CN115820245A - Near-infrared long-afterglow material and preparation method and application thereof - Google Patents
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Abstract
The invention relates to a near-infrared long afterglow material, a preparation method and application thereof, belonging to the technical field of inorganic luminescent materials. The chemical expression is Zn 1‑2x Li x Ga 2+x O 4 :Cr 3+ ，0<x<0.5; mixing zinc oxide, gallium oxide, lithium carbonate, chromium oxide and boric acid, adding absolute ethyl alcohol, and grinding into mixed powder; pressing the part of mixed powder into a green sheet, and firing the green sheet and the mixed powder together in the air at 1350 ℃ to obtain the near-infrared long afterglow material. The invention adopts ZnO and Li 2 CO 3 、Ga 2 O 3 、Cr 2 O 3 The material is used as a raw material to prepare the near-infrared long afterglow material, and the raw material is wide in material availability and low in cost; the operation process is simple, only the compounds are required to be mixed, ground and calcined, the operation environment is mild, a special gas atmosphere is not required, the operation is simple, and the method is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to a near-infrared long afterglow material, a preparation method and application thereof, belonging to the technical field of inorganic luminescent materials.
Background
The long afterglow luminescent material is a material which can emit light under the irradiation of excitation light, stores energy through traps inside the material, and emits the stored energy in the form of light after the excitation is stopped. Because of the unique light-storing property, the long-afterglow luminescent material is widely applied to the technical fields of biological imaging, emergency lighting, anti-counterfeiting and the like.
The near-infrared luminescent material can emit near-infrared light, the wavelength of the near-infrared light is longer than that of red light, the near-infrared light is invisible light, and the near-infrared luminescent material has good tissue penetrability. The near-infrared long afterglow material can still emit near-infrared light after the excitation is stopped, so that the interference of background light caused by in-situ excitation can be effectively avoided, and the near-infrared long afterglow material is widely applied to biological tissue imaging. Similarly, the hidden illumination under the dark field can be realized by utilizing the near-infrared afterglow illumination of the near-infrared long afterglow material.
The current near-infrared long afterglow material has wide research and is representative ZnGa 2 O 4 :Cr 3+ And LiGa 5 O 8 :Cr 3+ Has particularly excellent long afterglow performance. These two materials will be referred to as reference materials in the following description.
Disclosure of Invention
The invention aims to overcome the technical problems and provides a near-infrared long afterglow material, a preparation method and application thereof, the operation process is simple, the material is suitable for large-scale industrial production, visible light and near infrared light can be emitted under the excitation of X rays, ultraviolet light and partial visible light in an air environment, and visible red light and near infrared light can be emitted after the excitation of the X rays and the ultraviolet light is stopped.
The invention relates to a near-infrared long afterglow material, the chemical expression of which is Zn 1-2x Li x Ga 2+x O 4 :Cr 3 + ，0<x<0.5。
Further, mixing zinc oxide, gallium oxide, lithium carbonate, chromium oxide and boric acid, adding absolute ethyl alcohol, and grinding into mixed powder; firing the mixture in air at 1300-1400 ℃ to obtain the near-infrared long afterglow material.
Further, the molar ratio of the zinc oxide, the lithium carbonate, the gallium oxide and the chromium sesquioxide is as follows: 1-2x:0.5x: (1 + 0.5x): 0.005x, 0-straw-woven (x) layer in that respect.
Further, the mass of the boric acid is 3% -5% of the total mass of the zinc oxide, the gallium oxide, the lithium carbonate and the chromium oxide.
Further, zinc oxide, gallium oxide, lithium carbonate, chromium oxide and boric acid are uniformly mixed in absolute ethyl alcohol, and are continuously ground until the absolute ethyl alcohol is volatilized, so that uniformly distributed raw materials are obtained.
Further, the uniformly mixed raw material powder is pressed for 1-2 min under the pressure of 120-160 MPa by a pressing die to obtain the raw material sheet.
Further, placing the green sheet and the mixed powder in a crucible, firing at 1300-1400 ℃ for 3-5h, wherein the heating rate is 4-6 ℃/min, the heating atmosphere is air, and naturally cooling to obtain the near-infrared long afterglow material.
The invention also relates to the application of the near-infrared long afterglow material in near-infrared illumination.
The near-infrared long afterglow material can emit visible light and near infrared light under the excitation of X rays, ultraviolet light and partial visible light in the air environment, and can also emit visible red light and near infrared light after the excitation of the X rays and the ultraviolet light is stopped, wherein the near-infrared attenuation life of the near-infrared long afterglow material reaches 30min, and the naked-eye distinguishing time of the red light is more than 1 min.
The wavelength of the ultraviolet light is 250-400 nm.
