CN107033889B - Red light-near infrared long afterglow luminescent material and preparation method thereof - Google Patents
Red light-near infrared long afterglow luminescent material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000004020 luminiscence type Methods 0.000 claims abstract description 19
- 150000001875 compounds Chemical class 0.000 claims description 36
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 239000011575 calcium Substances 0.000 claims description 10
- 238000010304 firing Methods 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052797 bismuth Inorganic materials 0.000 claims description 9
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 9
- 229910052791 calcium Inorganic materials 0.000 claims description 9
- 229910052732 germanium Inorganic materials 0.000 claims description 9
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 9
- 239000011701 zinc Substances 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000011787 zinc oxide Substances 0.000 claims description 7
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 6
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 6
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 6
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 claims description 6
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011667 zinc carbonate Substances 0.000 claims description 3
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 3
- 235000004416 zinc carbonate Nutrition 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000005284 excitation Effects 0.000 description 10
- 238000000695 excitation spectrum Methods 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 7
- 238000012544 monitoring process Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
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- 238000011160 research Methods 0.000 description 4
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- 229910017623 MgSi2 Inorganic materials 0.000 description 1
- 229910017625 MgSiO Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910003668 SrAl Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- -1 ZnS: cu (green) Chemical class 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001650 dmitryivanovite Inorganic materials 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 229910001707 krotite Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
- C09K11/745—Germanates
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Abstract
本发明提供的红光‑近红外长余辉发光材料，以CaZnGe2O6为基质，Bi2+作为激活离子，其中，Bi2+的质量含量为0.3％≤x≤5％，最终获得的发光波长位于600nm～800nm，发光峰位于660～675nm处，余辉时间大于3600秒。这种红光‑近红外长余辉发光材料的发光中心和发光峰均不同于现有技术，为近红外长余辉发光材料在医学领域的应用提供了更多的选择。同时，本发明原材料取材广泛，价格低廉，制备方法简单，易于大规模推广。
The red-near-infrared long afterglow luminescent material provided by the present invention uses CaZnGe 2 O 6 as a matrix and Bi 2+ as an active ion, wherein the mass content of Bi 2+ is 0.3%≤x≤5%, and the final obtained luminescence The wavelength is located at 600nm-800nm, the luminescence peak is located at 660-675nm, and the afterglow time is greater than 3600 seconds. The luminescence center and luminescence peak of this red-near-infrared long-afterglow luminescent material are different from those of the prior art, which provides more choices for the application of the near-infrared long-afterglow luminescent material in the medical field. At the same time, the raw materials of the invention are widely used, the price is low, the preparation method is simple, and it is easy to be popularized on a large scale.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a red light-near infrared long afterglow luminescent material and a preparation method thereof.
Background
A long persistent material is a material that can be excited after a certain period of time (e.g., X-ray excitation, ultraviolet excitation, visible light excitation, electron beam excitation, etc.) and still observe luminescence after stopping excitation. Such luminescence may vary in duration from material to material, as little as a few seconds to weeks.
The research objects of the early long afterglow materials mainly focus on sulfides such as ZnS: cu (green), CaS: bi (blue light), CaS: eu, Tm (red light), but the sulfide stability is poor. Later developed rare earth doped aluminate long persistence phosphors (SrAl)2O4:Eu2+，Dy3+，CaAl2O4：Eu2+，Nd3+) And silicate materials (MgSiO)3：Eu2+，Dy3+，Mn2+，Ca3MgSi2O8：Eu2+，Dy3+Etc.) long afterglow time, high brightness, good water and alkali resistance, but the luminescent wave band of the long afterglow material is in the visible light region, and the research on the near infrared long afterglow luminescent material is still less.
With the increasing application of the long-afterglow materials in the biomedical field, researchers find that the near-infrared long-afterglow luminescent materials can be used for detecting living molecular targets, and the difficulty caused by in vivo background interference is reduced because the blood and tissues of living organisms are relatively transparent in the wavelength range. Compared with other imaging marker materials, the long afterglow material serving as the bioluminescent marker material has the unique advantage of being used for observing the diffusion of the marker material, which is not possessed by any other marker material. Obviously, the near-infrared long-afterglow luminescent material which has stable structure, good chemical stability, low price, simple preparation method and easy large-scale popularization has good application prospect. However, because human tissues have wavelength selectivity, the existing near-infrared long-afterglow luminescent materials have luminescent centers and luminescent bands which cannot meet the requirements of the medical field, and therefore, the development of long-afterglow luminescent materials with different luminescent bands is very meaningful.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a red-near infrared long afterglow luminescent material, wherein the luminescent wavelength is 600 nm-800 nm, the luminescent peak is 660-675 nm, and the afterglow time is longer than 3600 seconds.
