CN110093154A - Mg2+/Si4+Replace Ga3+Mix Cr3+Gallic acid zinc-base near-infrared long-afterglow material and preparation method - Google Patents
Mg2+/Si4+Replace Ga3+Mix Cr3+Gallic acid zinc-base near-infrared long-afterglow material and preparation method Download PDFInfo
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- CN110093154A CN110093154A CN201910435116.0A CN201910435116A CN110093154A CN 110093154 A CN110093154 A CN 110093154A CN 201910435116 A CN201910435116 A CN 201910435116A CN 110093154 A CN110093154 A CN 110093154A
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
- C09K11/685—Aluminates; Silicates
Abstract
The invention belongs to materials science fields, propose Mg2+/Si4+Replace Ga3+Mix Cr3+Gallic acid zinc-base near-infrared long-afterglow material and preparation method.The present invention by complexation process, denitrogenates process, 900~1300 DEG C of calcination process finally obtained near-infrared long lad phosphor as complexing agent using sol-gal process, trishydroxymethylaminomethane.Fluorescent powder size is in 100nm hereinafter, having good dispersibility.The present invention program is simple and easy, by regulating and controlling Mg2+/Si4+、Cr3+Doping can improve its afterglow property, illustrate good theoretical basis for the preparation of novel Commercial optical powder, have high directive significance and application prospect.
Description
Technical field
The invention belongs to materials science fields, and in particular to a kind of Mg2+/Si4+Replace Ga3+Mix Cr3+Gallic acid zinc-base is closely red
Outer long-afterglow material and preparation method.
Background technique
Long-afterglow material is a kind of absorption energy and stops the substance of subsequent supervention light in excitation, is illuminating, safety instruction,
The fields such as bio-medical extensive application.Common long-afterglow material has aluminate-base, silicate-base and metatitanic acid alkali etc..Closely
Infrared long-afterglow material is a kind of material of launch wavelength near infrared band, since near-infrared long-afterglow material has more than overlength
The brightness service life, and excitation, vivo detection in vitro may be implemented, excitation in situ and the damage of tissue auto fluorescence bring are avoided,
Recently biological living imaging is carried out using near-infrared long-afterglow material, medical diagnosis on disease becomes research hotspot.Cr3+It is that one kind can be sent out
The centre of luminescence dopant of near infrared band light is penetrated, and its wave band is placed exactly in " Photobiology " first window, therefore has
Very important application value.And gallic acid zinc mixes Cr3+And a kind of more near-infrared long after glow luminous material is studied at present.
ZnGa2O4:Cr3+The preparation of near-infrared long-afterglow material is prepared by solid phase method and hydro-thermal method mostly, and colloidal sol is solidifying
Glue method prepares relatively fewer.It is larger that particle is made relative to solid phase method, and liquid phase method is made that light-emitting phosphor intensity is lower, and colloidal sol is solidifying
Glue method integrates both the above preparation method advantage, has afterglow intensity height, the small advantage of particle size；ZnGa2O4Matrix is mixed
Cr3+Its afterglow property is relatively weak, passes through Mg2+/Si4+Doped and substituted Ga3+Ion can inhibit Ga3+The volatilization of ion generates
Electronic compensation defect and distortion of lattice defect, generate more traps, enhance its luminous intensity and afterglow property.
Summary of the invention
The present invention provides a kind of method for preparing near-infrared long-afterglow material, and using sol-gal process, and successfully, synthesis is close
Infrared long-afterglow material.And pass through control Mg2+/Si4+、Cr3+Doping can improve its afterglow property.
