CN109575920A - A kind of low temperature red long afterglow luminous material and preparation method thereof - Google Patents
A kind of low temperature red long afterglow luminous material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 76
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910002637 Pr6O11 Inorganic materials 0.000 claims abstract description 38
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 38
- 239000011812 mixed powder Substances 0.000 claims abstract description 22
- 238000001238 wet grinding Methods 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 12
- 230000007547 defect Effects 0.000 abstract description 31
- 229910003378 NaNbO3 Inorganic materials 0.000 abstract description 22
- 230000005284 excitation Effects 0.000 abstract description 11
- 230000003760 hair shine Effects 0.000 abstract description 11
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
- 150000002910 rare earth metals Chemical class 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 27
- 239000000843 powder Substances 0.000 description 19
- 235000019441 ethanol Nutrition 0.000 description 16
- 238000001228 spectrum Methods 0.000 description 11
- MUPJWXCPTRQOKY-UHFFFAOYSA-N sodium;niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Na+].[Nb+5] MUPJWXCPTRQOKY-UHFFFAOYSA-N 0.000 description 10
- 238000004020 luminiscence type Methods 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 8
- 239000003960 organic solvent Substances 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 7
- 238000000904 thermoluminescence Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- 238000003384 imaging method Methods 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 239000006184 cosolvent Substances 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical class OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 238000011503 in vivo imaging Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000002688 persistence Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- KRQUFUKTQHISJB-YYADALCUSA-N 2-[(E)-N-[2-(4-chlorophenoxy)propoxy]-C-propylcarbonimidoyl]-3-hydroxy-5-(thian-3-yl)cyclohex-2-en-1-one Chemical compound CCC\C(=N/OCC(C)OC1=CC=C(Cl)C=C1)C1=C(O)CC(CC1=O)C1CCCSC1 KRQUFUKTQHISJB-YYADALCUSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7767—Chalcogenides
- C09K11/7769—Oxides
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- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of low temperature red long afterglow luminous materials and preparation method thereof, belong to rare earth luminescent material technical field.Low temperature red long afterglow luminous material of the invention, chemical formula Na1‑xNbO3:xPr3+, wherein 0.004≤x≤0.016；The present invention is by high-purity Na2CO3、Nb2O5、Pr6O11And H3BO3It carries out wet-milling and obtains mixed powder；Mixed powder is placed in temperature to be 1100 ~ 1200 DEG C, roast 6 ~ 8h in air atmosphere, is cooled to room temperature, grinds up to low temperature red long afterglow luminous material.Pr of the present invention3+Adulterate NaNbO3Long after glow luminous material passes through rear-earth-doped and introducing H3BO3It adjusts its defect state structure, realizes that low temperature red long-afterglow shines, removed at a temperature of 200K and reach 16 hours red long-afterglows after excitation light source and shine.
Description
Technical field
The present invention relates to a kind of low temperature red long afterglow luminous materials and preparation method thereof, belong to rare earth luminescent material technology
Field.
Background technique
Traditional long after glow luminous material is one kind last for several seconds after removing excitation light source, several minutes or even a few hours
Luminescent material.In general, the carrier that it depends on trap level to be captured, can occur, at room temperature because thermal energy is enough to activate
The carrier that trap is captured so that defect center release carrier to be combined with the centre of luminescence, thus stop excite
Lasting shine is generated after source.
Currently, long after glow luminous material has caused extensive research interest, and it is widely used in emergency lighting, safety is shown
Device, electronic console and in-vivo imaging etc..Although short wavelength's long after glow luminous material achieves significant achievement, long wave now
The research and development of long long after glow luminous material is for the optical probe application in the marker and bio-imaging in in-vivo imaging
Demand it is growing.Although also, developing efficient long-persistence luminous material in aluminate, silicate and gallic acid salt system
Material, but the application of these materials is but only limitted to room temperature environment.
In fact, higher temperature can accelerate the release of carrier in trap, and when environment temperature is lower than room temperature, due to
Activation energy is insufficient, and carrier cannot discharge, this can all reduce the long afterglow performance of fluorescent powder.In recent years, it is designed in defect sturcture
Auxiliary under, develop gallate, silicate, the high temperature long lad phosphor of aluminate is that multidimensional is rewritable or advanced display
The bio-imaging and optical storage of data of technology provide potential application.However, up to the present there are no red about low temperature
The research of the fluorescent powder of color long afterglow reports which has limited application of the long lad phosphor in biomarker and imaging.