The invention provides a red light-near infrared long afterglow luminescent material, which is shown as a formula (I):
CaZnGe2O6：xBi2+(Ⅰ)
wherein, Bi2+The mass content of x is more than or equal to 0.3 percent and less than or equal to 5 percent.
Preferably, Bi2+The mass content of x is more than or equal to 0.3 percent and less than or equal to 0.5 percent.
The invention also provides a preparation method of the red light-near infrared long afterglow luminescent material, which comprises the following steps:
mixing a calcium-containing compound, a zinc-containing compound, a germanium-containing compound and a bismuth-containing compound, and firing at 1000-1150 ℃ for 4-6 h to obtain the red light-near infrared long afterglow luminescent material.
Preferably, the calcium-containing compound is calcium carbonate and/or calcium oxide.
Preferably, the zinc-containing compound is zinc oxide and/or zinc carbonate.
Preferably, the germanium-containing compound is germanium oxide.
Preferably, the bismuth-containing compound is bismuth oxide.
Preferably, the molar mass ratio of the calcium-containing compound, the zinc-containing compound, the germanium-containing compound and the bismuth-containing compound is 2: 2: 1: 0.0075-0.125.
Preferably, after the mixing, the method further comprises: and grinding and uniformly mixing the mixture obtained by mixing.
Preferably, the firing temperature is 1000-1100 ℃; the firing time is 4-5 h.
The invention provides a red light-near infrared long afterglow luminescent material, which is shown as a formula (I):
CaZnGe2O6：xBi2+(Ⅰ)
wherein, Bi2+The mass content of x is more than or equal to 0.3 percent and less than or equal to 5 percent.
The red light-near infrared long afterglow luminescent material provided by the invention uses CaZnGe2O6As a matrix, Bi2+As an activating ion, wherein, Bi2+The mass content of x is more than or equal to 0.3 percent and less than or equal to 5 percent, the finally obtained luminescence wavelength is between 600nm and 800nm, the luminescence peak is between 660 nm and 675nm, and the afterglow time is more than 3600 seconds. The luminescence center and the luminescence peak of the red light-near infrared long afterglow luminescent material are different from those of the prior art, and more choices are provided for the application of the near infrared long afterglow luminescent material in the medical field. Meanwhile, the raw materials of the invention are wide, the price is low, the preparation method is simple, and the invention is easy to be popularized in large scale.
Drawings
FIG. 1 is an XRD pattern of a red-near infrared long afterglow luminescent material prepared in example 1 of the present invention;
FIG. 2 is an excitation spectrum of a red-near infrared long afterglow luminescent material prepared in example 1 of the present invention at a monitoring wavelength of 675 nm;
FIG. 3 shows the emission spectrum of the red-near infrared long afterglow luminescent material prepared in example 1 of the present invention at an excitation wavelength of 340 nm;
FIG. 4 is a graph showing the decay of afterglow of a red-near infrared long afterglow luminescent material prepared in example 1 after being irradiated under ultraviolet light for 10 min;
FIG. 5 is an afterglow spectrum of the red light-near infrared long afterglow luminescent material prepared in example 2 of the present invention;
FIG. 6 shows the excitation spectrum of the red-near infrared long afterglow luminescent material prepared in example 2 of the present invention at a monitoring wavelength of 661 nm;
FIG. 7 is a graph showing the decay of afterglow of a red-near infrared long afterglow luminescent material prepared in example 2 of the present invention after being irradiated under UV light for 10 min;
FIG. 8 is an afterglow spectrum of a red light-near infrared long afterglow luminescent material prepared in example 3 of the present invention;
FIG. 9 is a graph showing the decay of afterglow of a red-near infrared long afterglow luminescent material prepared in example 3 of the present invention after being irradiated under ultraviolet light for 10 min.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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 invention provides a red light-near infrared long afterglow luminescent material, which is shown as a formula (I):
CaZnGe2O6：xBi2+(Ⅰ)
wherein, Bi2+The mass content of x is more than or equal to 0.3 percent and less than or equal to 5 percent.
Preferably, Bi2+The mass content of x is more than or equal to 0.3 percent and less than or equal to 0.5 percent. In some of the present inventionIn the examples, the Bi2+Is 0.3%, 0.5% or 5% by mass.
