CN110452696A - A kind of red long afterglow luminous material and preparation method thereof - Google Patents
A kind of red long afterglow luminous material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 46
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 46
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 23
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 23
- 229910002637 Pr6O11 Inorganic materials 0.000 claims abstract description 22
- 239000011812 mixed powder Substances 0.000 claims abstract description 18
- 238000001238 wet grinding Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 11
- 230000007547 defect Effects 0.000 abstract description 25
- 230000005284 excitation Effects 0.000 abstract description 14
- 230000003760 hair shine Effects 0.000 abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 4
- 150000002910 rare earth metals Chemical class 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- 235000019441 ethanol Nutrition 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 7
- ZTVIKZXZYLEVOL-DGKWVBSXSA-N 2-hydroxy-2-phenylacetic acid [(1R,5S)-8-methyl-8-azabicyclo[3.2.1]octan-3-yl] ester Chemical group C([C@H]1CC[C@@H](C2)N1C)C2OC(=O)C(O)C1=CC=CC=C1 ZTVIKZXZYLEVOL-DGKWVBSXSA-N 0.000 description 6
- 238000011049 filling Methods 0.000 description 6
- 238000004020 luminiscence type Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 230000002688 persistence Effects 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000003384 imaging method Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000000904 thermoluminescence Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000005084 Strontium aluminate Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001650 dmitryivanovite Inorganic materials 0.000 description 1
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical class OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 1
- 238000011503 in vivo imaging Methods 0.000 description 1
- 229910001707 krotite Inorganic materials 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- 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
- C09K11/7701—Chalogenides
- C09K11/7702—Chalogenides with zinc or cadmium
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Abstract
The invention discloses a kind of red long afterglow luminous materials and preparation method thereof, belong to rare earth luminescent material technical field.Red long afterglow luminous material of the invention, chemical formula Na2Ca1‑ xGe6O14:xPr3+, wherein 0.003≤x≤0.015；The present invention is by high-purity Na2CO3、CaCO3、GeO2And Pr6O11It carries out wet-milling and obtains mixed powder；Mixed powder is placed in temperature to be 1050-1150 DEG C, roast 6 ~ 8h in air atmosphere, is cooled to room temperature, grinds up to red long afterglow luminous material.Pr of the present invention3+Adulterate Na2CaGe6O14Long after glow luminous material realizes that red long-afterglow shines by adjusting rear-earth-doped concentration so as to adjust its defect state structure, removes at room temperature and reaches the red long-afterglow of 640 s after excitation light source and shine.
Description
Technical field
The present invention relates to a kind of red long afterglow luminous materials and preparation method thereof, belong to rare earth luminescent material technology neck
Domain.
Background technique
Long after glow luminous material is that one kind still is able to last for several seconds, several minutes or even several hours after removing excitation light source
Luminescent material.In general, the persistence of long after glow luminous material depends on the defect density and depth of material internal.In
Under room temperature, being suitable for long-persistence luminous depth of defect is 300-350K, and defect density is bigger, and the carrier of capture is got over
More, corresponding persistence is longer.
So far, more long after glow luminous material has been studied and has been widely used in emergency lighting, and safety is shown
Device, electronic console etc..Especially commercial blue long afterflow luminescent material is CaAl2O4:Eu2+,Nd3+, green Cheng Yu
Brightness luminescent material SrAl2O4:Eu2+,Dy3+, excellent afterglow property is concerned them.Although nowadays blue arrives yellow
The long after glow luminous material of wave band achieves great research achievement, especially in aluminate, silicate and gallic acid salt system
Efficient long after glow luminous material is developed, but they since penetration capacity is weaker, noise is relatively low, for current biology
Label and the application such as bio-imaging extremely unfavorable, with the needs of research and development, in in-vivo imaging marker and life
The research of the material of optical probe application in object imaging is increasingly valued by people.
Existing red emission long after glow luminous material is mainly the long after glow luminous material of oxysulfide series, is current
The best material of Characteristics of Long Luminosity in red long afterglow luminous material, material system are mainly Eu2+And Sm3+Activation
Y2O2S rare-earth oxide sulfate material.But synthetic material cost is too high, is possible to generate some pairs of air in synthesis process harmful
The substance of sulfur-bearing, simultaneously synthesizing material are also possible to toxic substances, and physical and chemical stability is poor, are unfavorable for the reality of material
Border application.Therefore synthesize nontoxic, the novel red long after glow luminous material of preparation condition simply is the current most important thing.
