CN106811197B - A kind of fluosilicic acid alkali up-conversion luminescence ceramic material and preparation method thereof - Google Patents
A kind of fluosilicic acid alkali up-conversion luminescence ceramic material and preparation method thereof Download PDFInfo
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Abstract
A kind of fluosilicic acid alkali up-conversion luminescence ceramic material of the present invention and preparation method thereof, chemical general formula Ca10‑ 10xEr10xYb10ySi3O15F2, wherein x is Er3+The stoichiometry score of doping, y are ytterbium ion Yb3+The stoichiometry score of doping, 0.001≤x+y < 0.2.Up-conversion luminescent material lattice structure produced by the present invention is stable, particle size is uniform, stable luminescent property, in the case where 976 nanometers of infrared lasers excite, occurs emitting red light peak, luminance purity height, upper high conversion efficiency near 670 nano wave lengths；Since matrix structure is stable, rare earth doped concentration is high, is conducive to enhance luminous efficiency and realizes the excitation under high power；The present invention mixes the compound containing element needed for synthesizing luminescent material when preparing in proportion, is prepared using high temperature solid-state method, simple process, and raw material sources are abundant, cheap；And it is discharged in technical process without waste water and gas, and nontoxic, it is environmentally friendly, it is conducive to further genralrlization and uses.
Description
Technical field
The present invention relates to solid fluorescent material field, especially a kind of fluosilicic acid alkali up-conversion luminescence ceramic material and its
Preparation method.
Background technique
In recent years, up-conversion luminescent material causes the extensive concern of people.In embedded photoluminescent material, two or more are absorbed
The luminescent material that the transmitting of a high-energy photon is generated after a photon compared with low energy is defined as up-conversion luminescent material (referred to as
UCPs).The upper conversion phenomena essence of this material is anti-Stokes effect, that is, the energy radiated is greater than absorbed energy,
When its principle of luminosity is that light source is irradiated to material surface, particle can absorb two or more low-lying excitation photon, electricity
Then son gives off high-energy photon from ground state transition to upper state outward, the high-energy photon frequency given off, which is greater than, absorbs light
Frequency.Up-conversion luminescent material can be effectively reduced photo ionization and host material caused to fail, and not need stringent phase
Bit pairing, and output wavelength has certain tunability, it is considered to be production solid-state laser, light emitting diode and fluorescence mark
The optimal materials such as note.
Up-conversion luminescent material is mainly to realize that it shines with rare earth doped element.Due to rare earth outer shell electronics pair
The shielding action of 4f electronics leads to that there is the luminous of metastable rare earth element to be mainly based upon the interelectric transition of 4f, people
The sightless infrared light of eye is converted into the visible light that people are observed that.This feature of people according to upper conversion, is answered
It uses on infrared detector, effectively raises sensitivity.In addition, up-conversion luminescent material be also widely used for laser technology,
The fields such as optical fiber communication technology, optical information storage and fibre amplifier, have larger in daily life and military project
Application potential.
It, can be with currently, up-conversion luminescent material is concentrated mainly on the systems such as rare-earth-doped fluoride, sulfide, halide
The transmitting of red, green, blue and white light is realized, but in practical applications, since the stability of these host materials is inadequate, preparation work
Skill is complicated, to up-conversion luminescent material use and popularization and application are brought greater impact.
Summary of the invention
In view of the above-mentioned problems of the prior art, the purpose of the present invention is to provide a kind of lattices and property to stablize, property
The excellent fluosilicic acid alkali up-conversion luminescence ceramic material of energy, another object of the present invention is to provide preparation processes simply easily to grasp
The preparation method of the up-conversion luminescence ceramic material of work.
To achieve the above object, the technical solution adopted by the present invention is that: a kind of fluosilicic acid alkali up-conversion luminescence ceramics material
Material, chemical formula Ca10-10xEr10xYb10ySi3O15F2, wherein x is Er3+The stoichiometry score of doping, y are ytterbium ion Yb3+It mixes
Miscellaneous stoichiometry score, 0.001≤x+y < 0.2.