The centers of different fluorescence bands and materials with near-infrared luminescence are visible everywhere, however, the near-infrared long afterglow material can not be obtained by doping each ion, and the near-infrared long afterglow material can not be prepared by doping the material with the near-infrared fluorescence center. Obviously, the obtaining of each near-infrared long afterglow luminescent material is very difficult. The red light-near infrared long afterglow luminescent material provided by the invention uses CaZnGe2O6As a matrix, doped with Bi2+In order to activate ions, the finally obtained luminescence wavelength is 600 nm-800 nm, the luminescence peak is 660-675 nm, and the afterglow time is more than 3600 seconds. In some embodiments of the present invention, the luminescence wavelength is 600nm to 720nm, the luminescence peak is 661nm, and the afterglow time is more than 3600 seconds. In some embodiments of the present invention, the luminescence wavelength is 600nm to 730nm, the luminescence peak is 674nm, and the afterglow time is more than 3600 seconds.
The red light-near infrared long afterglow luminescent material provided by the invention has a luminescent center and a luminescent peak which are different from those of the prior art, and provides more choices for the application of the near infrared long afterglow luminescent material in the medical field.
The invention also provides a preparation method of the red light-near infrared long afterglow luminescent material, which comprises the following steps:
mixing a calcium-containing compound, a zinc-containing compound, a germanium-containing compound and a bismuth-containing compound, and firing at 1000-1100 ℃ for 4-5 h to obtain the red light-near infrared long afterglow luminescent material.
In the present invention, the calcium-containing compound is preferably calcium carbonate and/or calcium oxide; more preferably calcium carbonate. The zinc-containing compound is preferably zinc oxide and/or zinc carbonate; more preferably zinc oxide. The germanium-containing compound is preferably germanium oxide. The bismuth-containing compound is preferably bismuth oxide. In the present invention, the source of the raw material used is not particularly limited, and may be generally commercially available.
The molar mass ratio of the calcium-containing compound, the zinc-containing compound, the germanium-containing compound, and the bismuth-containing compound is preferably 2: 2: 1: 0.0075-0.125; more preferably 2: 2: 1: 0.0075-0.0125.
After the calcium-containing compound, the zinc-containing compound, the germanium-containing compound, and the bismuth-containing compound are mixed, it is preferable to further include: and grinding and uniformly mixing the mixture obtained by mixing. The polishing method is not particularly limited, and may be any polishing method known to those skilled in the art. The blending method is not particularly limited, and the blending method known to those skilled in the art can be used.
In the invention, the firing temperature is 1000-1150 ℃; preferably 1000-1100 ℃; in certain embodiments of the invention, the firing temperature is 1000 ℃ or 1100 ℃. The firing time is 4-6 h, preferably 4-5 h; in certain embodiments of the invention, the firing time is 4 hours or 5 hours.
The preparation method of the red light-near infrared long afterglow luminescent material disclosed by the invention is simple and feasible, and is easy for large-scale popularization. The red light-near infrared long afterglow luminescent material prepared by the preparation method has the luminescent wavelength of 600 nm-800 nm, the luminescent peak of 660-675 nm and the afterglow time of more than 3600 seconds. The luminescence center and the luminescence peak of the red light-near infrared long afterglow luminescent material are different from those of the prior art, and more choices are provided for the application of the near infrared long afterglow luminescent material in the medical field.
In order to further illustrate the present invention, the following examples are provided to describe a red-near infrared long afterglow luminescent material and its preparation method in detail, but should not be construed as limiting the scope of the present invention.
Example 1
According to the molar mass ratio of 2: 2: 1: 0.0125 g of calcium carbonate, 0.581g of zinc oxide, 1.214g of germanium oxide and 0.007g of bismuth oxide are respectively weighed, ground, uniformly mixed and fired at 1100 ℃ for 4h to obtain the red light-near infrared long afterglow luminescent material. In the red light-near infrared long afterglow luminescent material, Bi2+The mass content of (A) is 0.5%.
Using X-ray diffractometer to obtain red light-near red lightThe results of the analysis of the external long afterglow luminescent material are shown in FIG. 1. FIG. 1 is an XRD diagram of a red-near infrared long afterglow luminescent material prepared in example 1 of the present invention. As can be seen from FIG. 1, the doping does not cause the generation of new phase, so that it can be proved that the red light-near infrared long afterglow luminescent material obtained in this embodiment is CaZnGe2O6Pure phase.
The excitation spectrum of the red light-near infrared long afterglow luminescent material obtained by research under the condition that the monitoring wavelength is 675nm is shown in figure 2. FIG. 2 shows the excitation spectrum of the red-near infrared long afterglow luminescent material prepared in example 1 of the present invention at a monitoring wavelength of 675 nm. As can be seen from FIG. 2, there are two excitation peaks in the excitation spectrum at the wavelength of 303nm and at the wavelength of 530nm, respectively, confirming that the luminescence center is Bi2+Ions.