The invention has the beneficial effects that:
(1) The near-infrared long afterglow material can emit visible light and near infrared light under the excitation of X rays, ultraviolet light and partial visible light in the air environment, and can also emit visible red light and near infrared light after the excitation of the X rays and the ultraviolet light is stopped, wherein the near-infrared attenuation life of the near-infrared long afterglow material can reach 30min, and the naked-eye distinguishing time of the red light is more than 1 min.
(2) The invention adopts ZnO and Li 2 CO 3 、Ga 2 O 3 、Cr 2 O 3 The material is used as a raw material to prepare the near-infrared long afterglow material, and the raw material is wide in material availability and low in cost; the operation process is simple, only the compounds are mixed, ground and calcined, the operation environment is mild, no special gas atmosphere is needed, and the operation is carried outSimple and suitable for large-scale industrial production.
Drawings
In order that the manner in which the above recited features of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to embodiments, some of which are illustrated in the appended drawings
FIG. 1 is an X-ray diffraction pattern of a reference material and materials prepared in examples 1-5 of the present invention.
FIG. 2 is a photograph of reference materials and materials prepared in examples 1-5 of the present invention under different excitation sources.
FIG. 3 is an excitation and emission spectrum of a reference material and materials prepared in examples 1-5 of the present invention.
FIG. 4 is a thermoluminescent spectrum of a reference material and materials prepared in examples 1-5 of the present invention.
FIG. 5 is a schematic diagram showing the energy of thermoluminescence of the material prepared by the present invention over the entire temperature range.
FIG. 6 is a long afterglow decay spectrum of the near infrared long afterglow material prepared in example 3 of the present invention after being excited by monochromatic light of different wavelengths for 2 minutes.
Fig. 7 is a photoluminescence photograph, a long afterglow photograph and a thermoluminescence photograph of the near-infrared long afterglow material prepared in example 3 of the present invention using X-rays as an excitation source.
Fig. 8 is an afterglow imaging graph of the reference material and the near-infrared long afterglow material prepared in embodiments 1-5 of the present invention in a small animal imaging system after being irradiated by 365nm ultraviolet lamps.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The material prepared by the invention is Zn 1-2x LixGa 2+x O 4 :Cr 3+ (0<x<0.5 Wherein the Cr3+ concentration is represented by only 1% in the examples.
Example 1
(1) Adding ZnO and Li 2 CO 3 、Ga 2 O 3 、Cr 2 O 3 According to a molar ratio of 1.6:0.1:2.1:0.002, adding H accounting for 3 to 6t percent of the total mass of the mixture 3 BO 3 And then uniformly grinding in absolute ethyl alcohol until the absolute ethyl alcohol is volatilized, so as to obtain uniformly distributed raw materials.
(2) And (2) pressing the raw material powder uniformly mixed in a proper amount in the step (1) for 1-2 min under the pressure of 120-160 Mpa by using a pressing die to obtain the raw material sheet.
(3) And (2) placing the green sheets and the green powder in a corundum crucible, firing for 4 hours at 1350 ℃ by high-temperature heating equipment such as a high-temperature tube furnace and the like, wherein the heating rate is 5 ℃/min, the heating atmosphere is air, and after natural cooling, proper grinding is carried out to obtain the near-infrared long afterglow material with x = 0.1.
Example 2
(1) Adding ZnO and Li 2 CO 3 、Ga 2 O 3 、Cr 2 O 3 According to a molar ratio of 1.2:0.2:2.2:0.004, adding H accounting for 3 to 6t percent of the total mass of the mixture 3 BO 3 And grinding the mixture evenly in absolute ethyl alcohol until the absolute ethyl alcohol is volatilized, thus obtaining evenly distributed raw materials.
(2) And pressing a proper amount of uniformly mixed raw material powder for 1-2 min under the pressure of 120-160 Mpa by using a pressing die to obtain the raw material tablet.
(3) And (2) placing the green sheets and the green powder in a corundum crucible, firing for 4 hours at 1350 ℃ by high-temperature heating equipment such as a high-temperature tube furnace and the like, wherein the heating rate is 5 ℃/min, the heating atmosphere is air, and after natural cooling, proper grinding is carried out to obtain the near-infrared long afterglow material with x = 0.2.
Example 3
(1) Adding ZnO and Li 2 CO 3 、Ga 2 O 3 、Cr 2 O 3 According to the mol ratio of 1:0.25:2.25:0.005, adding 3 to 6 weight percent of H3BO3, and grinding the mixture evenly in absolute ethyl alcohol until the absolute ethyl alcohol is volatilized to obtain evenly distributed raw materials.
(2) And pressing a proper amount of uniformly mixed raw material powder for 1-2 min under the pressure of 120-160 Mpa by using a pressing die to obtain the raw material tablet.
