zeolite and europium ion or terbium ion is 1: (0.5～2); Stir after 0.5～2 hour, be incubated 12～48 hours down, make the sodium element in europium ion or the terbium ion replacement mesoporous zeolite at 60～90 ℃; Supernatant liquor is removed in centrifugation, gets the precipitation oven dry and obtains precursor;
(2) with the precursor and the SiO that obtain 2Or H 3BO 3Thorough mixing promptly gets target product behind 1300～1600 ℃ of following sintering 6～10h; Precursor is in mesoporous zeolite, with SiO 2Or H 3BO 3Mol ratio is 1: (1～10).
Described sintering is at air atmosphere or N 2/ H 2Carry out under the mixed-gas atmosphere.
Specifically, obtain SiO at sintering under air atmosphere 2AAl 2O 3BB 2O 3CEu 2O 3Or SiO 2AAl 2O 3BB 2O 3CTb 2O 3N 2/ H 2The mixed-gas atmosphere sintering obtains SiO 2AAl 2O 3BB 2O 3CEuO; N 2/ H 2In the mixed gas, H 2Volume percent is 5%～20%.
Described europium salt is Europium trichloride or europium nitrate, and described terbium salt is terbium chloride or Terbium trinitrate.
Described europium salt or terbium concentration of salt solution are 0.05～1M.
Described mesoporous zeolite is 13X or 4A type zeolite.
The present invention adopts liquid phase method in conjunction with high temperature solid-state method, obtain a kind of multi-functional fluorescent glass that the long-wave broadband UV-light is sent red, green, blue and white light that absorbs, this fluorescent glass luminous efficiency height, and have very high chemistry and an optical stability, can be used for the source of the three primary colours in white light emitting device (LED), laser diode (LD) and the indicating meter that 370-420nm excites, can in the jumbotron color monitor, obtain to use.
Compared with prior art, the present invention has following beneficial effect:
1) the present invention has realized that first zeolite is the multi-functional fluorescent glass of the long-wave broadband burst of ultraviolel of matrix.Zeolite is a kind of mesoporous material, have high specific surface area and special pore structure, rare-earth activated dose of ionic group installed in the zeolite, and the fluorescence concentration quenching that can effectively avoid the reunion of activator to cause can effectively improve effciency of energy transfer and luminous efficiency between activator and the matrix.
2) the multi-functional fluorescent glass transparency height of long-wave broadband burst of ultraviolel of the present invention can be extended to the long wave ultraviolet region to the absorption broad of ultraviolet region, and luminous efficiency and range of application are higher than general commercial fluorescent glass at present.
3) preparation technology of the present invention is simple to operation, and raw material is cheap and easy to get, is fit to suitability for industrialized production, and reaction process does not have three industrial wastes substantially, has characteristics such as environmental protection, less energy-consumption, high benefit.
Description of drawings
Fig. 1 is the blue luminescent glass fluorescence spectrum figure of embodiment 7 wide band ultraviolet excitations
Fig. 2 is the green luminous glass fluorescence spectrum figure of embodiment 8 wide band ultraviolet excitations
Fig. 3 is the emitting red light glass fluorescence spectrum figure of embodiment 1 wide band ultraviolet excitation
Fig. 4 is the white luminous glass fluorescence spectrum figure of embodiment 6 wide band ultraviolet excitations
(in the above-mentioned spectrogram, the line on the left side is represented excitation spectrum, and the line on the right is represented emmission spectrum)
Embodiment
Further specify the present invention by the following examples.But should be understood that these examples are exemplary, the present invention is not limited to this.
Embodiment 1
Get 0.0035mol 13X type zeolite (Na 2OAl 2O 32.8SiO 26H 2O) the 0.1mol/L EuCl of input 30ml 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 24 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.4211gSiO that obtains 2Behind the thorough mixing, put into the 30mL crucible, promptly get target product after placing 1500 ℃ of following sintering 8h of High Temperature Furnaces Heating Apparatus air atmosphere.Measuring it with ultimate analysis (ICP) consists of: SiO 20.21Al 2O 30.08Eu 2O 3, have high-clarity, glow under the 380nm UV-irradiation.
Embodiment 2
Get 0.0035mol 13X type zeolite Na 2OAl 2O 32.8SiO 26H 2O drops into the 0.5mol/L EuCl of 30ml 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 20 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.4211g SiO that obtains 2Behind the thorough mixing, put into the 30mL crucible, promptly get target product after placing 1450 ℃ of following sintering 10h of High Temperature Furnaces Heating Apparatus air atmosphere.Measuring it with ultimate analysis (ICP) consists of it and consists of SiO 20.21Al 2O 30.12Eu 2O 3, glow under the 380nm UV-irradiation.