Summary of the invention
For red long-afterglow fluorescent powder the technical issues of, the present invention provides a kind of system of red long afterglow luminous material
Preparation Method, Pr of the present invention3+Adulterate Na2CaGe6O14Long after glow luminous material lacks by adjusting rear-earth-doped concentration so as to adjust it
State structure is fallen into, realizes that red long-afterglow shines, is removed at room temperature and is reached the red long-afterglow of 640 s after excitation light source and shine.
A kind of red long afterglow luminous material, chemical formula Na2Ca1-xGe6O14: xPr3+, wherein 0.003≤x≤
0.015。
A kind of preparation method of red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、CaCO3、GeO2And Pr6O11It carries out wet-milling and obtains mixed powder；
(2) mixed powder of step (1) is placed in temperature to be 1050-1150 DEG C, roast 6 ~ 8h in air atmosphere, is cooled to room
Temperature is ground up to red long afterglow luminous material.
Step (1) Na2CO3、CaCO3、GeO2、Pr6O11The molar ratio of middle Na, Ca, Ge and Pr are 2:(1-x): 6:x,
0.003≤x≤0.015。
In Na2CaGe6O14Pr is introduced in matrix3+As defect center and the centre of luminescence, by adjusting Pr3+The concentration of ion
So as to adjust the concentration of defect；Since to be suitable for room temperature long-persistence luminous for the depth of defect state, can be showed after filling at room temperature
Excellent red long-afterglow luminescent properties out.
Beneficial effects of the present invention:
(1) Pr of the invention3+Adulterate Na2CaGe6O14Long after glow luminous material removes it at room temperature there are a large amount of trap
The red long-afterglow for reaching 640 s after excitation light source shines；
(2) Pr of the invention3+Adulterate Na2CaGe6O14Long after glow luminous material can should in biomarker, bio-imaging etc. side
Face；
(3) simple process and low cost of the invention, obtained long after glow luminous material be it is single-phase, main phase structure belongs to six sides
Crystallographic system shows as red emission, and emission wavelength is in 614nm or so.
Detailed description of the invention
Fig. 1 is the Na that embodiment 4 is prepared2CaGe6O14: Pr3+The XRD spectrum of long after glow luminous material；
Fig. 2 is that embodiment 4 and comparative example prepare resulting Na2CaGe6O14: Pr3+Long after glow luminous material is in room temperature with ultraviolet
The Thermo-luminescence of (254 and 365nm) wavelength light write-in；
Fig. 3 is that embodiment 4 prepares resulting Na2CaGe6O14: Pr3+Long after glow luminous material is under the excitation of 250nm wavelength light
Emission spectrum removes the long-persistence luminous spectrum after excitation light source, and the transmitting under 254 and 365nm ultraviolet source irradiation
Radiograph and remove the afterglow picture after excitation light source；
Fig. 4 is that embodiment 4 prepares resulting Na2CaGe6O14: Pr3+Long after glow luminous material, in room temperature 254 and 365nm purple
After outer light source write-in, light source is removed, the persistence curve measured using long afterglow Time Measuring Instrument device；
Fig. 5 is that embodiment 4 prepares resulting Na2CaGe6O14: Pr3+Long after glow luminous material afterglow color is in CIE coordinate
Display figure on 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 red long afterglow luminous material of the present embodiment, chemical formula Na2Ca0.997Ge6O14: 0.003Pr3+；
A kind of preparation method of red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、CaCO3、GeO2And P6O11It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、CaCO3、
GeO2、Pr6O11The molar ratio of middle Na, Ca, Ge and Pr are 2:0.997:6:0.003；The organic solvent of wet-milling is that purity is AR's
Ethyl alcohol, Na2CO3、CaCO3、GeO2、Pr6O11Total volume and ethyl alcohol volume ratio be 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1100 DEG C, roast 8h in air atmosphere, is cooled to room temperature, grinding is
Obtain novel red long after glow luminous material；
In Na2CaGe6O14Pr is introduced in matrix3+As defect center and the centre of luminescence, by adjusting Pr3+The concentration of ion from
And adjust the concentration of defect；Since to be suitable for room temperature long-persistence luminous for the depth of defect state, can be shown after filling at room temperature
Excellent red long-afterglow luminescent properties；
The present embodiment red long afterglow luminous material removes the red long-afterglow hair for reaching about 410 s after excitation light source at room temperature
Light.