Summary of the invention
For low temperature red long-afterglow fluorescent powder the technical issues of, the present invention provides a kind of low temperature red long-afterglow and shines
The preparation method of material, Pr of the present invention3+Adulterate NaNbO3Long after glow luminous material passes through rear-earth-doped and introducing H3BO3Adjust it
Defect state structure realizes that low temperature red long-afterglow shines, and removes at a temperature of 200K and reaches 16 hours red after excitation light source
It is long-persistence luminous.
A kind of low temperature red long afterglow luminous material, chemical formula Na1-xNbO3: xPr3+, wherein 0.004≤x≤
0.016。
A kind of preparation method of low temperature red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、Nb2O5、Pr6O11And H3BO3It carries out wet-milling and obtains mixed powder；
(2) mixed powder of step (1) is placed in temperature to be 1100 ~ 1200 DEG C, roast 6 ~ 8h in air atmosphere, is cooled to room
Temperature is ground up to low temperature red long afterglow luminous material；
Step (1) Na2CO3、Nb2O5、Pr6O11The molar ratio of middle Na, Nb and Pr be (1-x): 1:x, 0.004≤x≤
0.016；
Step (1) H3BO3Additional amount be Na2CO3、Nb2O5And Pr6O11The 3 ~ 5% of gross mass.
In NaNbO3Pr is introduced in matrix3+As defect center and the centre of luminescence, H3BO3Addition improve fluorescent powder knot
Crystalline substance, while fluorescent powder being made to generate a large amount of, new shallower defect state structure；It, can only be low since defect states are shallower
It is filled under temperature, and can show its excellent afterglow property at low temperature.
Beneficial effects of the present invention:
(1) Pr of the invention3+Adulterate NaNbO3Long after glow luminous material removes it at 200K sharp there are a large amount of shallow trap
Reach 16 hours red long-afterglows after light emitting source to shine；
(2) Pr of the invention3+Adulterate NaNbO3Long after glow luminous material can should be in anti-fake, biomedical etc.；
(3) simple process and low cost of present invention side, obtained long after glow luminous material be it is single-phase, main phase structure belongs to just
Hand over crystallographic system, show as red-emitting luminescent in 612nm or so, and it is long in the red that 130K ~ 270K all has the long period more than
Brightness shines.
Detailed description of the invention
Fig. 1 is the NaNbO that embodiment 4 is prepared3: Pr3+The XRD spectrum of long after glow luminous material；
Fig. 2 is that embodiment 4 and comparative example prepare resulting NaNbO3: Pr3+Long after glow luminous material is in 273K with 254nm wave
The Thermo-luminescence of long light write-in；
Fig. 3 is that embodiment 4 prepares resulting NaNbO3: Pr3+Room temperature of the long after glow luminous material under the excitation of 310nm wavelength light
With emission spectrum when 200K, and after the write-in of 254 and 365nm ultraviolet source twilight sunset spectrum at room temperature and when 200K more than
Aura spectrum；
Fig. 4 is that embodiment 4 prepares resulting NaNbO3: Pr3+Long after glow luminous material is in 77K with 254 and 365nm wavelength light
The Thermo-luminescence and temperature corresponding diagram of write-in；
Fig. 5 is that embodiment 4 prepares resulting NaNbO3: Pr3+Long after glow luminous material, in 77K 254 and 365nm ultraviolet source
After write-in, light source is removed, the spectrum change figure for being warming up to 200K using temperature control device and keeping the temperature；
Fig. 6 is that embodiment 4 prepares resulting NaNbO3: Pr3+Long after glow luminous material, afterglow color is in CIE coordinate diagram
Display figure.
Specific embodiment
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
Embodiment 1: the low temperature red long afterglow luminous material of the present embodiment, chemical formula Na0.996NbO3: 0.004Pr3+；
A kind of preparation method of low temperature red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、Nb2O5、Pr6O11And H3BO3It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、Nb2O5、
Pr6O11The molar ratio of middle Na, Nb and Pr are 0.996:1:0.004；H3BO3Additional amount be Na2CO3、Nb2O5And Pr6O11Total matter
The 3% of amount；The organic solvent of wet-milling is the ethyl alcohol that purity is 98%, Na2CO3、Nb2O5、Pr6O11And H3BO3Total volume and ethyl alcohol
The ratio of volume is 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1200 DEG C, roast 8h in air atmosphere, is cooled to room temperature, grinding is
Obtain low temperature red long afterglow luminous material；
In NaNbO3Pr is introduced in matrix3+As defect center and the centre of luminescence, H3BO3Addition improve fluorescent powder crystallization
Property, while fluorescent powder being made to generate a large amount of, new shallower defect state structure；It, can only be in low temperature since defect states are shallower
Under be filled, and can show its excellent afterglow property at low temperature；
The present embodiment low temperature red long afterglow luminous material reaches after 200 K of temperature removes excitation light source more than the red length of 10h
Brightness shines.
