CN112680223A - Zinc-germanium oxide long-afterglow luminescent material and preparation method thereof - Google Patents
Zinc-germanium oxide long-afterglow luminescent material and preparation method thereof Download PDFInfo
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- CN112680223A CN112680223A CN202110072014.4A CN202110072014A CN112680223A CN 112680223 A CN112680223 A CN 112680223A CN 202110072014 A CN202110072014 A CN 202110072014A CN 112680223 A CN112680223 A CN 112680223A
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- 239000000463 material Substances 0.000 title claims abstract description 69
- HMRQSZREPBVTLZ-UHFFFAOYSA-N [Ge]=O.[Zn] Chemical compound [Ge]=O.[Zn] HMRQSZREPBVTLZ-UHFFFAOYSA-N 0.000 title claims description 23
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 229910005833 GeO4 Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract 2
- 239000011701 zinc Substances 0.000 claims description 12
- 229910005831 GeO3 Inorganic materials 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 238000000695 excitation spectrum Methods 0.000 claims description 7
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(III) nitrate Inorganic materials [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 4
- 238000000295 emission spectrum Methods 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 239000012190 activator Substances 0.000 abstract description 3
- 239000007795 chemical reaction product Substances 0.000 abstract description 3
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 abstract description 3
- 238000011503 in vivo imaging Methods 0.000 abstract description 2
- 238000004020 luminiscence type Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- 238000002626 targeted therapy Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 230000005284 excitation Effects 0.000 description 9
- 238000007605 air drying Methods 0.000 description 8
- 238000005485 electric heating Methods 0.000 description 8
- 238000002189 fluorescence spectrum Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 230000001678 irradiating effect Effects 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 230000002688 persistence Effects 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 240000006829 Ficus sundaica Species 0.000 description 1
- 239000005084 Strontium aluminate Substances 0.000 description 1
- 229910007486 ZnGa2O4 Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
A long-afterglow luminescent Zn-Ge oxide material2GeO4: XC, wherein C is Eu3+Or Dy3+X is more than or equal to 0.001 and less than or equal to 0.1. The preparation method of the oxide comprises the following steps: preparing a solution with a certain concentration from a proper amount of raw materials, mixing the solution in a beaker according to a certain proportion, uniformly stirring the solution by magnetic force after adjusting the pH value to a required value, putting the solution into a high-temperature reaction kettle with a polytetrafluoroethylene lining, heating the reaction kettle to 220 ℃, preserving heat for 4 hours, cooling the reaction kettle to room temperature after the reaction is finished, taking out a reaction product, and centrifuging, washing and drying the reaction product to obtain a product. The material obtained by the invention can emit green afterglow after being irradiated by ultraviolet light, the afterglow time can reach 500s, the long afterglow material takes Zn, Ge and O elements as matrixes and Dy3+Or Eu2+Is a luminescent center of afterglow and has better thermal stability and chemical stability. The invention is innovative in that rare earth material is introduced as an activator, and the long-afterglow luminescent material is synthesized by a hydrothermal synthesis method, has small and relatively uniform particle size, and simultaneouslyHas excellent sustainable luminescence property, and provides possibility for deep research of medical fields such as in vivo imaging, biological target therapy and the like.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and relates to a zinc-germanium oxide long-afterglow luminescent material and a preparation method thereof.
Background
A long persistence material is a photoluminescent material that absorbs energy when irradiated by excitation light and continues to emit light after the excitation light ceases. In recent years, long afterglow materials have a special function of eliminating tissue autofluorescence due to their property of maintaining luminescence after stopping excitation, and have become important materials in biomedicine. The long afterglow material is mostly doped with rare earth materials as an activator, such as the current commercial long afterglow material SrAl2O4：Eu2+，Dy3+And is synthesized by a high-temperature solid phase method, and has the characteristics of stable chemical property, high afterglow brightness and long afterglow time. However, the product synthesized by the high-temperature solid phase method has large and uneven particle size and poor dispersibility, and is not suitable for forming a probe to be applied to biomedical research. The hydrothermal synthesis method is favored by researchers because of high purity of synthesized particles, good dispersibility, good and controllable crystal form, low production cost and simple operation. At present, the long afterglow materials prepared by the hydrothermal method are mostly ZnGa2O4、Zn2GeO4As a substrate, doped with Cr2+Or Mn2+Can be used as activator. However, the long-afterglow luminescent material synthesized by the existing hydrothermal method has low afterglow intensity and relatively short afterglow time, so that the long-afterglow luminescent material which has more excellent synthesis performance and smaller and uniform particle size has important scientific significance and practical application prospect.
