CN110093154B - Mg2+/Si4+Substituted Ga3+Doped with Cr3+Zinc gallate based near-infrared long afterglow material and preparation method thereof - Google Patents
Mg2+/Si4+Substituted Ga3+Doped with Cr3+Zinc gallate based near-infrared long afterglow material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of material science and provides Mg2+/Si4+Substituted Ga3+Doped with Cr3+Zinc gallate based near infrared long afterglow material and its preparation process. The invention adopts a sol-gel method, takes trihydroxymethyl aminomethane as a complexing agent, and finally prepares the near-infrared long afterglow fluorescent powder through a complexing process, a nitrogen removing process and a calcining process at 900-1300 ℃. The size of the fluorescent powder is below 100nm, and the fluorescent powder has good dispersibility. The scheme of the invention is simple and easy to implement, and Mg is regulated and controlled2+/Si4+、Cr3+The doping amount can improve the performance of the rest glow, shows a good theoretical basis for the preparation of the novel commercial fluorescent powder, and has extremely high guiding significance and application prospect.
Description
Technical Field
The invention belongs to the field of material science, and particularly relates to Mg2+/Si4+Substituted Ga3+Doped with Cr3+Zinc gallate based near infrared long afterglow material and its preparation process.
Background
The long afterglow material is one kind of matter capable of absorbing energy and emitting light after stopping excitation, and has wide application in lighting, safety indication, biomedicine and other fields. Common long afterglow materials include aluminate, silicate, titanate, and the like. The near-infrared long afterglow material is a material with an emission wavelength in a near-infrared band, and has an ultra-long afterglow life, can realize in-vitro excitation and in-vivo detection, avoids the damage caused by in-situ excitation and tissue autofluorescence, and recently, the use of the near-infrared long afterglow material for biological living body imaging and disease diagnosis becomes a research hotspot. Cr (chromium) component3+The doped material is a luminescent center dopant capable of emitting light in a near infrared band, and the band of the dopant is just positioned in a first window of 'bio-optics', so the doped material has very important application value. And zinc gallate doped with Cr3+Is also a near-infrared long-afterglow luminescent material which is researched more at present.
ZnGa2O4:Cr3+The preparation of the near-infrared long-afterglow material is mostly prepared by a solid-phase method and a hydrothermal method, and the preparation by a sol-gel method is relatively less. Compared with the solid phase method for preparing larger particles, the liquid phaseThe fluorescent powder prepared by the method has lower luminous intensity, and the sol-gel method integrates the advantages of the two preparation methods, and has the advantages of high afterglow intensity and small particle size; ZnGa2O4Matrix doped with Cr3+The remaining glow is relatively weak, passing Mg2+/Si4+Doped with substituted Ga3+The ions can inhibit Ga3+The volatilization of ions generates electron compensation defects and lattice distortion defects, generates more traps and enhances the luminous intensity and afterglow performance of the traps.
Disclosure of Invention
The invention provides a method for preparing a near-infrared long-afterglow material, which adopts a sol-gel method and successfully synthesizes the near-infrared long-afterglow material. And by controlling Mg2+/Si4+、Cr3+The doping amount can improve the performance of the residual glow.
The technical scheme of the invention is as follows:
mg2+/Si4+Substituted Ga3+Doped with Cr3+The zinc gallate based near infrared long afterglow material preparing process includes the following steps:
step 1: adding Zn (NO)3)2Solution, Ga (NO)3)3Solution, SiO2Powder, Mg (NO)3)2Solution and Cr (NO)3)3Mixing the solutions, and mixing Zn in the solution2+、Ga3+、Mg2+、Si4+And Cr3+In a molar ratio of 1 (2-x) x/2: x/2: y, wherein 0<x is less than or equal to 2, and y is less than or equal to 0.001 and less than or equal to 0.1; zn in the solution2+、Ga3+、Mg2+、Si4+And Cr3+The total mole number of the N is set as N;
step 2: transferring the mixed solution obtained in the step (1) to a water bath kettle, covering a membrane and stirring for 1-2h at the water temperature of 80-90 ℃; removing the film, and then adding trihydroxymethyl aminomethane, wherein the ratio of the molar number of the trihydroxymethyl aminomethane to N is 1-2: 1; continuously covering the film and stirring for 1-2h at the temperature of 80-90 ℃; removing the film and evaporating water until the solution forms a gel state;
and step 3: transferring the gel into an oven, drying for 2-3 h at 180-230 ℃, and drying for 0.5-1h at 230-250 ℃ for nitrogen removal treatment to obtain black precursor powder; and grinding the precursor powder, and calcining at 900-1300 ℃ to obtain the fluorescent powder emitting the near-infrared long afterglow when excited by an ultraviolet lamp.