Embodiment 2: the low temperature red long afterglow luminous material of the present embodiment, chemical formula Na0.994NbO3: 0.006Pr3+；
A kind of preparation method of low temperature red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、Nb2O5、Pr6O11And H3BO3It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、Nb2O5、
Pr6O11The molar ratio of middle Na, Nb and Pr are 0.994:1:0.006；H3BO3Additional amount be Na2CO3、Nb2O5And Pr6O11Total matter
The 3.5% of amount；The organic solvent of wet-milling is the ethyl alcohol that purity is 98%, Na2CO3、Nb2O5、Pr6O11And H3BO3Total volume and second
The ratio of alcohol volume is 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1180 DEG C, roast 7.8h in air atmosphere, is cooled to room temperature, grinds
Up to low temperature red long afterglow luminous material；
In NaNbO3Pr is introduced in matrix3+As defect center and the centre of luminescence, H3BO3Addition improve fluorescent powder crystallization
Property, while fluorescent powder being made to generate a large amount of, new shallower defect state structure；It, can only be in low temperature since defect states are shallower
Under be filled, and can show its excellent afterglow property at low temperature；
The present embodiment low temperature red long afterglow luminous material reaches the red long-afterglow of 12h after temperature 200K removes excitation light source
It shines.
Embodiment 3: the low temperature red long afterglow luminous material of the present embodiment, chemical formula Na0.992NbO3: 0.008Pr3+；
A kind of preparation method of low temperature red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、Nb2O5、Pr6O11And H3BO3It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、Nb2O5、
Pr6O11The molar ratio of middle Na, Nb and Pr are 0.992:1:0.008；H3BO3Additional amount be Na2CO3、Nb2O5And Pr6O11Total matter
The 3.8% of amount；The organic solvent of wet-milling is the ethyl alcohol that purity is 98%, Na2CO3、Nb2O5、Pr6O11And H3BO3Total volume and second
The ratio of alcohol volume is 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1150 DEG C, roast 7.5h in air atmosphere, is cooled to room temperature, grinds
Up to low temperature red long afterglow luminous material；
In NaNbO3Pr is introduced in matrix3+As defect center and the centre of luminescence, H3BO3Addition improve fluorescent powder crystallization
Property, while fluorescent powder being made to generate a large amount of, new shallower defect state structure；It, can only be in low temperature since defect states are shallower
Under be filled, and can show its excellent afterglow property at low temperature；
The present embodiment low temperature red long afterglow luminous material reaches after 200 K of temperature removes excitation light source more than the red length of 14h
Brightness shines.
Embodiment 4: the low temperature red long afterglow luminous material of the present embodiment, chemical formula Na0.990NbO3: 0.010Pr3+；
A kind of preparation method of low temperature red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、Nb2O5、Pr6O11And H3BO3It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、Nb2O5、
Pr6O11The molar ratio of middle Na, Nb and Pr are 0.990:1:0.010；H3BO3Additional amount be Na2CO3、Nb2O5And Pr6O11Total matter
The 3% of amount；The organic solvent of wet-milling is the ethyl alcohol that purity is 98%, Na2CO3、Nb2O5、Pr6O11And H3BO3Total volume and ethyl alcohol
The ratio of volume is 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1200 DEG C, roast 8h in air atmosphere, is cooled to room temperature, grinding is
Obtain low temperature red long afterglow luminous material；
In NaNbO3Pr is introduced in matrix3+As defect center and the centre of luminescence, H3BO3Addition improve fluorescent powder crystallization
Property, while fluorescent powder being made to generate a large amount of, new shallower defect state structure；It, can only be in low temperature since defect states are shallower
Under be filled, and can show its excellent afterglow property at low temperature；
The present embodiment low temperature red long afterglow luminous material reaches after 200 K of temperature removes excitation light source more than the red length of 16h
Brightness shines；
The NaNbO that the present embodiment is prepared3: Pr3+The XRD spectrum of long after glow luminous material is as shown in Figure 1, with PDF card pair
Than no discovery miscellaneous peak, illustrate that the low temperature red long afterglow luminous material of the present embodiment is single-phase；
The present embodiment NaNbO3: Pr3+Long after glow luminous material in 273K with 254nm wavelength light be written Thermo-luminescence such as