Disclosure of Invention
The invention provides a zinc-germanium oxide long afterglow luminescent material which generates long afterglow under the excitation of 260-330nm, and the afterglow time reaches more than 500 s.
The invention also aims to provide the preparation method of the long afterglow luminescent material, which can obtain the long afterglow luminescent material with stable performance by hydrothermal reaction for 4 hours at the temperature of 220 ℃.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a zinc germanium oxide long afterglow luminescent material is characterized in that: the chemical composition formula is Zn2GeO4: XC, wherein C is Eu3+Or Dy3+，0.001≤X≤0.1。
The long afterglow luminescent material has excitation spectrum wavelength range of 260-330nm and emission spectrum of 472 nm.
The zinc-germanium oxide long-afterglow luminescent material provided by the invention can emit afterglow after being excited by excitation light of 254nm, the spectral wavelength of the afterglow is 472nm, the afterglow time can reach 500s, and the afterglow material has high thermal stability and chemical stability. The invention is innovative in that rare earth materials are introduced as activating agents, and the long-afterglow luminescent materials are synthesized by a hydrothermal synthesis method, have small and relatively uniform particle size and excellent sustainable luminescent performance, and provide possibility for deep research of medical fields such as in-vivo imaging, biological targeted therapy and the like.
Drawings
FIG. 1 is a SEM image of a long-afterglow luminescent material prepared in example 1 of the present invention;
FIG. 2 is a SEM image of the long-afterglow luminescent material obtained in example 2 of the present invention;
FIG. 3 is a SEM image of the long-afterglow luminescent material prepared in example 3 of the present invention;
FIG. 4 is a SEM image of long-afterglow luminescent material prepared in example 4 of the present invention;
FIG. 5 shows fluorescence emission spectra of long-lasting phosphors obtained in examples 1, 2, 3 and 4 of the present invention;
FIG. 6 shows fluorescence excitation spectra of long-afterglow luminescent materials obtained in examples 1, 2, 3 and 4 of the present invention;
FIG. 7 is a graph of afterglow of long-afterglow luminescent materials obtained in examples 1, 2, 3 and 4 of the present invention;
FIG. 8 is an XRD spectrum of the long persistence luminescent materials of examples 1, 2, 3 and 4 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited to these examples.
Example 1: this example has a chemical composition formula of Zn2GeO4：0.005Eu3+The preparation method of the long afterglow material comprises the following steps:
get GeO20.52364g of Na was dissolved in 10mL of 3mol/L NaOH solution to prepare Na2GeO3A solution; scale Zn (NO)3)2·3H2O 5.2996g，Eu(NO3)3·6H2O0.0043 g is respectively prepared into 100mL solution, 10mL is respectively taken out to be arranged in the same 100mL beaker, and concentrated nitric acid 3 mu is addedStirring for 5min after L adding Na2GeO3The solution was 2 mL. Adjusting the pH value to 6.5 by using concentrated ammonia water, continuously stirring for 1h, loading into a high-pressure reaction kettle with a 50mL polytetrafluoroethylene lining, placing into an electric heating forced air drying oven, heating to 220 ℃, preserving heat for 4h, naturally reducing to room temperature, taking out a reaction product, carrying out three to four times of high-speed centrifugal washing, placing into the electric heating forced air drying oven, preserving heat for 120 ℃, drying for 12h, and grinding to obtain the zinc-germanium oxide long-afterglow luminescent material.
The field emission scanning electron microscope picture of the zinc germanium oxide long afterglow luminescent material prepared in this example is shown in fig. 1, the fluorescence emission spectrum is shown in fig. 5, and the fluorescence excitation spectrum is shown in fig. 6. Excitation peak at 300nm and emission peak at 472nm, belonging to Eu3+4f of65d1→4f7And (4) transition. Irradiating with ultraviolet lamp for 10min, and observing in dark place after irradiation is stopped to give green afterglow. FIG. 7 is a graph showing the decay of afterglow of the material, and it can be seen that the material can continuously emit light for 500s or more. FIG. 8 is the XRD spectrum of the material, from which the diffraction peak can be seen to coincide with the standard card, which shows that the zinc germanium oxide long afterglow material is successfully prepared.