(3) And (2) placing the green sheets and the green powder in a corundum crucible, firing for 4 hours at 1350 ℃ by high-temperature heating equipment such as a high-temperature tube furnace and the like, wherein the heating rate is 5 ℃/min, the heating atmosphere is air, and after natural cooling, proper grinding is carried out to obtain the near-infrared long afterglow material with x = 0.25.
Example 4
(1) Adding ZnO and Li 2 CO 3 、Ga 2 O 3 、Cr 2 O 3 The molar ratio of the raw materials is 0.8:0.3:2.3:0.006, adding 3-6 wt% of H3BO3, and grinding in absolute ethyl alcohol until the absolute ethyl alcohol is volatilized to obtain uniformly distributed raw material.
(2) And pressing a proper amount of uniformly mixed raw material powder for 1-2 min under the pressure of 120-160 MPa by using a pressing die to obtain the raw material tablet.
(3) And (2) placing the green sheets and the green powder in a corundum crucible, firing for 4 hours at 1350 ℃ by high-temperature heating equipment such as a high-temperature tube furnace and the like, wherein the heating rate is 5 ℃/min, the heating atmosphere is air, and after natural cooling, proper grinding is carried out to obtain the near-infrared long afterglow material with x = 0.3.
Example 5
(1) Adding ZnO and Li 2 CO 3 、Ga 2 O 3 、Cr 2 O 3 According to a molar ratio of 0.4:0.4:2.4:0.008, adding 3-6 wt% of H3BO3, and grinding in absolute ethyl alcohol uniformly until the absolute ethyl alcohol is volatilized to obtain uniformly distributed raw materials.
(2) And pressing the raw material powder which is uniformly mixed in a proper amount for 1-2 min under the pressure of 120-160 MPa by a tabletting mould to obtain the raw material tablet.
(3) And (2) placing the green sheets and the green powder in a corundum crucible, firing for 4 hours at 1350 ℃ by high-temperature heating equipment such as a high-temperature tube furnace and the like, wherein the heating rate is 5 ℃/min, the heating atmosphere is air, and after natural cooling, proper grinding is carried out to obtain the x =0.4 near-infrared long afterglow material.
And (3) analyzing an experimental result:
ZnGa is synthesized by adopting the same conditions 2 O 4 :Cr 3+ And LiGa 5 O 8 :Cr 3+ Two reported near-infrared long afterglow materials are used as reference.
As shown in FIG. 1, the results of analyzing the near-infrared long afterglow phosphors and the reference materials obtained in examples 1 to 5 by an X-ray diffractometer show that Zn1 is the reference material -2x Li x Ga 2+x O 4 :Cr 3+ The diffraction patterns (x takes 0 and 0.5) were consistent with the corresponding standard diffraction patterns (PDF No.76-0199 and PDF No. 86-0411), indicating that at this temperature, cr was present 3+ The introduction of (2) does not cause the generation of a new phase, and a corresponding substance is successfully synthesized; while the material synthesized in the above examples is Zn 1-2x Li x Ga 2+ x O 4 :Cr 3+ (x is 0.1, 0.2, 0.25, 0.3 and 0.4 respectively) shows the transition of the two standard diffraction patterns, and indicates Zn 1-2x Li x Ga 2+x O 4 :Cr 3+ (0<x<0.5 With x does not lead to the presence of impurity phases in solid solution, and small amounts of Cr 3 + The dopant did not alter the crystalline phase of the host, and the evolution of the co-substitution process was clearly observed from the enlarged region of the main XRD peak from 35 ° to 38 °; in general, zn was confirmed 1-2x Li x Ga 2+x O 4 :Cr 3+ (0<x<0.5 ) successful synthesis of solid solutions.
The reference material and the sheet-shaped near-infrared long afterglow material prepared in the above example were excited by different excitation sources, and a vivo iqoo Z3 mobile phone was used to photograph, and fig. 2 was obtained, from which it can be seen that under excitation of most ultraviolet light, the whole material emits red light.
Reference materialThe spectrum test is carried out on the near-infrared long afterglow material prepared in the above embodiment to obtain an excitation spectrum and a photoluminescence spectrum, and the result is shown in figure 3, from which Zn can be known 1-2x Li x Ga 2+x O 4 :Cr 3+ The solid solution has three characteristic excitation bands and can emit near infrared rays; the change of x has little influence on the peak shape, and Zn can be obtained 1-2x Li x Ga 2+x O 4 :Cr 3+ (0<x<0.5 Has a wide emission band of 660nm to 780nm under effective excitation, successfully realizes that the Cr has 3+ Near infrared emission of (2).
