CN106811197A - 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, its chemical general formula is Ca10‑ 10xEr10xYb10ySi3O15F2, wherein x is Er3+The stoichiometry fraction of doping, y is ytterbium ion Yb3+The stoichiometry fraction of doping, 0.001≤x+y<0.2.Obtained up-conversion luminescent material lattice structure stabilization of the invention, grain size are uniform, stable luminescent property, in the case where 976 nanometers of infrared lasers are excited, occur emitting red light peak near 670 nano wave lengths, and luminance purity is high, upper high conversion efficiency；Because matrix structure stabilization, rare earth doped concentration are high, exciting under being conducive to strengthening luminous efficiency and realizing 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, process is simple, and raw material sources enrich, cheap；And discharged without waste water and gas in technical process, and it is nontoxic, it is environmentally friendly, used beneficial to further genralrlization.
Description
Technical field
The present invention relates to solid fluorescent material field, particularly a kind of fluosilicic acid alkali up-conversion luminescence ceramic material and its
Preparation method.
Background technology
In recent years, up-conversion luminescent material causes the extensive concern of people.In embedded photoluminescent material, two or many are absorbed
The luminescent material of a high-energy photon transmitting is produced to be defined as up-conversion luminescent material (referred to as after the individual photon compared with low energy
UCPs).The upper conversion phenomena essence of this material is anti-Stokes effect, that is, the energy for radiating is more than absorbed energy,
Its principle of luminosity for light source be irradiated to material surface when, particle can absorb two or more low-lying excitation photon, electricity
Then son outwards gives off high-energy photon from ground state transition to upper state, and the high-energy photon frequency that it gives off is more than absorption light
Frequency.Up-conversion luminescent material can effectively reduce photo ionization and cause host material to fail, it is not necessary to strict 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 with rare earth doped element to realize that it lights.Due to rare earth outer shell electronics pair
The shielding action of 4f electronics, cause with metastable rare earth element it is luminous be mainly based upon the interelectric transition of 4f, people
The sightless infrared light of eye is converted into the visible ray that people are observed that.People are answered according to this feature of upper conversion
Use on Infrared Detectors, effectively raise sensitivity.Additionally, 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.
At present, up-conversion luminescent material is concentrated mainly on the systems such as rare-earth-doped fluoride, sulfide, halide, can be with
The transmitting of red, green, blue and white light is realized, but in actual applications, because the stability of these host materials is inadequate, prepare work
Skill is complicated, and use and popularization and application to up-conversion luminescent material bring greater impact.
The content of the invention
For the problem that above-mentioned prior art is present, it is an object of the invention to provide a kind of lattice and stable in properties, property
The excellent fluosilicic acid alkali up-conversion luminescence ceramic material of energy, easily grasps another object of the present invention is to provide preparation process is simple
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：A kind of fluosilicic acid alkali up-conversion luminescence ceramics material
Material, chemical formula is Ca10-10xEr10xYb10ySi3O15F2, wherein x is Er3+The stoichiometry fraction of doping, y is ytterbium ion Yb3+Mix
Miscellaneous stoichiometry fraction, 0.001≤x+y<0.2.
Present invention also offers a kind of preparation method of fluosilicic acid alkali up-conversion luminescence ceramic material, using high temperature solid-state
Method, comprises the following steps：
(1) according to Ca10-10xEr10xYb10ySi3O15F2The stoichiometric proportion of middle each element, wherein 0.001≤x+y<0.2 point
Another name takes and contains 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 uniform,
Obtain mixture；
(2) calcium ion Ca is contained by what step (1) was 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 uniform, compacting
Into potsherd, pressing pressure is 10MPa~15MPa, is calcined in air atmosphere, and calcining heat is 900~1200 DEG C, during calcining
Between be 3~15 hours, natural cooling, obtain calcium fluosilicate ceramics.
Used as a preferred scheme of above-mentioned preparation method, the sintering temperature of step (2) is 800~900 DEG C, sintering time
It is 4~10 hours.
Used as a preferred scheme of above-mentioned preparation method, the calcining heat of step (3) is 950~1100 DEG C, during calcining
Between be 5~10 hours.
In above-mentioned preparation method：The calcium fluosilicate ceramics that step (3) is obtained are broken and ground and mixed uniformly can obtain fluorine
Calcium silicate ceramic powder body.
In preparation method of the present invention, described contains calcium ion Ca2+Compound for calcium carbonate, calcium nitrate, calcium hydroxide,
One kind of calcium oxalate, calcium oxide；It is described to contain silicon ion Si4+Compound be the one kind in 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 scheme of preparation method2+Compound mixed by two kinds of compounds,
One of which is calcirm-fluoride, and the calcium that calcirm-fluoride is provided accounts for the 10vol%~40vol% of TC, and another kind is calcium carbonate, nitric acid
One kind in calcium, calcium hydroxide, calcium oxalate, calcium oxide.
