CN111892924B - Cu ion doped gallate base orange red luminescent material and preparation method thereof - Google Patents

Cu ion doped gallate base orange red luminescent material and preparation method thereof Download PDF

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CN111892924B
CN111892924B CN202010816657.0A CN202010816657A CN111892924B CN 111892924 B CN111892924 B CN 111892924B CN 202010816657 A CN202010816657 A CN 202010816657A CN 111892924 B CN111892924 B CN 111892924B
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luminescent material
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red luminescent
doped gallate
barium
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CN111892924A (en
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屈冰雁
赵宁
赵靖
王彩路
刘梅真
许育东
周如龙
蒋阳
陈雷
王雷
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Hefei University of Technology
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    • C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
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Abstract

The invention discloses a Cu ion doped gallate-based orange red luminescent material and a preparation method thereof. After being excited by an ultraviolet/visible light source, the Cu ion doped gallate based orange red luminescent material has good long afterglow performance, and the longest long afterglow life can reach 56 minutes. The synthesized luminescent material is excited by an ultraviolet/visible light source and emits orange-red fluorescent light, can obtain broadband emission of 500-800 nm, can be used as a fluorescent lamp in the fields of illumination, LED and electronic device display and the like, and can also be used in the fields of decoration, building materials, coatings and the like. The invention has the advantages of stable material performance, stable and reliable process conditions, high luminous efficiency, simple preparation method and the like.

Description

Cu ion doped gallate base orange red luminescent material and preparation method thereof
Technical Field
The invention relates to the field of luminescent materials, in particular to a Cu ion doped gallate base orange red luminescent material and a preparation method thereof.
Background
The photoluminescent material has the characteristics of light absorption, light emission, storage and re-light emission, can realize continuous light emission after being excited by an ultraviolet/visible light source, is a novel green clean energy source, and is widely applied to emergency display, coating and decoration. With the development of long-afterglow material systems, the application fields of the materials are gradually increased and gradually expanded to the application fields of information storage, high-energy ray detection, biology and the like, so that the materials are concerned by a plurality of researchers. In the long afterglow materials, the preparation process of the luminescent materials such as blue, green and the like is mature day by day, and the long afterglow materials which emit light in red, orange, yellow and other long wave bands have poor luminescent performance, thus seriously hindering the multi-colorization process of the long afterglow materials. Therefore, it is of great significance to develop a long afterglow material which can be excited by near ultraviolet/visible light and emits light in red, orange, yellow and other long wavelength bands.
Most of the currently practical long-afterglow luminescent materials need to be doped with rare earth metal elements, but the related raw materials of rare earth ions are expensive, and part of the raw materials can generate toxic and harmful substances in the production process; some luminescent materials are usually prepared under conditions of high pressure, reducing or protective atmosphere. In contrast, the transition metal ion activated luminescent material has cheap and easily available raw materials and has more industrial development potential than the rare earth metal ions in the field of luminescence. Therefore, the research and development of a novel long-afterglow luminescent material doped with transition ions becomes a hotspot for the attention and research in the field.
In addition, in the prior art, the luminescent materials doped with Cu ions are mainly green and blue luminescent materials, such as ZnS: Cu, SrS: Cu, Na2Zn(PO4)Cl:Cu、SnO2:Cu、YAG:Cu、(H3O)Al3(SO4)2(OH)6:Cu、Li2NaBF6:Cu、Li2B4O7:Cu、SrAl2O4The emission band of the luminescent materials such as Cu is mainly in the green or blue region, and the high-efficiency luminescent materials with the luminescent position in the orange-red region are not reported. Therefore, the research and development of the orange-red long-afterglow luminescent material doped with the transition metal Cu ions becomes the focus of the current research.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a Cu ion doped gallate based orange-red luminescent material doped with transition metal Cu ions, which has better afterglow brightness and longer afterglow time, and the emission waveband of the Cu ion doped gallate based orange-red luminescent material is positioned in a red region, and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme: a Cu ion doped gallate base orange red luminescent material is prepared by mixing barium-containing compound, gallium-containing compound and copper-containing compound and sintering.