Example 2: this example has a chemical composition formula of Zn2GeO4：0.005Eu3+The preparation method of the long afterglow material comprises the following steps:
get GeO20.52364g of Na was dissolved in 10mL of 3mol/L NaOH solution to prepare Na2GeO3A solution; scale Zn (NO)3)2·3H2O 5.2996g，Eu(NO3)3·6H20.0043g of O is respectively prepared into 100mL of solution, 10mL of the solution is respectively put into the same 100mL beaker, 3 mu L of concentrated nitric acid is added, the mixture is stirred for 5min, and Na is added2GeO32mL of the solution. Adjusting the pH value to 6.5 by using concentrated ammonia water, continuously stirring for 1h, loading into a high-pressure reaction kettle with a 50mL polytetrafluoroethylene lining, placing into an electric heating forced air drying oven, heating to 220 ℃, preserving heat for 4h, naturally reducing to room temperature, taking out reactants, carrying out three to four times of high-speed centrifugal washing, placing into the electric heating forced air drying oven, preserving heat for 120 ℃, drying for 12h, and grinding to obtain the zinc-germanium oxide long-afterglow luminescent material.
The thermal field emission scanning electron microscope of the zinc-germanium oxide long-afterglow luminescent material prepared in this example is shown in fig. 2, the fluorescence emission spectrum is shown in fig. 5, and the fluorescence excitation spectrum is shown in fig. 6. Excitation peak at 300nm and emission peak at 472nm, belonging to Eu3+4f of65d1→4f7And (4) transition. Irradiating with ultraviolet lamp for 10min, and observing in dark place after irradiation is stopped to give green afterglow. FIG. 7 is a graph showing the decay of afterglow of the material, and it can be seen that the material can continuously emit light for 500s or more. FIG. 8 is the XRD spectrum of the material, from which diffraction peaks can be seen to be consistent with standard cards, which shows that the zinc germanium oxide long afterglow material is successfully prepared.
Example 3: this example has a chemical composition formula of Zn2GeO4：0.005Eu3+The preparation method of the long afterglow material comprises the following steps:
get GeO20.52364g of Na was dissolved in 10mL of 3mol/L NaOH solution to prepare Na2GeO3A solution; scale Zn (NO)3)2·3H2O 5.2996g，Eu(NO3)3·6H20.0043g of O is respectively prepared into 100mL of solution, 10mL of the solution is respectively put into the same 100mL beaker, 3 mu L of concentrated nitric acid is added, the mixture is stirred for 5min, and Na is added2GeO32mL of the solution. Adjusting the pH value to 8.5 by using concentrated ammonia water, continuously stirring for 1h, loading into a high-pressure reaction kettle with a 50mL polytetrafluoroethylene lining, placing into an electric heating forced air drying oven, heating to 220 ℃, preserving heat for 4h, naturally reducing to room temperature, taking out reactants, carrying out three to four times of high-speed centrifugal washing, placing into the electric heating forced air drying oven, preserving heat for 120 ℃, drying for 12h, and grinding to obtain the zinc-germanium oxide long-afterglow luminescent material.
The thermal field emission scanning electron microscope of the zinc-germanium oxide long-afterglow luminescent material prepared in this example is shown in fig. 3, the fluorescence emission spectrum is shown in fig. 5, and the fluorescence excitation spectrum is shown in fig. 6. Excitation peak at 300nm and emission peak at 472nm, belonging to Eu3+4f of65d1→4f7And (4) transition. Irradiating with ultraviolet lamp for 10min, and observing in dark place after irradiation is stopped to give green afterglow. FIG. 7 is an afterglow decay diagram of the material, fromAs can be seen in the figure, the material can continuously emit light for more than 500 s. FIG. 8 is the XRD spectrum of the material, from which diffraction peaks can be seen to be consistent with standard cards, which shows that the zinc germanium oxide long afterglow material is successfully prepared.