The emission spectrum of the red light-near infrared long afterglow luminescent material obtained by research under the excitation wavelength of 340nm is shown in figure 3. FIG. 3 shows the emission spectrum of the red-near infrared long afterglow luminescent material prepared in example 1 of the present invention at an excitation wavelength of 340 nm. As can be seen from FIG. 3, at a wavelength of 600nm to 800nm, there is a relatively significant emitted light, and the light emission peak is located at 675 nm.
The obtained red light-near infrared long afterglow luminescent material is irradiated for 10min under ultraviolet light, and then the afterglow attenuation condition is detected, as shown in figure 4. FIG. 4 is a graph of the decay of afterglow of the red light-near infrared long afterglow luminescent material prepared in example 1 of the present invention after being irradiated under ultraviolet light for 10 min. As can be seen from FIG. 4, the red-near infrared long afterglow luminescent material prepared by the present embodiment has a long afterglow of up to 3600 s; as a result of the detection, the long afterglow was found to be red.
Example 2
According to the molar mass ratio of 2: 2: 1: 0.125 g of calcium carbonate, 0.473g of zinc oxide, 1.214g of germanium oxide and 0.068g of bismuth oxide are respectively weighed, ground, uniformly mixed and fired at 1000 ℃ for 5 hours to obtain the red light-near infrared long afterglow luminescent material. In the red light-near infrared long afterglow luminescent material, Bi2+The mass content of (A) is 5%.
The afterglow spectrum of the red light-near infrared long afterglow luminescent material prepared in this example is measured, as shown in fig. 5. FIG. 5 is the afterglow spectrum of the red light-near infrared long afterglow luminescent material prepared in example 2 of the present invention. As can be seen from FIG. 5, the red light-near infrared long afterglow luminescent material prepared by the present embodiment has long afterglow fluorescence at a wavelength of 600nm to 720nm, which indicates that the material has long afterglow characteristics. The peak of luminescence is located at 661 nm.
The excitation spectrum of the obtained red-near infrared long afterglow luminescent material was investigated at a monitoring wavelength of 661nm, as shown in fig. 6. FIG. 6 shows the excitation spectrum of the red-near infrared long afterglow luminescent material prepared in example 2 of the present invention at a monitoring wavelength of 661 nm. As can be seen from FIG. 6, there are two excitation peaks in the excitation spectrum, one at a wavelength of 258nm, corresponding to Bi2+(ii) a transition of an ion; the other is located at the wavelength of 295nm, corresponding to Bi2+Ion transition, thereby confirming that the luminescence center is Bi2+Ions.
The obtained red light-near infrared long afterglow luminescent material is irradiated for 10min under ultraviolet light, and then the afterglow attenuation condition is detected, as shown in fig. 7. FIG. 7 is a graph showing the decay of afterglow of the red-near infrared long afterglow luminescent material prepared in example 2 of the present invention after being irradiated under ultraviolet light for 10 min. As can be seen from FIG. 7, the red-near infrared long afterglow luminescent material prepared by the present embodiment has a long afterglow of up to 3600 s; as a result of the detection, the long afterglow was found to be red.
Example 3
According to the molar mass ratio of 2: 2: 1: 0.0075, 0.581g of calcium carbonate, 0.473g of zinc oxide, 1.214g of germanium oxide and 0.004g of bismuth oxide are respectively weighed, ground, uniformly mixed and fired at 1100 ℃ for 5 hours to obtain the red light-near infrared long afterglow luminescent material. In the red light-near infrared long afterglow luminescent material, Bi2+The mass content of (A) is 0.3%.
The afterglow spectrum of the red light-near infrared long afterglow luminescent material prepared in this example is measured, as shown in fig. 8. FIG. 8 is the afterglow spectrum of the red light-near infrared long afterglow luminescent material prepared in example 3 of the present invention. As can be seen from FIG. 8, the red light-near infrared long afterglow luminescent material prepared by the present embodiment has long afterglow fluorescence at a wavelength of 600nm to 730nm, which indicates that the material has long afterglow characteristics. The luminescence peak is at 674 nm.
The obtained red light-near infrared long afterglow luminescent material is irradiated for 10min under ultraviolet light, and then the afterglow attenuation condition is detected, as shown in fig. 9. FIG. 9 is a graph showing the decay of afterglow of a red-near infrared long afterglow luminescent material prepared in example 3 of the present invention after being irradiated under ultraviolet light for 10 min. As can be seen from FIG. 9, the red-near infrared long afterglow luminescent material prepared by the present embodiment has a long afterglow of up to 3600 s; as a result of the detection, the long afterglow was found to be red.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
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| Luminescence properties of a new Mn2+-activated red long-afterglow phosphor;Guangbo Che et al.;《Journal of Physics and Chemistry of Solids》;20080312;第69卷;第2091-2095页 * |
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