Furthermore, x is more than or equal to 0.01 and less than or equal to 0.2, and y is more than or equal to 0.004 and less than or equal to 0.006 in the step 1.
Preferably, in step 1, x is 0.01.
Preferably, in step 1, y is 0.005.
The invention has the beneficial effects that:
the sol-gel method is used to prepare the near-infrared long-afterglow nano material, the size of which is below 100nm, and the dispersibility of which is good. By controlling Mg2+/Si4+、Cr3+The doping amount can be made to be ZnGa2O4:Cr3+The luminescent property and afterglow property of the near infrared long afterglow material are greatly improved.
Drawings
FIG. 1 is an XRD pattern of the products prepared in examples 1-4 of the present invention;
FIG. 2 is a luminescence spectrum of a product prepared by a comparative example of the present invention;
FIG. 3 is an afterglow spectrum of a product prepared according to a comparative example of the present invention after excitation with a 254nm laser for five minutes;
FIG. 4 is a luminescence spectrum of a product prepared in example 1 of the present invention;
FIG. 5 is an afterglow spectrum of a product prepared in example 1 of the present invention after being excited by a 254nm laser for five minutes;
FIG. 6 is a luminescence spectrum of a product prepared in example 2 of the present invention;
FIG. 7 is an afterglow spectrum of a product prepared in example 2 of the present invention after being excited by a 254nm laser for five minutes;
FIG. 8 is a luminescence spectrum of a product prepared in example 3 of the present invention;
FIG. 9 is an afterglow spectrum of a product prepared in example 3 of the present invention after being excited by a 254nm laser for five minutes;
FIG. 10 is a luminescence spectrum of a product prepared in example 4 of the present invention;
FIG. 11 is an afterglow spectrum of a product prepared in example 4 of the present invention after being excited by a 254nm laser for five minutes.
Detailed Description
The following detailed description of the embodiments of the invention refers to the accompanying drawings.
The chemical reagents used in the examples of the present invention are analytical grade products.
Comparative example (x-0, y-0.005,900 ℃ C.)
Ga (NO) of 0.4mol/L is accurately measured3)3Solution 10mL, 1mol/L Zn (NO)3)2Solution 2mL, 0.1mol/L Cr (NO)3)30.1mL of the solution was added to 50mL of deionized water with stirring. The solution was transferred to a water bath and stirred for 1h at 85 ℃ with a cover membrane. After the membrane is removed, 0.725g of tris (hydroxymethyl) aminomethane is added, and the membrane is covered continuously and the stirring is carried out for 1h at the temperature of 85 ℃. And (5) removing the film, evaporating water for 4-5 h, and forming a gel state by the solution after water is evaporated. Transferring the gel into a drying oven, drying for 2h at 200 ℃, drying for 30min at 230 ℃ for nitrogen removal treatment to obtain ZnGa2O4:0.005Cr3+Black precursor powder. Grinding the precursor, transferring the ground precursor into an alumina crucible, heating to 700 ℃ at 5 ℃/min by using a programmed heating resistance box furnace under the condition of oxygen, heating to 900 ℃ from 700 ℃ at 8 ℃/min, preserving heat for 4h at 900 ℃, cooling to 700 ℃ at 5 ℃/min, and then cooling along with the furnace. Grinding to obtain ZnGa2O4:0.005Cr3+And (3) fluorescent powder.
Example 1 (x-0.01, y-0.1,900 ℃ C.)