Shown in Fig. 2, as can be seen from Figure 2, cosolvent boric acid, which is added, can effectively adjust its defect state structure, be advantageously implemented more than low temperature length
The purpose of brightness continuous illumination；
The present embodiment NaNbO3: Pr3+Transmitting of the long after glow luminous material in the room temperature and 200K under 310nm wavelength light excites
Spectrum and twilight sunset spectrum such as Fig. 3 institute in the twilight sunset spectrum and 200K after 254 and 365nm ultraviolet source is written at room temperature
Show, as can be seen from Figure 3, Emission Spectrum Peals are identical as twilight sunset spectrum peak value to be all located at 612nm or so, shows as feux rouges；
The present embodiment prepares resulting NaNbO3: Pr3+Long after glow luminous material is written in 77K with 254 and 365nm wavelength light
Thermo-luminescence and temperature corresponding diagram as shown in figure 4, as can be seen from Figure 4, as the temperature rises, the carrier in defect is opened
Begin to discharge, and the brightness of light reaches maximum value at 250K, then begins to reduce；Thermo-luminescence can be synthesized to 4 heat
Photopeak is released, peak value is respectively in 130K, 200K, 230K, 250K；
The present embodiment prepares resulting NaNbO3: Pr3+Long after glow luminous material is written in 77K 254 and 365nm ultraviolet source
The spectrum change figure connection highest point obtained persistence for removing light source afterwards and being warming up to 200K using temperature control device and keeping the temperature
For spectrum as shown in figure 5, as can be seen from Figure 5, sample is red in the twilight sunset of 200K, persistence is up to 16 hours；
The present embodiment NaNbO3: Pr3+Long after glow luminous material, the display figure such as Fig. 6 of afterglow color in CIE coordinate diagram
It is shown, it is red functional to illustrate that its afterglow is shown as.
Embodiment 5: the low temperature red long afterglow luminous material of the present embodiment, chemical formula Na0.988NbO3: 0.012Pr3+；
A kind of preparation method of low temperature red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、Nb2O5、Pr6O11And H3BO3It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、Nb2O5、
Pr6O11The molar ratio of middle Na, Nb and Pr are 0.988:1:0.012；H3BO3Additional amount be Na2CO3、Nb2O5And Pr6O11Total matter
The 4.0% of amount；The organic solvent of wet-milling is the ethyl alcohol that purity is 98%, Na2CO3、Nb2O5、Pr6O11And H3BO3Total volume and second
The ratio of alcohol volume is 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1130 DEG C, roast 7.0h in air atmosphere, is cooled to room temperature, grinds
Up to low temperature red long afterglow luminous material；
In NaNbO3Pr is introduced in matrix3+As defect center and the centre of luminescence, H3BO3Addition improve fluorescent powder crystallization
Property, while fluorescent powder being made to generate a large amount of, new shallower defect state structure；It, can only be in low temperature since defect states are shallower
Under be filled, and can show its excellent afterglow property at low temperature；
The present embodiment low temperature red long afterglow luminous material reaches the red long-afterglow of 14h after temperature 200K removes excitation light source
It shines.
Embodiment 6: the low temperature red long afterglow luminous material of the present embodiment, chemical formula Na0.986NbO3: 0.014Pr3+；
A kind of preparation method of low temperature red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、Nb2O5、Pr6O11And H3BO3It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、Nb2O5、
Pr6O11The molar ratio of middle Na, Nb and Pr are 0.986:1:0.014；H3BO3Additional amount be Na2CO3、Nb2O5And Pr6O11Total matter
The 5.0% of amount；The organic solvent of wet-milling is the ethyl alcohol that purity is 98%, Na2CO3、Nb2O5、Pr6O11And H3BO3Total volume and second
The ratio of alcohol volume is 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1200 DEG C, roast 6.0h in air atmosphere, is cooled to room temperature, grinds
Up to low temperature red long afterglow luminous material；
In NaNbO3Pr is introduced in matrix3+As defect center and the centre of luminescence, H3BO3Addition improve fluorescent powder crystallization
Property, while fluorescent powder being made to generate a large amount of, new shallower defect state structure；It, can only be in low temperature since defect states are shallower
Under be filled, and can show its excellent afterglow property at low temperature；
The present embodiment low temperature red long afterglow luminous material reaches the red long-afterglow of 12h after temperature 200K removes excitation light source
It shines.