Further, the Cu ion-doped gallate-based orange red luminescent material is prepared by mixing BaGa2O4As a substrate, Cu ions are used as activating ions.
Further, the chemical structural formula is Ba(1-x)CuxGa2O4Wherein x is 0.01-0.08.
Further, the barium-containing compound is at least one of barium oxide, barium carbonate, barium oxalate, barium acetate, barium nitrate and barium hydroxide.
Further, the gallium-containing compound is at least one of an oxide, a carbonate, an oxalate, an acetate, a nitrate and a hydroxide of gallium.
Further, the copper-containing compound is at least one of copper oxide, carbonate, oxalate, acetate, nitrate and hydroxide.
The invention also provides a preparation method of the Cu ion doped gallate based orange red luminescent material, which comprises the following steps: and mixing a barium-containing compound, a gallium-containing compound and a copper-containing compound, sintering in air or an oxygen-containing atmosphere, and cooling along with the furnace to obtain the Cu ion-doped gallate-based orange-red luminescent material.
Further, the sintering process specifically comprises: keeping the temperature for 5-8 h at 1200-1500 ℃.
The invention has the beneficial effects that:
1. the Cu ion doped gallate based orange red luminescent material takes Cu ions as a luminescent center, and BaGa2O4As a substrate, Cu ions are doped to enter Ba mainly2+The substitutional doping is realized through lattice positions, after ultraviolet/visible light excitation, the material has broadband emission within the wavelength range of 500-800 nm, and the highest peak value of the emission is within the wavelength range of 600-630 nm, so that orange red emission is shown.
In the present inventionIn the course of research, the inventors tried BaO or Ga2O3To replace BaGa2O4As a substrate, it was found that both Cu-doped BaO and Ga2O3In the above-mentioned manner, no luminescence occurred in any of the obtained materials, and therefore, it was concluded that BaGa2O4The substrate is an indispensable factor of the material for emitting orange-red light, and the luminescent property of the Cu ion doped gallate based orange-red luminescent material is that a proper amount of Cu ions are doped in BaGa2O4Realized by a matrix.
2. After being excited by an ultraviolet/visible light source, the Cu ion doped gallate based orange red luminescent material has better afterglow brightness and longer afterglow time, and the long afterglow life can reach 56 minutes at most (in the red long afterglow luminescent material in the prior art, rare earth ions are mainly used as an activator), so that the red long afterglow luminescent material activated by transition metal ions is more rare and has good application prospect.
3. The Cu ion doped gallate based orange red luminescent material does not adopt rare earth as a luminescent center, utilizes Cu which is widely supplied as an active ion, is doped in gallate, and has an emission main peak positioned in an orange red wave band, and the luminescent property is greatly different from the luminescent property of the Cu doped luminescent material related to the prior literature or patent, thereby expanding the research range of the material.
4. The preparation method of the Cu ion doped gallate base orange red luminescent material is carried out in air or oxygen-containing atmosphere, and reducing atmosphere is not needed, so that the performance requirement on production equipment is greatly reduced, the production cost is also reduced, and the safety in the production process is improved.
Drawings
BaGa in the lower part of figure 12O4The upper part of the XRD spectrum corresponding to the standard card of (1) is Ba prepared in the example 2 of the invention0.985Cu0.015Ga2O4XRD pattern of the luminescent material.
Fig. 2 is a diagram of a Cu ion-doped gallate-based orange red luminescent material prepared in example 2 of the present invention, fig. 2a, 2b, and 2c are SEM (scanning electron microscope) images at different magnifications, fig. 2b is a portion selected and magnified in fig. 2a, fig. 2c is a portion selected and magnified in fig. 2b, fig. 2d is an EDS (X-ray spectroscopy) diagram of scanning a selected portion of fig. 2c, and fig. 2e is a distribution diagram of Ba, Ga, O, and Cu elements of the selected portion scanned in fig. 2 c.
Fig. 3 is an excitation spectrum of a Cu ion-doped gallate-based orange-red luminescent material prepared in each example of the present invention.
Fig. 4 is an emission spectrum of a Cu ion-doped gallate-based orange-red luminescent material prepared in each example of the present invention.