The present invention also provides a kind of preparation methods of fluosilicic acid alkali up-conversion luminescence ceramic material, using high temperature solid-state
Method, comprising the following steps:
(1) according to Ca10-10xEr10xYb10ySi3O15F2The stoichiometric ratio of middle each element, wherein 0.001≤x+y < 0.2 point
Also known as take containing calcium ion Ca2+Compound, contain silicon ion Si4+Compound, contain erbium ion Er3+Compound, contain
Ytterbium ion Yb3+Compound, contain fluorine ion F-Compound as raw material, and calcium ion Ca will be contained2+Compound, contain
Silicon ion Si4+Compound, contain erbium ion Er3+Compound, contain ytterbium ion Yb3+Compound mix and grind uniformly,
Obtain mixture；
(2) contain calcium ion Ca for what step (1) obtained2+Compound, contain silicon ion Si4+Compound, contain erbium
Ion Er3+Compound, contain ytterbium ion Yb3+Mixture be sintered in air atmosphere, sintering temperature be 750~950
DEG C, sintering time is 3~10 hours, and after natural cooling, ground and mixed is uniform；
(3) powder mixture for obtaining step (2) with contain fluorine ion F-Compound mix and grind uniformly, compacting
At potsherd, pressing pressure is 10MPa~15MPa, is calcined in air atmosphere, and calcination temperature is 900~1200 DEG C, when calcining
Between be 3~15 hours, natural cooling, obtain calcium fluosilicate ceramics.
As a preferred embodiment of above-mentioned preparation method, the sintering temperature of step (2) is 800~900 DEG C, sintering time
It is 4~10 hours.
As a preferred embodiment of above-mentioned preparation method, the calcination temperature of step (3) is 950~1100 DEG C, when calcining
Between be 5~10 hours.
In above-mentioned preparation method: the calcium fluosilicate ceramics that step (3) obtains being crushed and fluorine uniformly can be obtained in ground and mixed
Calcium silicate ceramic powder body.
In preparation method of the present invention, described contains calcium ion Ca2+Compound be calcium carbonate, calcium nitrate, calcium hydroxide,
One kind of calcium oxalate, calcium oxide；It is described to contain silicon ion Si4+Compound be one of silica or silicic acid；Described
Contain fluorine ion F-Compound be calcirm-fluoride；Described contains erbium ion Er3+Compound be erbium oxide；Described contains ytterbium
Ion Yb3+Compound be ytterbium oxide.
It is described to contain calcium ion Ca as the preferred embodiment of preparation method2+Compound mixed by two kinds of compounds,
One of which is calcirm-fluoride, and the calcium that calcirm-fluoride provides accounts for 10vol%~40vol% of total calcium content, and another kind is calcium carbonate, nitric acid
One of calcium, calcium hydroxide, calcium oxalate, calcium oxide.