The reference material and the sheet near-infrared long afterglow material prepared in the above embodiment are pre-excited by ultraviolet light, then the intensity of thermoluminescence is measured at 200-600k, and the thermoluminescence spectrum is obtained, and the result is shown in fig. 4, and the corresponding spectrum area integral can be used to approximately represent the energy of thermoluminescence of the material in the whole temperature range, that is, the weight of the energy stored corresponding to the internal defect of the material, and the result is shown in fig. 5. It can be seen that the x =0.2, x =0.25, x =0.3 and x =0.4 samples stored energy more defectively than the two-terminal reference material, confirming that the solid solution strategy achieved a breakthrough in performance.
After the x =0.25 near-infrared long afterglow material in the embodiment 3 is charged with monochromatic light with different wavelengths for two minutes, the change of the afterglow emission intensity at 709nm is detected, and the afterglow attenuation curves of different excitation sources, shown in fig. 6, are obtained; it can be seen that the pre-excitation of 250-420 nm can realize the near-infrared long afterglow, and after the pre-excitation of the optimal excitation wavelength of 330nm, the emission intensity of 709nm is still obviously higher than the background intensity within 3 minutes, thus proving the excellent long afterglow performance.
The near-infrared long afterglow material with x =0.25 in the embodiment 3 has a radiation induced luminescence phenomenon under the irradiation of x-rays, and can have long afterglow after the excitation is stopped; the pyro-luminescence phenomenon appears when the long afterglow stops and is stimulated by heat, and the result is shown in figure 7; the photographs in the figure show the luminescence of the material in the above 3 states, visible to the naked eye as red emission.
The reference material and the near-infrared long afterglow material prepared in the above embodiment are monitored by a small animal imager for the near-infrared long afterglow intensity, a 365nm handheld ultraviolet lamp is used as an excitation source, after irradiation for 1 minute, the sample is immediately placed into an IVIS system, and continuous luminescence imaging is performed at room temperature to obtain a graph 8, which clearly shows that the near-infrared long afterglow can reach more than 30 min.
Claims (10)
1. A near-infrared long afterglow material is characterized in that: the chemical expression is Zn 1-2x Li x Ga 2+x O 4 :Cr 3+ ，0<x<0.5。
2. The preparation method of the near-infrared long afterglow material as claimed in claim 1, which is characterized in that: mixing zinc oxide, gallium oxide, lithium carbonate, chromium oxide and boric acid, adding absolute ethyl alcohol, and grinding into mixed powder; firing the mixture in air at 1300-1400 ℃ to obtain the near-infrared long afterglow material.
3. The method for preparing the near-infrared long-afterglow material as claimed in claim 2, which is characterized in that: the molar ratio of the zinc oxide, the lithium carbonate, the gallium oxide and the chromium sesquioxide is as follows: 1-2x:0.5x: (1 + 0.5x): 0.005x, 0-straw-woven (x) layer in that respect.
4. The method for preparing the near-infrared long-afterglow material as claimed in claim 2, which is characterized in that: the mass of the boric acid is 3-5% of the total mass of the zinc oxide, the gallium oxide, the lithium carbonate and the chromium oxide.
5. The method for preparing the near-infrared long-afterglow material as claimed in claim 2, which is characterized in that: uniformly mixing zinc oxide, gallium oxide, lithium carbonate, chromium sesquioxide and boric acid in absolute ethyl alcohol, continuously grinding until the absolute ethyl alcohol is volatilized, and obtaining uniformly distributed raw materials.
6. The method for preparing the near-infrared long-afterglow material as claimed in claim 5, which is characterized in that: and pressing the uniformly mixed raw material powder for 1-2 min under the pressure of 120-160 MPa by using a pressing die to obtain a raw material sheet.
7. The method for preparing the near-infrared long-afterglow material as claimed in claim 6, which is characterized in that: and placing the green sheet and the mixed powder into a crucible, firing at 1300-1400 ℃ for 3-5h, wherein the heating rate is 4-6 ℃/min, the heating atmosphere is air, and naturally cooling to obtain the near-infrared long afterglow material.
8. The use of the near-infrared long afterglow material as defined in claim 1, wherein: it is applied to near infrared illumination.
9. The use of the near-infrared long afterglow material as set forth in claim 8, wherein: the near-infrared long afterglow material can emit visible light and near infrared light under the excitation of X rays, ultraviolet light and partial visible light in the air environment, and can also emit visible red light and near infrared light after the excitation of the X rays and the ultraviolet light is stopped, wherein the near-infrared attenuation life of the near-infrared long afterglow material reaches 30min, and the naked-eye distinguishing time of the red light is more than 1 min.
10. The use of the near-infrared long afterglow material as defined in claim 9, wherein: the wavelength of the ultraviolet light is 250-400 nm.
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