Embodiment 3
Get 0.004mol 4A type zeolite Na 2OAl 2O 32SiO 24.5H 2O drops into the 0.1mol/L EuCl of 30ml 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 24 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.004mol SiO that obtains 2Behind the thorough mixing, put into the 30mL crucible, promptly get target product after placing 1450 ℃ of following sintering 10h of High Temperature Furnaces Heating Apparatus air atmosphere.Measure it with ultimate analysis (ICP) and consist of SiO 20.33Al 2O 30.11Eu 2O 3, glow under the 380nm UV-irradiation.
Embodiment 4
Get 0.004mol 4A type zeolite Na 2OAl 2O 32SiO 24.5H 2O drops into the 0.1mol/L EuCl of 30ml 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 24 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.004mol SiO that obtains 2Behind the thorough mixing, put into the 30mL crucible, place High Temperature Furnaces Heating Apparatus at N 2/ H 2(5%H 2+ 95%N 2) promptly get target product behind the following 1500 ℃ of following sintering 8h of atmosphere.Measure it with ultimate analysis (ICP) and consist of SiO 20.33Al 2O 30.092EuO, blue light-emitting under the 380nm UV-irradiation.
Embodiment 5
Get 0.0035mol 13X type zeolite Na 2OAl 2O 32.8SiO 26H 2O drops into the 0.1mol/L EuCl of 30ml 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 24 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.4333gH that obtains 3BO 3(0.007mol) behind the thorough mixing, put into the 30mL crucible, promptly get target product after placing 1300 ℃ of following sintering 10h of High Temperature Furnaces Heating Apparatus.Measure it with ultimate analysis (ICP) and consist of SiO 20.36Al 2O 30.357B 2O 30.061 Eu 2O 3, glow under the 380nm UV-irradiation.
Embodiment 6
Get the 0.1mol/L EuCl that 0.0035mol 13X type zeolite drops into 30ml 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 18 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.4211gSiO that obtains 2(0.007mol) behind the thorough mixing, put into the 30mL crucible, place High Temperature Furnaces Heating Apparatus at N 2/ H 2(15%H 2+ 85%N 2) promptly get target product behind the following 1500 ℃ of following sintering 8h of atmosphere.Measure it with ultimate analysis (ICP) and consist of SiO 20.21Al 2O 30.16EuO, emit white light under the 380nm UV-irradiation.
Embodiment 7
Get the 0.5mol/L EuCl that 13X type zeolite 0.0035mol drops into 30ml 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 20 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.2106gSiO that obtains 2(0.0035mol) behind the thorough mixing, put into the 30mL crucible, place High Temperature Furnaces Heating Apparatus at N 2/ H 2(20%H 2+ 80%N 2) promptly get target product behind the following 1450 ℃ of following sintering 8h of atmosphere.Measure it with ultimate analysis (ICP) and consist of SiO 20.26Al 2O 30.18EuO, blue light-emitting under the 380nm UV-irradiation.
Embodiment 8
Get the 0.1mol/L Tb (NO that 13X type zeolite 0.0035mol drops into 35ml 3) 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 18 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.4211gSiO that obtains 2(0.007mol) behind the thorough mixing, put into the 30mL crucible, promptly get target product after placing 1500 ℃ of following sintering 8h of High Temperature Furnaces Heating Apparatus air atmosphere.Measuring it with ultimate analysis (ICP) consists of: SiO 20.21Al 2O 30.072Tb 2O 3, green light under the 380nm UV-irradiation.
Embodiment 9
Get the 0.1mol/L Tb (NO that 13X type zeolite 0.0035mol drops into 35ml 3) 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 20 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.6317gSiO that obtains 2(0.0105mol) behind the thorough mixing, put into the 30mL crucible, promptly get target product after placing 1500 ℃ of following sintering 10h of High Temperature Furnaces Heating Apparatus air atmosphere.Measuring it with ultimate analysis (ICP) consists of: SiO 20.172Al 2O 30.043Tb 2O 3, green light under the 380nm UV-irradiation.
Embodiment 10
Get 13X type zeolite Na 2OAl 2O 32.8SiO 26H 2O 0.0035mol drops into the 0.1mol/L Eu (NO of 35ml 3) 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 30 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.4211gSiO that obtains 2(0.007mol) behind the thorough mixing, put into the 30mL crucible, promptly get target product after placing 1550 ℃ of following sintering 6h of High Temperature Furnaces Heating Apparatus air atmosphere.Measure it with ultimate analysis (ICP) and consist of SiO 20.21Al 2O 30.063Eu 2O 3, glow under the 380nm UV-irradiation.