Compared with prior art, the present invention has the advantages that：
(1) fluosilicate up-conversion luminescent material lattice structure stabilization of the invention, phonon energy are low, are conducive to improving
Change luminous efficiency and excite 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, obtained up-conversion luminescent material grain size are uniform, stable luminescent property,
Compared with other oxysulfides, halide up-conversion luminescent material, with novelty and repeatability preferably；
(2) in the case where 976 nanometers of infrared lasers are excited, the emitting red light peak near 670 nano wave lengths can be launched, is lighted
Purity is high；Because the rare earth concentration of matrix structure stabilization, doping is high, it is advantageously implemented exciting under high power and strengthens luminous effect
Rate, can apply as red upconverting fluorescent material.Apply it on Infrared Detectors, can effectively improve sensitive
Degree, it can in addition contain be widely used in the necks such as laser technology, optical fiber communication technology, optical information storage and fibre amplifier
, there is larger 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, process is simple, raw material sources enrich, cheap；And discharged without waste water and gas in technical process, and it is nontoxic, it is right
It is environment-friendly, used beneficial to further genralrlization.
Brief description of the drawings
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
It is 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
Metering ratio, weighs calcium carbonate CaCO3：8.503 grams, silicon oxide sio2：1.8024 grams, erbium oxide Er2O3：0.0010 gram, ytterbium oxide
Yb2O3：0.010 gram, after grinding and be well mixed in agate mortar, selection air atmosphere is pre-sintered, and sintering temperature is 800 DEG C,
Sintering time 10 hours, is subsequently cooled to room temperature, takes out sample and grinds and be well mixed；By pre-sintered mixture and 0.7808
Gram calcirm-fluoride CaF2It is sufficiently mixed grinding uniform, and mixed powder is pressed, pressing pressure is 10MPa, in sky
Calcined again in gas atmosphere, 1100 DEG C of calcining heat, calcination time 5 hours, natural cooling ground and mixed uniformly obtains fluorine silicon
Sour calcium fluorescence ceramics.
Referring to accompanying drawing 1, it is the X-ray powder diffraction pattern that the present embodiment technical scheme prepares sample, XRD test results
It has been shown that, prepared Ca9.45Er0.05Yb0.5Si3O15F2It is monophase materialses, there is no other dephasigns, and crystallinity is preferably,
Show trivalent erbium ion Er3+With trivalent ytterbium ion Yb3+Doping on the structure of matrix without influence.
Referring to accompanying drawing 2, it is the scanning electron microscope diagram spectrum that the present embodiment technical scheme prepares sample, can be with from figure
Find out, the dispersion of gained sample particle is more uniform.
Referring to accompanying drawing 3, it is the sample Ca prepared by the present embodiment technical scheme9.45Er0.05Yb0.5Si3O15F2Received 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, in 670 nms, is red up-conversion luminescence.
Embodiment 2：
Prepare Ca9.49Er0.01Yb0.5Si3O15F2, according to chemical formula Ca9.49Er0.01Yb0.5Si3O15F2The chemistry of middle each element
Metering ratio, 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, after grinding and be well mixed in agate mortar, selection air atmosphere is pre-sintered, and sintering temperature is
950 DEG C, sintering time 3 hours is subsequently cooled to room temperature, takes out sample and grinds and be well mixed；By pre-sintered raw material with
2.3424 grams of calcirm-fluoride CaF2It is sufficiently mixed grinding uniform, and mixed powder is pressed, pressing pressure is
15MPa, calcines again in air atmosphere, 950 DEG C of calcining heat, calcination time 10 hours, and natural cooling ground and mixed is uniform
Obtain calcium fluosilicate fluorescence ceramics.
Sample manufactured in the present embodiment, its 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
Amount ratio, 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, after grinding and be well mixed in agate mortar, selection air atmosphere is pre-sintered, and sintering temperature is 900 DEG C,
Sintering time 4 hours, is subsequently cooled to room temperature, takes out sample and grinds and be well mixed；By pre-sintered raw material again with
1.5616 grams of calcirm-fluoride CaF2It is sufficiently mixed grinding uniform and mixed powder is compressing, pressing pressure is 12MPa,
Calcined again in air atmosphere, 900 DEG C of calcining heat, calcination time 15 hours, natural cooling ground and mixed uniformly obtains fluorine
Calcium silicates fluorescence ceramics.
Sample manufactured in the present embodiment, its 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 calcium oxide CaO respectively：3.5625 grams, silicon oxide sio2：1.8027 grams, erbium oxide Er2O3：0.040 gram, ytterbium oxide
Yb2O3：0.016 gram, after grinding and be well mixed in agate mortar, selection air atmosphere is pre-sintered, and sintering temperature is 750 DEG C,
Sintering time 10 hours, is subsequently cooled to room temperature, takes out sample and grinds and be well mixed；By pre-sintered raw material again with
1.952 grams of calcirm-fluoride CaF2It is sufficiently mixed grinding uniform, and mixed powder is pressed, pressing pressure is 13MPa,
Calcined again in air atmosphere, 1200 DEG C of calcining heat, calcination time 3 hours, natural cooling ground and mixed is uniformly obtained
Calcium fluosilicate fluorescence ceramics.