FIG. 5 shows Ba prepared in example 3 of the present invention0.98Cu0.02Ga2O4Long afterglow life decay curve.
Fig. 6 is a trend graph of afterglow life of the Cu ion-doped gallate-based orange-red luminescent material prepared in the embodiment of the present invention.
Detailed Description
The present invention will be described in detail with reference to examples.
The various starting materials used in the following examples are all commercially available products known in the art unless otherwise specified.
Example 1
Cu ion doped gallate base orange red luminescent material Ba0.99Cu0.01Ga2O4The preparation method comprises the following steps:
mixing BaCO3、Ga2O3CuO as a raw material, according to BaCO3:Ga2O3Mixing CuO in a molar ratio of 99:100:1, putting the mixture into an agate mortar, fully grinding the mixture to uniformly mix the mixture to obtain a mixture, putting the mixture into a muffle furnace for sintering, heating the mixture to 1350 ℃ from room temperature, preserving the heat for 6 hours at the temperature of 1350 ℃, cooling the mixture to the room temperature after the heat preservation is finished to obtain Ba0.99Cu0.01Ga2O4And (3) carrying out the whole sintering process in an air atmosphere on the orange-red fluorescent material finished product.
The Cu ion-doped gallate-based orange red luminescent material Ba prepared in the embodiment0.99Cu0.01Ga2O4Excitation and emission ofThe spectra are shown in fig. 3 and 4, and it can be seen from fig. 3 and 4 that the excitation peak of the material is 353nm, the emission peak is 625nm, and the emission intensity at the highest peak position of the emission peak is about 195 counting intensities.
Example 2
Cu ion doped gallate base orange red luminescent material Ba0.985Cu0.015Ga2O4The preparation method comprises the following steps:
mixing BaCO3、Ga2O3CuO as a raw material, according to BaCO3:Ga2O3Mixing CuO with a molar ratio of 98.5:100:1.5, putting the mixture into an agate mortar, fully grinding the mixture to be uniformly mixed to obtain a mixture, putting the mixture into a muffle furnace for sintering, heating the mixture to 1350 ℃ from room temperature, preserving the heat for 6 hours at 1350 ℃, cooling the mixture to room temperature after the heat preservation is finished to obtain Ba0.985Cu0.015Ga2O4And (3) carrying out the whole sintering process in an air atmosphere on the orange-red fluorescent material finished product.
The Cu ion-doped gallate-based orange red luminescent material Ba prepared in the embodiment0.985Cu0.015Ga2O4The excitation and emission spectra of (A) are shown in FIGS. 3 and 4, and it can be seen from FIGS. 3 and 4 that the excitation peak of the material is located at 350nm, the emission peak is located at 607nm, and the luminescence intensity at the highest peak position of the emission peak is around 780 count intensities.
Example 3
Cu ion doped gallate base orange red luminescent material Ba0.98Cu0.02Ga2O4The preparation method comprises the following steps:
mixing BaCO3、Ga2O3CuO as a raw material, according to BaCO3:Ga2O3Mixing CuO in a molar ratio of 98:100:2, putting the mixture into an agate mortar, fully grinding the mixture to uniformly crush and mix the mixture to obtain a mixture, putting the mixture into a muffle furnace for sintering, heating the mixture to 1350 ℃ from room temperature, preserving the heat for 6 hours at the temperature of 1350 ℃, cooling the mixture to the room temperature after the heat preservation is finished to obtain Ba0.98Cu0.02Ga2O4And (3) carrying out the whole sintering process in an air atmosphere on the orange-red fluorescent material finished product.
The Cu ion-doped gallate-based orange red luminescent material Ba prepared in the embodiment0.98Cu0.02Ga2O4The excitation and emission spectra of the material are shown in fig. 3 and 4, and it can be seen from fig. 3 and 4 that the excitation peak of the material is at 353nm, the emission peak is at 621nm, and the luminescence intensity at the highest peak position of the emission peak is around 604 count intensities.