Accurately weigh 0.0006g SiO2Measuring 0.1mol/L of Mg (NO)20.1ml of solution, accurately measuring Ga (NO) of 0.4mol/L3)3Solution 9.95mL, 1mol/L Zn (NO)3)2Solution 2mL, 0.1mol/L Cr (NO)3)32mL of the solution was added to 50mL of deionized water with stirring. The solution was transferred to a water bath and stirred for 1h at 85 ℃ with a cover membrane. After the membrane is removed, 0.725g of tris (hydroxymethyl) aminomethane is added, and the membrane is covered continuously and the stirring is carried out for 1h at the temperature of 85 ℃. And (5) removing the film, evaporating water for 4-5 h, and forming a gel state by the solution after water is evaporated. Transferring the gel into a drying oven, drying for 2h at 200 ℃, drying for 30min at 230 ℃ for nitrogen removal treatment to obtain ZnGa1.99(Mg2+/Si4+)0.01O4:0.1Cr3+Black precursor powder. Grinding the precursor, transferring the ground precursor into an alumina crucible, heating to 700 ℃ at 5 ℃/min by using a programmed heating resistance box furnace under the condition of oxygen, heating to 900 ℃ from 700 ℃ at 8 ℃/min, preserving heat for 4h at 900 ℃, cooling to 700 ℃ at 5 ℃/min, and then cooling along with the furnace. Grinding to obtain ZnGa1.99(Mg2 +/Si4+)0.01O4:0.1Cr3+And (3) fluorescent powder.
Example 2(x 0.01, y 0.005,1000 ℃)
Accurately weighing 0.0006gSiO2Measuring 0.1mol/L of Mg (NO)2Solution 0.1ml, 0.4mol/L Ga (NO)3)3Solution 9.95mL, 1mol/L Zn (NO)3)2Solution 2mL, 0.1mol/L Cr (NO)3)30.1mL of the solution was added to 50mL of deionized water with stirring. The solution was transferred to a water bath and stirred for 1h at 85 ℃ with a cover membrane. After the film is uncovered, 1.088g of tris (hydroxymethyl) aminomethane is added, and the film is covered continuously and stirred for 1h at 85 ℃. And (5) removing the film, evaporating water for 4-5 h, and forming a gel state by the solution after water is evaporated. Transferring the gel into a drying oven, drying for 2h at 200 ℃, drying for 30min at 230 ℃ for nitrogen removal treatment to obtain ZnGa1.99(Mg2+/Si4+)0.01O4:0.005Cr3+Black precursor powder. Grinding the precursor, transferring the ground precursor into an alumina crucible, heating to 700 ℃ at 5 ℃/min by using a programmed heating resistance box furnace under the condition of oxygen, heating to 900 ℃ from 700 ℃ at 8 ℃/min, preserving heat for 4h, cooling to 700 ℃ at 5 ℃/min, and then cooling along with the furnace. Then calcining at 1000 ℃ with the same heating rate and process as 900 ℃. Grinding to obtain ZnGa1.99(Mg2+/Si4+)0.01O4:0.005Cr3+And (3) fluorescent powder.
Example 3 (x-1, y-0.001,1200 ℃ C.)
Accurately weighing 0.06gSiO2Measuring 0.1mol/L of Mg (NO)2Solution 10ml, 0.4mol/L Ga (NO)3)3Solution 5mL, 1mol/L Zn (NO)3)2Solution 2mL, 0.1mol/L Cr (NO)3)30.02mL of the solution was stirredDeionized water was added to 50 mL. The solution was transferred to a water bath and stirred for 1h at 85 ℃ with a cover membrane. After the film is uncovered, 1.233g of tris (hydroxymethyl) aminomethane is added, and the film is covered continuously and stirred for 1h at 85 ℃. And (5) removing the film, evaporating water for 4-5 h, and forming a gel state by the solution after water is evaporated. Transferring the gel into an oven, drying at 200 deg.C for 2h, and drying at 230 deg.C for 30min for removing nitrogen to obtain ZnGa (Mg)2+/Si4+)O4: 0.001Cr3+Black precursor powder. Grinding the precursor, transferring the ground precursor into an alumina crucible, heating to 700 ℃ at 5 ℃/min by using a programmed heating resistance box furnace under the condition of oxygen, heating to 900 ℃ from 700 ℃ at 8 ℃/min, preserving heat for 4h, cooling to 700 ℃ at 5 ℃/min, and then cooling along with the furnace. Then, the sintering is carried out at 1200 ℃, and the heating rate and the process are the same as 900 ℃. After grinding ZnGa (Mg) is obtained2+/Si4+)O4:0.001Cr3+And (3) fluorescent powder.
Example 4 (x-2, y-0.005,1300 ℃ C.)