Technical solution of the present invention:
A kind of Mg2+/Si4+Replace Ga3+Mix Cr3+Gallic acid zinc-base near-infrared long-afterglow material preparation method, including step is such as
Under:
Step 1: by Zn (NO3)2Solution, Ga (NO3)3Solution, SiO2Powder, Mg (NO3)2Solution and Cr (NO3)3Solution is mixed
It closes, Zn in mixed solution2+、Ga3+、Mg2+、Si4+And Cr3+Molar ratio be 1:(2-x): x/2:x/2:y, wherein 0 < x≤2,
0.001≤y≤0.1；By the Zn in solution2+、Ga3+、Mg2+、Si4+And Cr3+Total mole number be set as N；
Step 2: the mixed solution that step 1 is obtained is transferred in water-bath, stirs 1- in 80-90 DEG C of water temperature hypophragm
2h；Trishydroxymethylaminomethane is added after taking off film, the molal quantity of trishydroxymethylaminomethane and the ratio of N are 1~2:1；After
1-2h is stirred at continuous 80-90 DEG C of epiphragma；It takes off film and steams water to solution formation gel state；
Step 3: gel being transferred in baking oven, 2~3h is dried at 180~230 DEG C, 0.5-1h is dried at 230~250 DEG C and carries out
Processing is denitrogenated, black precursor powder is made；900~1300 DEG C of calcinings are carried out after precursor powder is ground, and obtain ultraviolet lamp
Emit the fluorescent powder of near-infrared long afterglow when excitation.
Further, 0.01≤x≤0.2 in above-mentioned steps 1,0.004≤y≤0.006.
X=0.01 in preferred steps 1.
Y=0.005 in preferred steps 1.
Beneficial effects of the present invention:
Sol-gal process prepares near-infrared long-persistence nano material, and size is in 100nm hereinafter, good dispersion.Pass through
Control Mg2+/Si4+、Cr3+Doping can make ZnGa2O4:Cr3+The luminescent properties and twilight sunset of near-infrared long-afterglow material
It can improve a lot.
Detailed description of the invention
Fig. 1 is the XRD spectrum of the product of 1-4 of embodiment of the present invention preparation；
Fig. 2 is the luminous map of the product of comparative example preparation of the present invention；
Fig. 3 is twilight sunset map of the product of comparative example preparation of the present invention after 254nm laser excitation five minutes；
Fig. 4 is the luminous map of product prepared by the embodiment of the present invention 1；
Fig. 5 is twilight sunset map of the product of the preparation of the embodiment of the present invention 1 after 254nm laser excitation five minutes；
Fig. 6 is the luminous map of product prepared by the embodiment of the present invention 2；
Fig. 7 is twilight sunset map of the product of the preparation of the embodiment of the present invention 2 after 254nm laser excitation five minutes；
Fig. 8 is the luminous map of product prepared by the embodiment of the present invention 3；
Fig. 9 is twilight sunset map of the product of the preparation of the embodiment of the present invention 3 after 254nm laser excitation five minutes；
Figure 10 is the luminous map of product prepared by the embodiment of the present invention 4；
Figure 11 is twilight sunset map of the product of the preparation of the embodiment of the present invention 4 after 254nm laser excitation five minutes.
Specific embodiment
Specific embodiments of the present invention are described in detail below in conjunction with technical solution and attached drawing.
Chemical reagent employed in present example is the pure grade product of analysis.
Comparative example (x=0, y=0.005,900 DEG C)
Accurate Ga (the NO for measuring 0.4mol/L3)3Zn (the NO of solution 10mL, 1mol/L3)2Solution 2mL, 0.1mol/L's
Cr(NO3)3Deionized water is added to 50mL in solution 0.1mL while stirring.Above-mentioned solution is transferred in water-bath, at 85 DEG C
Water temperature hypophragm stirs 1h.0.725g trishydroxymethylaminomethane is added after taking off film, continues to stir 1h at 85 DEG C of epiphragma.Take off film steaming
4~5h of water waits for that moisture evaporates, and solution forms gel state.Gel is transferred in baking oven, 2h is dried at 200 DEG C, is dried at 230 DEG C
30min carries out denitrogenating processing, and ZnGa is made2O4:0.005Cr3+Black precursor powder.It will be transferred to after the grinding of above-mentioned presoma
In alumina crucible, be warming up to 700 DEG C under Oxygen Condition using temperature programming resistance batch-type furnace with 5 °/min, 8 °/min from
700 DEG C are warming up to 900 DEG C, and 4h is kept the temperature at 900 DEG C, and 5 °/min is cooled to 700 DEG C, furnace cooling later.It is obtained after grinding
ZnGa2O4:0.005Cr3+Fluorescent powder.