Embodiment 2: the red long afterglow luminous material of the present embodiment, chemical formula Na2Ca0.994Ge6O14: 0.006Tb3+；
A kind of preparation method of red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、CaCO3、GeO2And Pr6O11It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、CaCO3、
GeO2、Pr6O11The molar ratio of middle Na, Ca, Ge and Pr are 2:0.994:6:0.006；The organic solvent of wet-milling is that purity is AR's
Ethyl alcohol, Na2CO3、CaCO3、GeO2、Pr6O11Total volume and ethyl alcohol volume ratio be 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1150 DEG C, roast 7h in air atmosphere, is cooled to room temperature, grinding is
Obtain novel red long after glow luminous material；
In Na2CaGe6O14Pr is introduced in matrix3+As defect center and the centre of luminescence, by adjusting Pr3+The concentration of ion from
And adjust the concentration of defect；Since to be suitable for room temperature long-persistence luminous for the depth of defect state, can be shown after filling at room temperature
Excellent red long-afterglow luminescent properties；
The present embodiment red long afterglow luminous material reaches the red long-afterglow hair of about 468 s after room temperature removes excitation light source
Light.
Embodiment 3: the red long afterglow luminous material of the present embodiment, chemical formula Na2Ca0.991Ge6O14: 0.009Tb3+；
A kind of preparation method of red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、CaCO3、GeO2And Pr6O11It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、CaCO3、
GeO2、Pr6O11The molar ratio of middle Na, Ca, Ge and Pr are 2:0.991:6:0.009；The organic solvent of wet-milling is that purity is AR's
Ethyl alcohol, Na2CO3、CaCO3、GeO2、Pr6O11Total volume and ethyl alcohol volume ratio be 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1050 DEG C, roast 6.5h in air atmosphere, is cooled to room temperature, grinds
Up to novel red long after glow luminous material；
In Na2CaGe6O14Pr is introduced in matrix3+As defect center and the centre of luminescence, by adjusting Pr3+The concentration of ion from
And adjust the concentration of defect；Since to be suitable for room temperature long-persistence luminous for the depth of defect state, can be shown after filling at room temperature
Excellent red long-afterglow luminescent properties；
The red long-afterglow that the present embodiment red long afterglow luminous material reaches about 572s after room temperature removes excitation light source shines.
Embodiment 4: the red long afterglow luminous material of the present embodiment, chemical formula Na2Ca0.988Ge6O14: 0.012Tb3+；
A kind of preparation method of red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、CaCO3、GeO2And Pr6O11It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、CaCO3、
GeO2、Pr6O11The molar ratio of middle Na, Ca, Ge and Pr are 2:0.988:6:0.012；The organic solvent of wet-milling is that purity is AR's
Ethyl alcohol, Na2CO3、CaCO3、GeO2、Pr6O11Total volume and ethyl alcohol volume ratio be 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1080 DEG C, roast 6h in air atmosphere, is cooled to room temperature, grinding is
Obtain novel red long after glow luminous material；
In Na2CaGe6O14Pr is introduced in matrix3+As defect center and the centre of luminescence, by adjusting Pr3+The concentration of ion from
And adjust the concentration of defect；Since to be suitable for room temperature long-persistence luminous for the depth of defect state, can be shown after filling at room temperature
Excellent red long-afterglow luminescent properties；
The red long-afterglow that the present embodiment red long afterglow luminous material reaches about 640s after room temperature removes excitation light source shines；
The Na that the present embodiment is prepared2CaGe6O14: Pr3+The XRD spectrum of long after glow luminous material is as shown in Figure 1, with PDF card
Piece comparison diffraction maximum matches good no discovery miscellaneous peak with PDF card, illustrates the novel red long-persistence luminous material of the present embodiment
Material is single-phase；
The present embodiment Na2CaGe6O14:Pr3+Long after glow luminous material is in room temperature with 254 and 365 nm wavelength light irradiation 10 minutes
The Thermo-luminescence of U-V writing is as shown in Fig. 2, as can be seen from Figure 2, Pr3+The concentration of ion changes changing with sintering time simultaneously
Change can effectively adjust defect density, be conducive to adjust the red long-afterglow luminous time；
The present embodiment Na2CaGe6O14: Pr3+Long after glow luminous material 250 nm wavelength lights excitation under emission spectrum, remove
Long-persistence luminous spectrum after excitation light source, and the afterglow picture after the write-in of 254 and 365nm ultraviolet source, from Fig. 3
It is found that the position at emission spectrum peak is identical as the position of long-after-glow light spectral peak, it is all located at 614nm or so, shows as red emission；
The present embodiment prepares resulting Na2CaGe6O14: Pr3+Long after glow luminous material, in room temperature 254 and 365nm ultraviolet light
Source is written after ten minutes, and long-persistence luminous attenuation curve after removing light source is novel as shown in figure 4, as can be seen from Figure 4
Na2CaGe6O14: Pr3+The afterglow color of long after glow luminous material is red, and persistence is up to 640s；
The present embodiment Na2CaGe6O14: Pr3+Long after glow luminous material, display figure of the afterglow color in CIE coordinate diagram is such as
Shown in Fig. 5, it is red functional to illustrate that its afterglow is shown as.