Accurately weighing 0.12gSiO2Measuring 0.1mol/L of Mg (NO)220ml of solution, 1mol/L of Zn (NO)3)2Solution 2mL, 0.1mol/L Cr (NO)3)30.1mL of the solution was added to 50mL of deionized water with stirring. The solution was transferred to a water bath and stirred for 1h at 85 ℃ with a cover membrane. After the film is removed, 1.45g of tris (hydroxymethyl) aminomethane is added, and the film is covered continuously and stirred for 1h at the temperature of 85 ℃. And (5) removing the film, evaporating water for 4-5 h, and forming a gel state by the solution after water is evaporated. Transferring the gel into an oven, drying at 200 deg.C for 2 hr, drying at 230 deg.C for 30min for removing nitrogen to obtain Zn (Mg)2+/Si4+)2O4:0.005Cr3+Black precursor powder. Grinding the precursor, transferring the ground precursor into an alumina crucible, heating to 700 ℃ at 5 ℃/min by using a programmed heating resistance box furnace under the condition of oxygen, heating to 900 ℃ from 700 ℃ at 8 ℃/min, preserving heat for 4h, cooling to 700 ℃ at 5 ℃/min, and then cooling along with the furnace. Then, the mixture is calcined at 1300 ℃, the temperature is increased to 700 ℃ at 5 ℃/min, the temperature is increased from 700 ℃ to 1300 ℃ at 5 ℃/min, the temperature is kept for 4h, the temperature is reduced to 700 ℃ at 5 ℃/min, and then the mixture is cooled along with the furnace. Zn (Mg) is obtained after grinding2+/Si4+)2O4:0.005Cr3+And (3) fluorescent powder.
Mg can be seen by comparing the emission spectrum intensity in the luminescence spectrum with the afterglow intensity in the afterglow spectrum2+/Ge4+Substituted Ga3+Post-doped Cr3+The zinc gallate based near infrared long afterglow fluorescent material has raised luminous and afterglow performance.
Claims (5)
1. Mg2+/Si4+Substituted Ga3+Doped with Cr3+The preparation method of the zinc gallate based near-infrared long afterglow material is characterized by comprising the following steps:
step 1: adding Zn (NO)3)2Solution, Ga (NO)3)3Solution, SiO2Powder, Mg (NO)3)2Solution and Cr (NO)3)3Mixing the solutions, and mixing Zn in the solution2+、Ga3+、Mg2+、Si4+And Cr3+In a molar ratio of 1 (2-x) x/2: x/2: y, wherein 0<x<2, y is more than or equal to 0.001 and less than or equal to 0.1; zn in the solution2+、Ga3+、Mg2+、Si4+And Cr3+The total mole number of the N is set as N;
step 2: transferring the mixed solution obtained in the step (1) to a water bath kettle, covering a membrane and stirring for 1-2h at the water temperature of 80-90 ℃; removing the film, and adding trihydroxymethyl aminomethane, wherein the ratio of the molar number of the trihydroxymethyl aminomethane to N is 1-2: 1; continuously covering the film and stirring for 1-2h at the temperature of 80-90 ℃; removing the film and evaporating water until the solution forms a gel state;
and step 3: transferring the gel into an oven, drying for 2-3 h at 180-230 ℃, and drying for 0.5-1h at 230-250 ℃ for nitrogen removal treatment to obtain black precursor powder; and grinding the precursor powder, and calcining at 900-1300 ℃ to obtain the fluorescent powder emitting the near-infrared long afterglow when excited by an ultraviolet lamp.
2. Mg of claim 12+/Si4+Substituted Ga3+Doped with Cr3+The preparation method of the zinc gallate based near-infrared long afterglow material is characterized in that x is more than or equal to 0.01 and less than or equal to 0.2, and y is more than or equal to 0.004 and less than or equal to 0.006 in the step 1.
3. Mg of claim 12+/Si4+Substituted Ga3+Doped with Cr3+The zinc gallate based near infrared long afterglow material preparing process features that in step 1, x is 0.01.
4. Mg of claim 12+/Si4+Substituted Ga3+Doped with Cr3+The zinc gallate based near infrared long afterglow material preparing process features that in step 1, y is 0.005.
5. Mg obtainable by a process according to any one of claims 1 to 42+/Si4+Substituted Ga3+Doped with Cr3+Zinc gallate based near infrared long afterglow material.
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