Embodiment 1 (x=0.01, y=0.1,900 DEG C)
Accurately weigh 0.0006g SiO2, measure the Mg (NO) of 0.1mol/L2Solution 0.1ml is accurate to measure 0.4mol/L's
Ga(NO3)3Zn (the NO of solution 9.95mL, 1mol/L3)2Cr (the NO of solution 2mL, 0.1mol/L3)3Solution 2mL, while stirring plus
Enter deionized water to 50mL.Above-mentioned solution is transferred in water-bath, stirs 1h in 85 DEG C of water temperature hypophragms.It is added after taking off film
0.725g trishydroxymethylaminomethane continues to stir 1h at 85 DEG C of epiphragma.It takes off film steaming 4~5h of water and waits for that moisture evaporates, solution is formed
Gel state.Gel is transferred in baking oven, 2h is dried at 200 DEG C, 30min is dried at 230 DEG C and carries out denitrogenating processing, be made
ZnGa1.99(Mg2+/Si4+)0.01O4:0.1Cr3+Black precursor powder.Alumina crucible will be transferred to after the grinding of above-mentioned presoma
In, 700 DEG C are warming up to 5 °/min under Oxygen Condition using temperature programming resistance batch-type furnace, 8 °/min is warming up to from 700 DEG C
900 DEG C, 4h is kept the temperature at 900 DEG C, 5 °/min is cooled to 700 DEG C, furnace cooling later.ZnGa is obtained after grinding1.99(Mg2+/
Si4+)0.01O4:0.1Cr3+Fluorescent powder.
Embodiment 2 (x=0.01, y=0.005,1000 DEG C)
Accurately weigh 0.0006gSiO2, measure the Mg (NO) of 0.1mol/L2Ga (the NO of solution 0.1ml, 0.4mol/L3)3
Zn (the NO of solution 9.95mL, 1mol/L3)2Cr (the NO of solution 2mL, 0.1mol/L3)3Solution 0.1mL is added goes while stirring
Ionized water is to 50mL.Above-mentioned solution is transferred in water-bath, stirs 1h in 85 DEG C of water temperature hypophragms.It is added after taking off film
1.088g trishydroxymethylaminomethane continues to stir 1h at 85 DEG C of epiphragma.It takes off film steaming 4~5h of water and waits for that moisture evaporates, solution is formed
Gel state.Gel is transferred in baking oven, 2h is dried at 200 DEG C, 30min is dried at 230 DEG C and carries out denitrogenating processing, be made
ZnGa1.99(Mg2+/Si4+)0.01O4:0.005Cr3+Black precursor powder.Aluminium oxide earthenware will be transferred to after the grinding of above-mentioned presoma
In crucible, 700 DEG C are warming up to 5 °/min under Oxygen Condition using temperature programming resistance batch-type furnace, 8 °/min heats up from 700 DEG C
To 900 DEG C, 4h is kept the temperature, 5 °/min is cooled to 700 DEG C, furnace cooling later.1000 DEG C of calcinings, heating rate and mistake are carried out later
Journey is the same as 900 DEG C.ZnGa is obtained after grinding1.99(Mg2+/Si4+)0.01O4:0.005Cr3+Fluorescent powder.