Embodiment 7: the low temperature red long afterglow luminous material of the present embodiment, chemical formula Na0.984NbO3: 0.016Pr3+；
A kind of preparation method of low temperature red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、Nb2O5、Pr6O11And H3BO3It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、Nb2O5、
Pr6O11The molar ratio of middle Na, Nb and Pr are 0.984:1:0.016；H3BO3Additional amount be Na2CO3、Nb2O5And Pr6O11Total matter
The 4.5% of amount；The organic solvent of wet-milling is the ethyl alcohol that purity is 98%, Na2CO3、Nb2O5、Pr6O11And H3BO3Total volume and second
The ratio of alcohol volume is 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1150 DEG C, roast 7.0h in air atmosphere, is cooled to room temperature, grinds
Up to low temperature red long afterglow luminous material；
In NaNbO3Pr is introduced in matrix3+As defect center and the centre of luminescence, H3BO3Addition improve fluorescent powder crystallization
Property, while fluorescent powder being made to generate a large amount of, new shallower defect state structure；It, can only be in low temperature since defect states are shallower
Under be filled, and can show its excellent afterglow property at low temperature；
The present embodiment low temperature red long afterglow luminous material reaches the red long-afterglow of 11h after temperature 200K removes excitation light source
It shines.
Comparative example: the low temperature red long afterglow luminous material of this comparative example, chemical formula Na0.990NbO3: 0.010Pr3+；
The preparation method of low temperature red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、Nb2O5And Pr6O11It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、Nb2O5、Pr6O11In
The molar ratio of Na, Nb and Pr are 0.990:1:0.010；The organic solvent of wet-milling is the ethyl alcohol that purity is 98%, Na2CO3、Nb2O5、
Pr6O11And H3BO3Total volume and ethyl alcohol volume ratio be 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1200 DEG C, roast 8h in air atmosphere, is cooled to room temperature, grinding is
Obtain low temperature red long afterglow luminous material；
The NaNbO of comparative example3: Pr3+Long after glow luminous material in 273K with 254nm wavelength light be written Thermo-luminescence such as
Shown in Fig. 2, as can be seen from Figure 2, cosolvent boric acid, which is added, can effectively adjust its defect state structure, be conducive to reach more than low temperature length
The luminous purpose of brightness.
Claims (4)
1. a kind of low temperature red long afterglow luminous material, it is characterised in that: chemical formula Na1-xNbO3: xPr3+, wherein 0.004
≤x≤0.016。
2. a kind of preparation method of low temperature red long afterglow luminous material, which is characterized in that specific step is as follows:
(1) by high-purity Na2CO3、Nb2O5、Pr6O11And H3BO3It carries out wet-milling and obtains mixed powder；
(2) mixed powder of step (1) is placed in temperature to be 1100 ~ 1200 DEG C, roast 6 ~ 8h in air atmosphere, is cooled to room
Temperature is ground up to low temperature red long afterglow luminous material.
3. the preparation method of low temperature red long afterglow luminous material according to claim 1, it is characterised in that: step (1)
Na2CO3、Nb2O5、Pr6O11The molar ratio of middle Na, Nb and Pr are (1-x): 1:x, 0.004≤x≤0.016.
4. the preparation method of low temperature red long afterglow luminous material according to claim 1, it is characterised in that: step (1)
H3BO3Additional amount be Na2CO3、Nb2O5And Pr6O11The 3 ~ 5% of gross mass.
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| CN113355094A (en) * | 2021-05-17 | 2021-09-07 | 武汉大学 | Heterostructure material capable of realizing repetitive stress luminescence and preparation method thereof |
| CN114907847A (en) * | 2022-05-18 | 2022-08-16 | 五邑大学 | Fluorescent temperature measuring material and preparation method and application thereof |
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| CN109468132A (en) * | 2018-10-10 | 2019-03-15 | 阜阳师范学院 | A kind of rear-earth-doped composite red color stress light emitting material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113355094A (en) * | 2021-05-17 | 2021-09-07 | 武汉大学 | Heterostructure material capable of realizing repetitive stress luminescence and preparation method thereof |
| CN114907847A (en) * | 2022-05-18 | 2022-08-16 | 五邑大学 | Fluorescent temperature measuring material and preparation method and application thereof |
| CN114907847B (en) * | 2022-05-18 | 2023-01-03 | 五邑大学 | Fluorescent temperature measuring material and preparation method and application thereof |
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Application publication date: 20190405 |