Example 4
Cu ion doped gallate base orange red luminescent material Ba0.97Cu0.03Ga2O4The preparation method comprises the following steps:
mixing BaCO3、Ga2O3CuO as a raw material, according to BaCO3:Ga2O3Mixing CuO in a molar ratio of 97:100:3, putting the mixture into an agate mortar, fully grinding the mixture to uniformly crush and mix the mixture to obtain a mixture, putting the mixture into a muffle furnace for sintering, heating the mixture to 1200 ℃ from room temperature, preserving the heat at 1200 ℃ for 8 hours, cooling the mixture to room temperature after the heat preservation is finished to obtain Ba0.97Cu0.03Ga2O4The whole sintering process of the orange-red long afterglow fluorescent material finished product is carried out in the air atmosphere.
The Cu ion doped gallate based orange red luminescent material Ba prepared in the embodiment0.97Cu0.03Ga2O4The excitation and emission spectra of (a) are shown in fig. 3 and 4, and it can be seen from fig. 3 and 4 that the excitation peak of the material is located at 356nm, the emission peak is located at 620nm, and the luminescence intensity at the highest peak position of the emission peak is around 405 count intensities.
Example 5
Cu ion doped gallate base orange red luminescent material Ba0.95Cu0.05Ga2O4The preparation method comprises the following steps:
mixing BaCO3、Ga2O3CuO as a raw material, according to BaCO3:Ga2O3Mixing CuO 95:100:5 in a molar ratio, putting the mixture into an agate mortar, fully grinding the mixture to uniformly crush and mix the mixture to obtain a mixture, putting the mixture into a muffle furnace for sintering, heating the mixture to 1500 ℃ from room temperature, and preserving heat at 1500 DEG C5h, cooling to room temperature after heat preservation is finished to obtain Ba0.95Cu0.05Ga2O4The whole sintering process of the orange-red long afterglow fluorescent material finished product is carried out in the air atmosphere.
The Cu ion-doped gallate-based orange red luminescent material Ba prepared in the embodiment0.95Cu0.05Ga2O4The excitation and emission spectra of (A) are shown in FIGS. 3 and 4, and it can be seen from FIGS. 3 and 4 that the excitation peak of the material is at 352nm, the emission peak is at 620nm, and the emission intensity at the highest peak position of the emission peak is around 331 counts.
Example 6
Cu ion doped gallate base orange red luminescent material Ba0.92Cu0.08Ga2O4The preparation method comprises the following steps:
mixing BaCO3、Ga2O3CuO as a raw material, according to BaCO3:Ga2O3Mixing CuO 92:100:8 in a molar ratio, putting the mixture into an agate mortar, fully grinding the mixture to uniformly crush and mix the mixture to obtain a mixture, putting the mixture into a muffle furnace for sintering, heating the mixture to 1350 ℃ from room temperature, preserving the heat for 6 hours at the temperature of 1350 ℃, cooling the mixture to the room temperature after the heat preservation is finished to obtain Ba0.92Cu0.08Ga2O4The whole sintering process of the orange-red long afterglow fluorescent material finished product is carried out in the air atmosphere.
The Cu ion doped gallate based orange red luminescent material Ba prepared in the embodiment0.92Cu0.08Ga2O4The excitation and emission spectra of (a) are shown in fig. 3 and 4, and it can be seen from fig. 3 and 4 that the excitation peak of the material is at 364nm, the emission peak is at 623nm, and the emission intensity at the highest peak position of the emission peak is around 146 count intensities.
Example 7
Cu ion doped gallate base orange red luminescent material Ba0.99Cu0.01Ga2O4The preparation method comprises the following steps:
mixing BaNO3、Ga2O3、Cu(OH)2As a raw material, according to BaNO3:Ga2O3:Cu(OH)2Mixing the materials according to a molar ratio of 99:100:1, putting the mixture into an agate mortar, fully grinding the mixture to uniformly crush and mix the mixture to obtain a mixture, putting the mixture into a muffle furnace for sintering, heating the mixture to 1350 ℃ from room temperature, preserving heat for 6 hours at 1350 ℃, cooling the mixture to room temperature after the heat preservation is finished to obtain Ba0.99Cu0.01Ga2O4The whole sintering process of the orange-red long afterglow fluorescent material finished product is carried out in the air atmosphere.