Embodiment 5: the red long afterglow luminous material of the present embodiment, chemical formula Na2Ca0.985Ge6O14: 0.015Tb3+；
A kind of preparation method of red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、CaCO3、GeO2And Pr6O11It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、CaCO3、
GeO2、Pr6O11The molar ratio of middle Na, Ca, Ge and Pr are 2:0.985:6:0.015；The organic solvent of wet-milling is that purity is AR's
Ethyl alcohol, Na2CO3、CaCO3、GeO2、Pr6O11Total volume and ethyl alcohol volume ratio be 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1120 DEG C, roast 6h in air atmosphere, is cooled to room temperature, grinding is
Obtain novel red long after glow luminous material；
In Na2CaGe6O14Pr is introduced in matrix3+As defect center and the centre of luminescence, by adjusting Pr3+The concentration of ion from
And adjust the concentration of defect；Since to be suitable for room temperature long-persistence luminous for the depth of defect state, can be shown after filling at room temperature
Excellent red long-afterglow luminescent properties；
The present embodiment red long afterglow luminous material reaches the red long-afterglow hair of about 445 s after room temperature removes excitation light source
Light.
Comparative example: the red long afterglow luminous material of this comparative example, chemical formula Na2Ca0.988Ge6O14: 0.012Pr3+；
The preparation method of red long afterglow luminous material, the specific steps are as follows:
(1) by high-purity Na2CO3、CaCO3、GeO2And Pr6O11It carries out wet-milling and obtains mixed powder；Wherein Na2CO3、CaCO3、
GeO2、Pr6O11The molar ratio of middle Na, Ca, Ge and Pr are 2:0.988:6:0.012；The organic solvent of wet-milling is that purity is AR's
Ethyl alcohol, Na2CO3、CaCO3、GeO2、Pr6O11Total volume and ethyl alcohol volume ratio be 1:1；
(2) mixed powder of step (1) is placed in temperature to be 1050 and 1150 DEG C, roast 6h in air atmosphere, is cooled to room temperature,
It grinds up to novel red long after glow luminous material；
The Na of comparative example2CaGe6O14: Pr3+The sample that long after glow luminous material is sintered at 1050 and 1150 DEG C respectively is in room temperature item
10 minutes Thermo-luminescences are written as shown in Fig. 2, as can be seen from Figure 2 with 254 and 365 nm wavelength lights under part, not only sintering time
Will affect the generation of fault in material state, the height of sintering temperature can also seriously affect the generation of defect state, while adjust rare earth from
Sub- concentration can adjust the concentration of defect, and therefore, the doping concentration of suitable sintering temperature and rare earth ion is conducive to reach long
Time long-persistence luminous purpose.
Claims (3)
1. a kind of red long afterglow luminous material, it is characterised in that: chemical formula Na2Ca1-xGe6O14: xPr3+, wherein 0.003
≤x≤0.015。
2. a kind of preparation method of red long afterglow luminous material, which is characterized in that specific step is as follows:
(1) by high-purity Na2CO3、CaCO3、GeO2And Pr6O11It carries out wet-milling and obtains mixed powder；
(2) mixed powder of step (1) is placed in temperature to be 1050-1150 DEG C, roast 6 ~ 8h in air atmosphere, is cooled to room
Temperature is ground up to red long afterglow luminous material.
3. the preparation method of red long afterglow luminous material according to claim 1, it is characterised in that: step (1) Na2CO3、
CaCO3、GeO2、Pr6O11The molar ratio of middle Na, Ca, Ge and Pr are 2:(1-x): 6:x, 0.003≤x≤0.015.
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| CN114184299A (en) * | 2021-12-11 | 2022-03-15 | 中国科学院长春光学精密机械与物理研究所 | Rare earth element doping-based thermoluminescence temperature measurement method |
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| TANG XUE: "A thermal-sensitizing and thermochromic phosphor", 《JOURNAL OF MATERIALS CHEMISTRY C》 * |
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| CN114184299A (en) * | 2021-12-11 | 2022-03-15 | 中国科学院长春光学精密机械与物理研究所 | Rare earth element doping-based thermoluminescence temperature measurement method |
| CN114184299B (en) * | 2021-12-11 | 2023-03-07 | 中国科学院长春光学精密机械与物理研究所 | Rare earth element doping-based thermoluminescence temperature measurement method |
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Application publication date: 20191115 |