Compared with prior art, the invention has the following beneficial effects:
(1) fluosilicate up-conversion luminescent material lattice structure of the invention is stable, phonon energy is low, is conducive in raising
Convert luminous efficiency and the excitation stability under high-power；Due to Ca10Si3O15F2Better heat stability, it is easy to accomplish dilute
The efficient doping of native ion, upper high conversion efficiency, up-conversion luminescent material particle size obtained is uniform, stable luminescent property,
Compared with other oxysulfides, halide up-conversion luminescent material, there is innovative and repeatability preferably；
(2) in the case where 976 nanometers of infrared lasers excite, the emitting red light peak near 670 nano wave lengths can be launched, shone
Purity is high；Since matrix structure is stable, the rare earth concentration height of doping, the excitation being advantageously implemented under high power and the luminous effect of enhancing
Rate can be used as red upconverting fluorescent material to apply.It applies it on infrared detector, can effectively improve sensitive
Degree, in addition it can be widely used in the necks such as laser technology, optical fiber communication technology, optical information storage and fibre amplifier
There is biggish application potential in domain in daily life and military project；
(3) preparation method of up-conversion luminescent material of the present invention is relative to other oxyfluorides, oxysulfide, halide
For, simple process, raw material sources are abundant, cheap；And it is discharged in technical process without waste water and gas, and nontoxic, it is right
It is environmental-friendly, it is conducive to further genralrlization and uses.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention 1 prepares sample Ca9.45Er0.05Yb0.5Si3O15F2X-ray powder diffraction pattern；
Fig. 2 is that the embodiment of the present invention 1 prepares sample Ca9.45Er0.05Yb0.5Si3O15F2Scanning electron microscope diagram；
Fig. 3 is that the embodiment of the present invention 1 prepares sample Ca9.45Er0.05Yb0.5Si3O15F2In 976 nanometers, excitation energy intensity
For the up-conversion luminescence spectrogram obtained under 1.5 watts infrared ray excited；
Fig. 4 is that the embodiment of the present invention 4 prepares sample Ca9.3Er0.2Yb0.5Si3O15F2Scanning electron microscope diagram；
Fig. 5 is that the embodiment of the present invention 4 prepares sample Ca9.3Er0.2Yb0.5Si3O15F2It is in 976 nanometers, excitation energy intensity
The up-conversion luminescence spectrogram obtained under 1.5 watts infrared ray excited.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1:
Prepare Ca9.45Er0.05Yb0.5Si3O15F2, according to chemical formula Ca9.45Er0.05Yb0.5Si3O15F2The chemistry of middle each element
Ratio is measured, calcium carbonate CaCO is weighed3: 8.503 grams, silicon oxide sio2: 1.8024 grams, erbium oxide Er2O3: 0.0010 gram, ytterbium oxide
Yb2O3: 0.010 gram, in the agate mortar grinding and after mixing, select air atmosphere pre-sintering, sintering temperature is 800 DEG C,
It sintering time 10 hours, then cools to room temperature, takes out sample and grind and be uniformly mixed；By the mixture of pre-sintering and 0.7808
Gram calcirm-fluoride CaF2It is sufficiently mixed grinding uniformly, and mixed powder is pressed, pressing pressure 10MPa, in sky
It is calcined again in gas atmosphere, 1100 DEG C of calcination temperature, calcination time 5 hours, natural cooling ground and mixed uniformly obtains fluorine silicon
Sour calcium fluorescence ceramics.
Referring to attached drawing 1, it is the X-ray powder diffraction pattern that the present embodiment technical solution prepares sample, XRD test result
It has been shown that, prepared Ca9.45Er0.05Yb0.5Si3O15F2For monophase materials, exist without other miscellaneous phases, and crystallinity is preferable,
Show trivalent erbium ion Er3+With trivalent ytterbium ion Yb3+Doping on the structure of matrix without influence.
Referring to attached drawing 2, it is the scanning electron microscope diagram spectrum that the present embodiment technical solution prepares sample, can be with from figure
Find out, the dispersion of gained sample particle is more uniform.
Referring to attached drawing 3, it is the sample Ca prepared by the present embodiment technical solution9.45Er0.05Yb0.5Si3O15F2It is received 976
Rice, excitation energy intensity are the up-conversion luminescence spectrogram obtained under 1.5 watts infrared ray excited, as seen from Figure 3: the material
Material transmitting main peak is red up-conversion luminescence near 670 nanometers.