Embodiment 3 (x=1, y=0.001,1200 DEG C)
Accurately weigh 0.06gSiO2, measure the Mg (NO) of 0.1mol/L2Ga (the NO of solution 10ml, 0.4mol/L3)3Solution
Zn (the NO of 5mL, 1mol/L3)2Cr (the NO of solution 2mL, 0.1mol/L3)3Solution 0.02mL, is added deionized water while stirring
To 50mL.Above-mentioned solution is transferred in water-bath, stirs 1h in 85 DEG C of water temperature hypophragms.Tri- hydroxyl of 1.233g is added after taking off film
Aminomethane continues to stir 1h at 85 DEG C of epiphragma.It takes off film steaming 4~5h of water and waits for that moisture evaporates, solution forms gel state.It will
Gel is transferred in baking oven, and 2h is dried at 200 DEG C, 30min is dried at 230 DEG C and carries out denitrogenating processing, ZnGa (Mg is made2+/Si4+)O4:
0.001Cr3+Black precursor powder.It will be transferred in alumina crucible after the grinding of above-mentioned presoma, use temperature programming resistance
Batch-type furnace is warming up to 700 DEG C under Oxygen Condition with 5 °/min, and 8 °/min is warming up to 900 DEG C from 700 DEG C, keeps the temperature 4h, and 5 °/min
700 DEG C are cooled to, later furnace cooling.1200 DEG C of calcinings are carried out later, and heating rate and process are the same as 900 DEG C.After grinding
To ZnGa (Mg2+/Si4+)O4:0.001Cr3+Fluorescent powder.
Embodiment 4 (x=2, y=0.005,1300 DEG C)
Accurately weigh 0.12gSiO2, measure the Mg (NO) of 0.1mol/L2Zn (the NO of solution 20ml, 1mol/L3)2Solution
Cr (the NO of 2mL, 0.1mol/L3)3Deionized water is added to 50mL in solution 0.1mL while stirring.Above-mentioned solution is transferred to water
In bath, 1h is stirred in 85 DEG C of water temperature hypophragms.1.45g trishydroxymethylaminomethane is added after taking off film, continues 85 DEG C of epiphragma
Lower stirring 1h.It takes off film steaming 4~5h of water and waits for that moisture evaporates, solution forms gel state.Gel is transferred in baking oven, at 200 DEG C
2h is dried, 30min is dried at 230 DEG C and carries out denitrogenating processing, Zn (Mg is made2+/Si4+)2O4:0.005Cr3+Black precursor powder.It will
It is transferred in alumina crucible after above-mentioned presoma grinding, using temperature programming resistance batch-type furnace with 5 °/min under Oxygen Condition
700 DEG C are warming up to, 8 °/min is warming up to 900 DEG C from 700 DEG C, keeps the temperature 4h, and 5 °/min is cooled to 700 DEG C, furnace cooling later.It
1300 DEG C of calcinings are carried out afterwards, are warming up to 700 DEG C with 5 °/min, 5 °/min is warming up to 1300 DEG C from 700 DEG C, keep the temperature 4h, 5 °/min
700 DEG C are cooled to, later furnace cooling.Zn (Mg is obtained after grinding2+/Si4+)2O4:0.005Cr3+Fluorescent powder.
It can be seen that Mg by comparing the afterglow intensity in the intensity of emission spectra and twilight sunset map in the map that shines2+/
Ge4+Replace Ga3+Afterwards mix Cr3+Shine and the afterglow property of gallic acid zinc-base near-infrared long-afterglow fluorescent material are improved.
Claims (5)
1. a kind of Mg2+/Si4+Replace Ga3+Mix Cr3+Gallic acid zinc-base near-infrared long-afterglow material preparation method, which is characterized in that
It comprises the following steps that
Step 1: by Zn (NO3)2Solution, Ga (NO3)3Solution, SiO2Powder, Mg (NO3)2Solution and Cr (NO3)3Solution mixing, is mixed
Close Zn in solution2+、Ga3+、Mg2+、Si4+And Cr3+Molar ratio be 1:(2-x): x/2:x/2:y, wherein 0 < x≤2,0.001≤y
≤0.1；By the Zn in solution2+、Ga3+、Mg2+、Si4+And Cr3+Total mole number be set as N；
Step 2: the mixed solution that step 1 is obtained is transferred in water-bath, stirs 1-2h in 80-90 DEG C of water temperature hypophragm；
Trishydroxymethylaminomethane is added after taking off film, the molal quantity of trishydroxymethylaminomethane and the ratio of N are 1~2:1；Continue to cover
1-2h is stirred at 80-90 DEG C of film；It takes off film and steams water to solution formation gel state；
Step 3: gel being transferred in baking oven, 2~3h is dried at 180~230 DEG C, 0.5-1h is dried at 230~250 DEG C and is denitrogenated
Black precursor powder is made in processing；900~1300 DEG C of calcinings are carried out after precursor powder is ground, and obtain ultraviolet lamp excitation
When emit near-infrared long afterglow fluorescent powder.