Embodiment 11
Get 13X type zeolite Na 2OAl 2O 32.8SiO 26H 2O 0.0035mol drops into the 0.1mol/L EuCl of 35ml 3In the solution, stirred 2 hours, place 80 ℃ of water-baths 30 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 1.8951gSiO that obtains 2(0.0315mol) behind the thorough mixing, put into the 30mL crucible, promptly get target product after placing 1500 ℃ of following sintering 9h of High Temperature Furnaces Heating Apparatus air atmosphere.Measure it with ultimate analysis (ICP) and consist of SiO 20.085Al 2O 30.024Eu 2O 3, glow under the 380nm UV-irradiation.
Embodiment 12
Get 4A type zeolite 0.004mol (Na 2OAl 2O 32SiO 24.5H 2O) the 0.1mol/L EuCl of input 30ml 3In the solution, stirred 1 hour, place 80 ℃ of water-baths 24 hours, supernatant liquor is removed in centrifugation, and the baking oven of putting into 100 ℃ is dried.With precursor and the 0.036mol H that obtains 3BO 3Behind the thorough mixing, put into the 30mL crucible, place High Temperature Furnaces Heating Apparatus promptly getting target product behind 1500 ℃ of following sintering 8h under the air atmosphere.Measure it with ultimate analysis (ICP) and consist of SiO 20.5Al 2O 32.25B 2O 30.1 Eu 2O 3, glow under the 380nm UV-irradiation.

Claims (7)

1. the multi-functional fluorescent glass of a long-wave broadband burst of ultraviolel is characterized in that, forms and is represented by following general formula: SiO 2AAl 2O 3BB 2O 3CRe xO y
Wherein, a=0.085～0.5, b=0～2.25, c=0.024～0.18 is mol ratio; Re xO yBe EuO, Eu 2O 3Or Tb 2O 3
2. the preparation method of the multi-functional fluorescent glass of the described a kind of long-wave broadband burst of ultraviolel of claim 1 is characterized in that, comprises the steps:
(1) mesoporous zeolite and europium salt or terbium salt solution mix is even, the mol ratio of sodium element in the mesoporous zeolite and europium ion or terbium ion is 1: (0.5～2); Stir after 0.5～2 hour, be incubated 12～48 hours down at 60～90 ℃, supernatant liquor is removed in centrifugation, gets the precipitation oven dry and obtains precursor;
(2) with the precursor and the SiO that obtain 2Or H 3BO 3Thorough mixing promptly gets target product behind 1300～1600 ℃ of following sintering 6～10h; Precursor is in mesoporous zeolite, with SiO 2Or H 3BO 3Mol ratio is 1: (1～10).
3. the preparation method of the multi-functional fluorescent glass of the described a kind of long-wave broadband burst of ultraviolel of claim 2 is characterized in that, described mesoporous zeolite is 13X or 4A type zeolite.
4. the preparation method of the multi-functional fluorescent glass of the described a kind of long-wave broadband burst of ultraviolel of claim 2 is characterized in that, described europium salt is Europium trichloride or europium nitrate, and described terbium salt is terbium chloride or Terbium trinitrate.
5. the preparation method of the multi-functional fluorescent glass of claim 2 or 4 described a kind of long-wave broadband burst of ultraviolel is characterized in that, described europium salt or terbium concentration of salt solution are 0.05～1mol/L.
6. the preparation method of the multi-functional fluorescent glass of the described a kind of long-wave broadband burst of ultraviolel of claim 2 is characterized in that, described sintering is at air atmosphere or N 2/ H 2Carry out under the mixed-gas atmosphere.
7. the preparation method of the multi-functional fluorescent glass of the described a kind of long-wave broadband burst of ultraviolel of claim 6 is characterized in that, described N 2/ H 2In the mixed gas, H 2Volume percent is 5%～20%.
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CN102173583B (en) * 2010-11-29 2013-02-20 天津理工大学 Rare earth activated white light luminescent glass material as well as preparation method and application thereof
CN111646703A (en) * 2020-05-18 2020-09-11 东华大学 Fluoride/oxyfluoride fluorescent glass ceramic and preparation method and application thereof
CN111847883A (en) * 2020-08-31 2020-10-30 贵州赛义光电科技有限公司 Fluorescent glass ceramic and preparation method thereof

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