Embodiment 2:
Prepare Ca9.49Er0.01Yb0.5Si3O15F2, according to chemical formula Ca9.49Er0.01Yb0.5Si3O15F2The chemistry of middle each element
Ratio is measured, weighs calcium hydroxide Ca (OH) respectively2: 4.9648 grams, silicic acid H2SiO3: 2.34 grams, erbium oxide Er2O3: 0.0020 gram,
Ytterbium oxide Yb2O3: 0.010 gram, grinding and after mixing in the agate mortar selects air atmosphere pre-sintering, sintering temperature is
It 950 DEG C, sintering time 3 hours, then cools to room temperature, takes out sample and grind and be uniformly mixed；By the raw material of pre-sintering with
2.3424 gram calcirm-fluoride CaF2It is sufficiently mixed grinding uniformly, and mixed powder is pressed, pressing pressure is
15MPa is calcined again in air atmosphere, and 950 DEG C of calcination temperature, calcination time 10 hours, natural cooling ground and mixed was uniform
Obtain calcium fluosilicate fluorescence ceramics.
Sample manufactured in the present embodiment, X-ray powder diffraction pattern, primary structure pattern, up-conversion luminescence spectrogram with
Embodiment 1 is similar.
Embodiment 3:
Prepare Ca9.4Er0.1Yb0.5Si3O15F2, according to chemical formula Ca9.4Er0.1Yb0.5Si3O15F2The chemistry meter of middle each element
Ratio is measured, weighs calcium oxalate CaC respectively2O4: 9.507 grams, silicic acid H2SiO3: 2.34 grams, erbium oxide Er2O3: 0.020 gram, ytterbium oxide
Yb2O3: 0.010 gram, in the agate mortar grinding and after mixing, select air atmosphere pre-sintering, sintering temperature is 900 DEG C,
It sintering time 4 hours, then cools to room temperature, takes out sample and grind and be uniformly mixed；By the raw material of pre-sintering again with
1.5616 gram calcirm-fluoride CaF2It is sufficiently mixed grinding uniformly, and by mixed powder compression moulding, pressing pressure 12MPa,
It is calcined again in air atmosphere, 900 DEG C of calcination temperature, calcination time 15 hours, natural cooling ground and mixed uniformly obtains fluorine
Calcium silicates fluorescence ceramics.
Sample manufactured in the present embodiment, X-ray powder diffraction pattern, primary structure pattern, up-conversion luminescence spectrogram with
Embodiment 1 is similar.
Embodiment 4:
Prepare Ca9Er0.2Yb0.8Si3O15F2, according to chemical formula Ca9Er0.2Yb0.8Si3O15F2The stoichiometry of middle each element
Than weighing CaO:3.5625 grams of calcium oxide respectively, silicon oxide sio2: 1.8027 grams, erbium oxide Er2O3: 0.040 gram, ytterbium oxide
Yb2O3: 0.016 gram, in the agate mortar grinding and after mixing, select air atmosphere pre-sintering, sintering temperature is 750 DEG C,
It sintering time 10 hours, then cools to room temperature, takes out sample and grind and be uniformly mixed；By the raw material of pre-sintering again with
1.952 grams of calcirm-fluoride CaF2It is sufficiently mixed grinding uniformly, and mixed powder is pressed, pressing pressure 13MPa,
It is calcined again in air atmosphere, 1200 DEG C of calcination temperature, calcination time 3 hours, natural cooling ground and mixed uniformly obtains
Calcium fluosilicate fluorescence ceramics.
Referring to attached drawing 4, be by the electron scanning micrograph of the sample of this implementation technical solution preparation, can be with from figure
Find out, the dispersion of gained sample particle is more uniform.
Referring to attached drawing 5, be by the present embodiment technical solution preparation sample 976 nanometers, excitation energy intensity be 1.5 watts
It is infrared ray excited under obtained up-conversion luminescence spectrogram, as seen from Figure 5: it is attached at 670 nanometers that the material emits main peak
It closely, is red up-conversion luminescence.