2. Mg according to claim 12+/Si4+Replace Ga3+Mix Cr3+Gallic acid zinc-base near-infrared long-afterglow material preparation side
Method, which is characterized in that 0.01≤x≤0.2 in step 1,0.004≤y≤0.006.
3. Mg according to claim 12+/Si4+Replace Ga3+Mix Cr3+Gallic acid zinc-base near-infrared long-afterglow material preparation side
Method, which is characterized in that x=0.01 in step 1.
4. Mg according to claim 12+/Si4+Replace Ga3+Mix Cr3+Gallic acid zinc-base near-infrared long-afterglow material preparation side
Method, which is characterized in that y=0.005 in step 1.
5. the Mg being prepared using any the method for claim 1-42+/Si4+Replace Ga3+Mix Cr3+Gallic acid zinc-base is closely red
Outer long-afterglow material.
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Cited By (5)
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| CN111187620A (en) * | 2020-01-19 | 2020-05-22 | 南京邮电大学 | Novel Zn2GeO4Base green long afterglow nano material and its preparation method |
| CN113046066A (en) * | 2021-03-29 | 2021-06-29 | 喀什大学 | Size-adjustable near-infrared luminescent long-afterglow nano material and preparation method thereof |
| CN113881427A (en) * | 2021-10-19 | 2022-01-04 | 喀什大学 | Preparation of long afterglow luminescent nano material with double emission and anti-counterfeiting encryption application thereof |
| CN113956873A (en) * | 2021-11-15 | 2022-01-21 | 广东工业大学 | Near-infrared broad-spectrum fluorescent powder with beta-gallium oxide structure and preparation method thereof |
| CN114540013A (en) * | 2022-02-19 | 2022-05-27 | 华南理工大学 | Lifting CaO Eu2+Method for luminous intensity and thermal stability of near-infrared fluorescent powder and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111187620A (en) * | 2020-01-19 | 2020-05-22 | 南京邮电大学 | Novel Zn2GeO4Base green long afterglow nano material and its preparation method |
| CN113046066A (en) * | 2021-03-29 | 2021-06-29 | 喀什大学 | Size-adjustable near-infrared luminescent long-afterglow nano material and preparation method thereof |
| CN113881427A (en) * | 2021-10-19 | 2022-01-04 | 喀什大学 | Preparation of long afterglow luminescent nano material with double emission and anti-counterfeiting encryption application thereof |
| CN113956873A (en) * | 2021-11-15 | 2022-01-21 | 广东工业大学 | Near-infrared broad-spectrum fluorescent powder with beta-gallium oxide structure and preparation method thereof |
| CN113956873B (en) * | 2021-11-15 | 2023-02-28 | 广东工业大学 | Near-infrared broad-spectrum fluorescent powder with beta-gallium oxide structure and preparation method thereof |
| CN114540013A (en) * | 2022-02-19 | 2022-05-27 | 华南理工大学 | Lifting CaO Eu2+Method for luminous intensity and thermal stability of near-infrared fluorescent powder and application thereof |
| CN114540013B (en) * | 2022-02-19 | 2023-10-20 | 华南理工大学 | Lifting CaO-Eu 2+ Method for preparing near infrared fluorescent powder with luminous intensity and thermal stability and application thereof |
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