The Cu ion-doped gallate-based orange red luminescent material Ba prepared in the embodiment0.99Cu0.01Ga2O4An excitation peak at 353nm, an emission peak at 622nm, and a luminescence intensity at the highest peak position of the emission peak of about 170 count intensities, which was similar to Ba, a luminescent material synthesized in example 10.99Cu0.01Ga2O4Ba synthesized by different raw material compounds with similar luminous peak positions and different surfaces(1-x)CuxGa2O4Luminescent materials, have similar luminescent properties.
Ba prepared in other examples from the XRD pattern of FIG. 1 (due to the relatively small amount of doping)(1-x)CuxGa2O4The XRD pattern of the luminescent material is the same as that of example 2, and therefore, the detailed description is omitted), it can be seen that the Cu ion doped gallate based orange red luminescent material prepared by the present invention is well matched with the standard card, and has good crystallization property, indicating that the doping does not change the BaGa2O4The crystal structure of (1), Cu ions enter Ba after being doped2+Realizing substitutional doping by lattice; it can be seen from fig. 2a, 2b, 2c, and 2d that the Cu ion doped gallate based orange red luminescent material prepared by the present invention is composed of Ba, Ga, O and Cu elements. FIG. 2c shows Ba0.985Cu0.015Ga2O4The element distribution diagram of (a) can be seen that the doped ions are uniformly distributed in the luminescent material.
FIG. 3 shows a Cu ion-doped gallate-based orange-red luminescent material Ba prepared in each example(1-x)CuxGa2O4Excitation and emission spectra of the invention, it can be seen from fig. 3 and 4 that the luminescent material Ba according to the invention(1-x)CuxGa2O4Presenting orangesRed light is emitted, and the emission luminance increases and then decreases with increasing concentration, and is strongest when x is 0.015. FIG. 5 shows Ba prepared in example 30.98Cu0.02Ga2O4The long afterglow life decay curve of the luminescent material can be seen from the figure, and the long afterglow life reaches 56 minutes. FIG. 6 shows Ba of the present invention(1-x)CuxGa2O4The trend graph of the afterglow life of the luminescent material shows that the long afterglow life increases and then decreases with the increase of the Cu ion concentration, and when x is 0.02, the afterglow life is optimal and can reach 56 minutes.
It should be understood that the examples and embodiments described herein are for illustrative purposes only and are not intended to limit the scope of the present disclosure, and that various modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the spirit and purview of this disclosure.

Claims (7)

1. A Cu ion doped gallate based orange red luminescent material is characterized in that: is prepared by mixing and sintering a barium-containing compound, a gallium-containing compound and a copper-containing compound;
the Cu ion doped gallate based orange red luminescent material is prepared by using BaGa2O4As a substrate, Cu ions are used as activating ions.
2. The Cu ion-doped gallate-based orange-red luminescent material of claim 1, wherein: the chemical structural formula is Ba x（1-）Cu x Ga2O4Wherein, in the step (A),x0.01 to 0.08.
3. The Cu ion-doped gallate-based orange-red luminescent material of claim 1 or 2, wherein: the barium-containing compound is at least one of barium oxide, barium carbonate, barium oxalate, barium acetate, barium nitrate and barium hydroxide.
4. The Cu ion-doped gallate-based orange-red luminescent material of claim 1 or 2, wherein: the gallium-containing compound is at least one of gallium oxide, carbonate, oxalate, acetate, nitrate and hydroxide.
5. The Cu ion-doped gallate-based orange-red light emitting material of claim 1 or 2, wherein: the copper-containing compound is at least one of copper oxide, carbonate, oxalate, acetate, nitrate and hydroxide.
6. The method according to any one of claims 1 to 5, wherein the Cu ion-doped gallate-based orange-red luminescent material comprises: the method comprises the following steps: and mixing a barium-containing compound, a gallium-containing compound and a copper-containing compound, sintering in air or an oxygen-containing atmosphere, and cooling along with a furnace to obtain the Cu ion-doped gallate-based orange-red luminescent material.
7. The method of claim 6, wherein the Cu ion-doped gallate-based orange-red luminescent material comprises: the sintering process specifically comprises the following steps: keeping the temperature for 5-8 h at 1200-1500 ℃.
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