Embodiment 5:
Prepare Ca9.7Er0.2Yb0.1Si3O15F2, according to chemical formula Ca9.7Er0.2Yb0.1Si3O15F2The chemistry meter of middle each element
Ratio is measured, weighs calcium nitrate Ca (NO respectively3)2·4H2O:19.088 grams, silicon oxide sio2: 1.8027 grams, erbium oxide Er2O3:
0.040 gram, ytterbium oxide Yb2O3: 0.002 gram, in the agate mortar grinding and after mixing, select air atmosphere be pre-sintered, burning
Junction temperature is 870 DEG C, sintering time 5 hours, is then cooled to room temperature, and sample is taken out；By the raw material of pre-sintering again with
1.1712 gram calcirm-fluoride CaF2It is sufficiently mixed grinding uniformly, and mixed powder is pressed, pressing pressure 14MPa,
It is calcined again in air atmosphere, 980 DEG C of calcination temperature, calcination time 7 hours, natural cooling ground and mixed uniformly obtains fluorine
Calcium silicates fluorescence ceramics.
Sample manufactured in the present embodiment, primary structure pattern, up-conversion luminescence spectrogram are similar to Example 4.
Embodiment 6:
Prepare Ca8.3Er0.2Yb1.5Si3O15F2, according to chemical formula Ca8.3Er0.2Yb1.5Si3O15F2The chemistry meter of middle each element
Ratio is measured, weighs CaO:3.491 grams of calcium oxide respectively, silicon oxide sio2: 1.8027 grams, erbium oxide Er2O3: 0.040 gram, ytterbium oxide
Yb2O3: 0.030 gram, in the agate mortar grinding and after mixing, select air atmosphere pre-sintering, sintering temperature is 920 DEG C,
It sintering time 7 hours, then cools to room temperature, takes out sample and grind and be uniformly mixed；By the raw material of pre-sintering again with
3.1232 gram calcirm-fluoride CaF2It is sufficiently mixed grinding uniformly, and mixed powder is pressed, pressing pressure 14MPa,
It is calcined again in air atmosphere, 1050 DEG C of calcination temperature, calcination time 6 hours, natural cooling ground and mixed uniformly obtains
Calcium fluosilicate fluorescence ceramics.
Sample manufactured in the present embodiment, primary structure pattern, up-conversion luminescence spectrogram are similar to Example 4.
Claims (7)
1. a kind of fluosilicic acid alkali up-conversion luminescence ceramic material, it is characterised in that: chemical formula Ca10- 10xEr10xYb10ySi3O15F2, wherein x is Er3+The stoichiometry score of doping, y are ytterbium ion Yb3+The stoichiometry of doping point
Number, 0.001≤x+y < 0.2.
2. a kind of preparation method of fluosilicic acid alkali up-conversion luminescence ceramic material as described in claim 1, which is characterized in that
Using high temperature solid-state method, comprising the following steps:
(1) according to Ca10-10xEr10xYb10ySi3O15F2The stoichiometric ratio of middle each element, wherein 0.001≤x+y < 0.2 claims respectively
It takes containing calcium ion Ca2+Compound, contain silicon ion Si4+Compound, contain erbium ion Er3+Compound, containing ytterbium from
Sub- Yb3+Compound, contain fluorine ion F-Compound as raw material, and calcium ion Ca will be contained2+Compound, containing silicon from
Sub- Si4+Compound, contain erbium ion Er3+Compound, contain ytterbium ion Yb3+Compound mix and grind uniformly, obtain
Mixture；
(2) contain calcium ion Ca for what step (1) obtained2+Compound, contain silicon ion Si4+Compound, contain erbium ion
Er3+Compound, contain ytterbium ion Yb3+Mixture be sintered in air atmosphere, sintering temperature be 750~950 DEG C,
Sintering time is 3~10 hours, and after natural cooling, ground and mixed is uniform；
(3) powder mixture for obtaining step (2) with contain fluorine ion F-Compound mix and grind uniformly, be pressed into pottery
Tile, pressing pressure are 10MPa~15MPa, are calcined in air atmosphere, and calcination temperature is 900~1200 DEG C, and calcination time is
3~15 hours, natural cooling obtained fluosilicic acid alkali up-conversion luminescence ceramic material.
3. the preparation method of fluosilicic acid alkali up-conversion luminescence ceramic material according to claim 2, it is characterised in that: step
Suddenly the sintering temperature of (2) is 800~900 DEG C, and sintering time is 4~10 hours.