Example 4: this example has a chemical composition formula of Zn2GeO4：0.005Eu3+The preparation method of the long afterglow material comprises the following steps:
get GeO20.52364g of Na was dissolved in 10mL of 3mol/L NaOH solution to prepare Na2GeO3A solution; scale Zn (NO)3)2·3H2O 5.2996g，Eu(NO3)3·6H20.0043g of O is respectively prepared into 100mL of solution, 10mL of the solution is respectively put into the same 100mL beaker, 3 mu L of concentrated nitric acid is added, the mixture is stirred for 5min, and Na is added2GeO3The solution was 2 mL. Adjusting the pH value to 9.5 by using concentrated ammonia water, continuously stirring for 1h, loading into a high-pressure reaction kettle with a 50mL polytetrafluoroethylene lining, placing into an electric heating forced air drying oven, heating to 220 ℃, preserving heat for 4h, naturally reducing to room temperature, taking out reactants, carrying out three to four times of high-speed centrifugal washing, placing into the electric heating forced air drying oven, preserving heat for 120 ℃, drying for 12h, and grinding to obtain the zinc-germanium oxide long-afterglow luminescent material.
The thermal field emission scanning electron microscope of the zinc-germanium oxide long-afterglow luminescent material prepared in this example is shown in fig. 4, the fluorescence emission spectrum is shown in fig. 5, and the fluorescence excitation spectrum is shown in fig. 6. Excitation peak at 300nm and emission peak at 472nm, belonging to Eu3+4f of65d1→4f7And (4) transition. Irradiating with ultraviolet lamp for 10min, and observing in dark place after irradiation is stopped to give green afterglow. FIG. 7 is a graph showing the decay of afterglow of the material, and it can be seen that the material can continuously emit light for 500s or more. FIG. 8 is the XRD spectrum of the material, from which diffraction peaks can be seen to be consistent with standard cards, which shows that the zinc germanium oxide long afterglow material is successfully prepared.
Claims (5)
1. A zinc germanium oxide long afterglow luminescent material is characterized in that: the chemical composition formula is Zn2GeO4: XC, wherein C is Eu3+OrDy3+，0.001≤X≤0.1。
2. The long afterglow material of claim 1 wherein the oxide has an excitation spectrum ranging from 260 to 330nm, an emission spectrum ranging from 400 to 500nm, and a peak around 472 nm.
3. A method for preparing the zinc-germanium oxide long-afterglow luminescent material of claim 1 or claim 2, which comprises the following steps: separately preparing Zn (NO)3)2，Na2GeO3，Eu(NO3)3，Dy(NO3)3The aqueous solution of (1) is fully mixed according to the proportion; continuously stirring for 1h after the pH value is adjusted to be 6-10; putting the mixed solution into a high-temperature reaction kettle with a polytetrafluoroethylene lining, reacting for 4 hours at 220 ℃, cooling to room temperature, and taking out reactants; after washing and drying treatment, the product zinc germanium oxide long afterglow luminescent material is obtained.
4. The method for preparing the zinc-germanium oxide long-afterglow luminescent material as claimed in claim 3, wherein the method comprises the following steps: zn (NO) in the reaction mixture3)2And Na2GeO3The molar ratio of (A) to (B) is 2: 1.
5. The method for preparing the zinc-germanium oxide long-afterglow luminescent material as claimed in claim 3, wherein the method comprises the following steps: zn (NO) in the reaction mixture3)2And the proportion of the deionized water is 1-10 mmol/20 mL.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113425684A (en) * | 2021-06-07 | 2021-09-24 | 江南大学 | Zinc germanate based nano material capable of performing afterglow light monitoring, slowly releasing and resisting bacteria and preparation method thereof |
| CN114149804A (en) * | 2021-10-12 | 2022-03-08 | 宁夏大学 | Strontium-europium-doped zinc germanate-based blue long-afterglow nano material |
| CN115873594A (en) * | 2022-12-06 | 2023-03-31 | 济南大学 | Low-temperature solution method synthesis process of transparent cadmium-based long-afterglow crystal |
-
2021
- 2021-01-20 CN CN202110072014.4A patent/CN112680223A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113425684A (en) * | 2021-06-07 | 2021-09-24 | 江南大学 | Zinc germanate based nano material capable of performing afterglow light monitoring, slowly releasing and resisting bacteria and preparation method thereof |
| CN114149804A (en) * | 2021-10-12 | 2022-03-08 | 宁夏大学 | Strontium-europium-doped zinc germanate-based blue long-afterglow nano material |
| CN115873594A (en) * | 2022-12-06 | 2023-03-31 | 济南大学 | Low-temperature solution method synthesis process of transparent cadmium-based long-afterglow crystal |
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