It is the electron scanning micrograph of the sample prepared by this implementation technical scheme referring to accompanying drawing 4, can be with from figure
Find out, the dispersion of gained sample particle is more uniform.
It is that the sample prepared by the present embodiment technical scheme is 1.5 watts in 976 nanometers, excitation energy intensity referring to accompanying drawing 5
It is infrared ray excited under the up-conversion luminescence spectrogram that obtains, as seen from Figure 5：Material transmitting main peak is attached at 670 nanometers
Closely, it 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
Amount ratio, 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, after grinding and be well mixed in agate mortar, selection air atmosphere is pre-sintered, burns
Junction temperature is 870 DEG C, sintering time 5 hours, is subsequently cooled to room temperature, takes out sample；By pre-sintered raw material again with
1.1712 grams of calcirm-fluoride CaF2It is sufficiently mixed grinding uniform, and mixed powder is pressed, pressing pressure is 14MPa,
Calcined again in air atmosphere, 980 DEG C of calcining heat, calcination time 7 hours, natural cooling ground and mixed uniformly obtains fluorine
Calcium silicates fluorescence ceramics.
Sample manufactured in the present embodiment, its 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
Amount ratio, weighs calcium oxide CaO respectively：3.491 grams, silicon oxide sio2：1.8027 grams, erbium oxide Er2O3：0.040 gram, ytterbium oxide
Yb2O3：0.030 gram, after grinding and be well mixed in agate mortar, selection air atmosphere is pre-sintered, and sintering temperature is 920 DEG C,
Sintering time 7 hours, is subsequently cooled to room temperature, takes out sample and grinds and be well mixed；By pre-sintered raw material again with
3.1232 grams of calcirm-fluoride CaF2It is sufficiently mixed grinding uniform, and mixed powder is pressed, pressing pressure is 14MPa,
Calcined again in air atmosphere, 1050 DEG C of calcining heat, calcination time 6 hours, natural cooling ground and mixed is uniformly obtained
Calcium fluosilicate fluorescence ceramics.
Sample manufactured in the present embodiment, its 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 is Ca10- 10xEr10xYb10ySi3O15F2, wherein x is Er3+The stoichiometry fraction of doping, y is 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 claimed in claim 1, it is characterised in that
Using high temperature solid-state method, comprise the following steps：
(1) according to Ca10-10xEr10xYb10ySi3O15F2The stoichiometric proportion of middle each element, wherein 0.001≤x+y<0.2 claims respectively
Take and contain 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 uniform, obtain
Mixture；
(2) calcium ion Ca is contained by what step (1) was 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 uniform, be pressed into pottery
Ceramics, pressing pressure is 10MPa~15MPa, is calcined in air atmosphere, and calcining heat is 900~1200 DEG C, and calcination time is
3~15 hours, natural cooling obtained calcium fluosilicate ceramics.
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 calcining heat 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) is obtained are broken and ground and mixed uniformly can obtain calcium fluosilicate ceramic 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, one kind of calcium oxide；It is described to contain
There is silicon ion Si4+Compound be the one kind in silica or silicic acid；Described contains fluorine ion F-Compound for 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
State and contain calcium ion Ca2+Compound mixed by two kinds of compounds, one of which is calcirm-fluoride, and the calcium that calcirm-fluoride is provided is accounted for
10vol%~the 40vol% of TC, another kind is in calcium carbonate, calcium nitrate, calcium hydroxide, calcium oxalate, 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 |
|---|
| LIHUA ZHOU，ET AL.: "Transparent glass ceramic containing Er3+:CaF2 nano-crystals prepared by sol-gel method", 《MATERIALS LETTERS》 * |
| SHIQING XU ET AL.: "Upconversion fluorescence spectroscopy of Er3+/Yb3+-codoped lead oxyfluorosilicate glass", 《CHEMICAL PHYSICS LETTERS》 * |
| 徐时清，等: "Er3+/Yb3+共掺杂氧氟硅酸盐玻璃的上转换发光", 《光学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019136830A1 (en) * | 2018-01-10 | 2019-07-18 | 深圳光峰科技股份有限公司 | Wavelength conversion apparatus |
| US11296263B2 (en) | 2018-01-10 | 2022-04-05 | Appotronics Corporation | Wavelength conversion apparatus |
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Effective date of registration: 20191120 Address after: 210000 No. 22 Jingang Road, Dongping Town, Lishui District, Nanjing City, Jiangsu Province Patentee after: Nanjing Tongli Crystal Materials Research Institute Co., Ltd. Address before: 221100 Shanghai Road, Copper Mt. New District, Jiangsu, No. 101, No. Patentee before: Jiangsu Normal University |