4. the preparation method of fluosilicic acid alkali up-conversion luminescence ceramic material according to claim 2, it is characterised in that: step
Suddenly the calcination temperature of (3) is 950~1100 DEG C, and calcination time is 5~10 hours.
5. the preparation method of fluosilicic acid alkali up-conversion luminescence ceramic material according to claim 2, it is characterised in that: will
The calcium fluosilicate ceramics that step (3) obtains are broken and fluosilicic acid alkali up-conversion luminescence ceramic material uniformly can be obtained in ground and mixed
Powder.
6. the preparation method of fluosilicic acid alkali up-conversion luminescence ceramic material according to claim 2, it is characterised in that: institute
That states contains calcium ion Ca2+Compound be calcium carbonate, calcium nitrate, calcium hydroxide, calcium oxalate, calcium oxide one kind；It is described to contain
There is silicon ion Si4+Compound be one of silica or silicic acid；Described contains fluorine ion F-Compound be fluorination
Calcium；Described contains erbium ion Er3+Compound be erbium oxide；Described contains ytterbium ion Yb3+Compound be ytterbium oxide.
7. the preparation method of fluosilicic acid alkali up-conversion luminescence ceramic material according to claim 2, it is characterised in that: institute
It states containing calcium ion Ca2+Compound mixed by two kinds of compounds, one of which is calcirm-fluoride, and the calcium that calcirm-fluoride provides accounts for
10vol%~40vol% of total calcium content, another kind are calcium carbonate, calcium nitrate, calcium hydroxide, calcium oxalate, one in calcium oxide
Kind.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4122349A (en) * | 1976-02-05 | 1978-10-24 | Rhone-Poulenc Industries | Novel luminophores emitting ultraviolet radiation, and uses thereof |
| CN102373062A (en) * | 2011-12-12 | 2012-03-14 | 苏州大学 | Fluosilicate red fluorescent powder suitable for white-light LED (Light-Emitting Diode) and preparation method thereof |
| CN103173225A (en) * | 2013-04-03 | 2013-06-26 | 苏州大学 | Blue fluosilicate fluorescent powder as well as preparation method and application |
| CN103242830A (en) * | 2013-05-16 | 2013-08-14 | 苏州大学 | Fluorosilicate-based blue-green fluorescent powder as well as preparation method and applications of fluorescent powder |
-
2017
- 2017-01-24 CN CN201710053762.1A patent/CN106811197B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4122349A (en) * | 1976-02-05 | 1978-10-24 | Rhone-Poulenc Industries | Novel luminophores emitting ultraviolet radiation, and uses thereof |
| CN102373062A (en) * | 2011-12-12 | 2012-03-14 | 苏州大学 | Fluosilicate red fluorescent powder suitable for white-light LED (Light-Emitting Diode) and preparation method thereof |
| CN103173225A (en) * | 2013-04-03 | 2013-06-26 | 苏州大学 | Blue fluosilicate fluorescent powder as well as preparation method and application |
| CN103242830A (en) * | 2013-05-16 | 2013-08-14 | 苏州大学 | Fluorosilicate-based blue-green fluorescent powder as well as preparation method and applications of fluorescent powder |
Non-Patent Citations (3)
| Title |
|---|
| Er3+/Yb3+共掺杂氧氟硅酸盐玻璃的上转换发光;徐时清，等;《光学学报》;20040917;第24卷(第8期);第1103-1106页 |
| Transparent glass ceramic containing Er3+:CaF2 nano-crystals prepared by sol-gel method;Lihua Zhou，et al.;《Materials Letters》;20070112;第61卷;第3988-3990页 |
| Upconversion fluorescence spectroscopy of Er3+/Yb3+-codoped lead oxyfluorosilicate glass;Shiqing Xu et al.;《Chemical Physics Letters》;20040119;第385卷;第263-267页 |
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