CN107527983B - Full-inorganic flexible up-conversion luminescent device and preparation method thereof - Google Patents
Full-inorganic flexible up-conversion luminescent device and preparation method thereof Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 10
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- 239000010408 film Substances 0.000 claims abstract description 20
- 239000010445 mica Substances 0.000 claims abstract description 20
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 20
- 239000010409 thin film Substances 0.000 claims abstract description 13
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract 2
- 239000013077 target material Substances 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000003776 cleavage reaction Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 238000005137 deposition process Methods 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 230000007017 scission Effects 0.000 claims description 3
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052627 muscovite Inorganic materials 0.000 claims description 2
- 229910052628 phlogopite Inorganic materials 0.000 claims description 2
- 238000000053 physical method Methods 0.000 claims description 2
- 238000004891 communication Methods 0.000 abstract description 4
- 238000013473 artificial intelligence Methods 0.000 abstract description 2
- 239000000090 biomarker Substances 0.000 abstract 1
- 238000001259 photo etching Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 20
- 238000000034 method Methods 0.000 description 8
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 238000000151 deposition Methods 0.000 description 6
- 238000004020 luminiscence type Methods 0.000 description 5
- -1 rare earth ions Chemical class 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
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- 230000003287 optical effect Effects 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001748 luminescence spectrum Methods 0.000 description 2
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- 230000008018 melting Effects 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000001215 fluorescent labelling Methods 0.000 description 1
- 229940104869 fluorosilicate Drugs 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
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- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
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- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
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Abstract
The invention discloses a full-inorganic flexible up-conversion luminescent device and a preparation method thereof, and the device comprises a flexible ultrathin mica substrate and an inorganic up-conversion luminescent thin film layer, wherein the inorganic up-conversion luminescent thin film layer is Ba doped with 0.75% Er and 0.75% Yb0.85Ca0.15TiO3A film. The invention obtains the full inorganic flexible up-conversion luminescent device by directly growing the inorganic up-conversion luminescent film on the flexible ultrathin mica substrate, the preparation method is very simple, the cost is low, and the mass production can be realized; the invention can be widely applied to the fields of biomarkers, solar cells, photoetching, submarine communication, video display, fire-proof channel indication boards, wearable equipment and artificial intelligence.
Description
Technical Field
The invention belongs to the field of up-conversion luminescent devices, and particularly relates to an all-inorganic flexible up-conversion luminescent device.
Background
Upconversion luminescence is a luminescent process in which the emission wavelength is shorter than the excitation wavelength, and is an anti-stokes process. The up-conversion luminescence of the rare earth doped material is an important way for realizing light wave frequency conversion, and multi-photon conversion of rare earth ions is converted into single photon output, so that short wavelength fluorescence output is realized. The up-conversion inorganic luminescent material taking rare earth ions as luminescent centers and having frequencies from near infrared to visible bands has wide application prospects in the fields of laser, optical communication, flat panel display, fluorescent labeling, photoelectronic devices and the like. At present, the power of the rare earth ion upconversion laser is equivalent to that of a short-wavelength laser directly excited by a wide-bandgap semiconductor material, but the rare earth ion upconversion laser has incomparable advantages compared with the wide-bandgap semiconductor laser in the aspects of beam quality, stability and the like, so that upconversion luminescence is more beneficial to the development of a simple, cheap and compact-structure small laser system.
With the development of artificial intelligent robots and wearable devices, higher requirements are put on the physical properties of traditional up-conversion luminescent materials. In addition to achieving high upconversion performance, materials are required to have high flexibility, bending characteristics, and fatigue resistance. However, current all-inorganic up-conversion luminescent materials are mainly based on rare earth ion doped oxide rigid materials and corresponding thin film materials grown on rigid substrates. The materials have high rigidity coefficient and high Young modulus, and cannot meet the application requirement of flexible and wearable materials. Therefore, the invention provides a new idea for preparing the all-inorganic rare earth up-conversion luminescent material by using the layered two-dimensional material as the substrate and growing the layered two-dimensional material at a high temperature through a pulse laser deposition method based on the current research situation.
The pulsed laser deposition method is a means of bombarding an object with laser and then depositing the bombarded substance on different substrates to obtain a deposit or a thin film. The method comprises four basic processes of interaction of laser radiation and a target, dynamic state of a melting substance, deposition of the melting substance on a substrate, nucleation and generation of a thin film on the surface of the substrate. The film preparation method has the advantages of high deposition rate, short test period, low requirement on substrate temperature, uniform prepared film and the like.
At present, no relevant Chinese patent of an all-inorganic flexible upconversion luminescent device exists, and a few patents introduce rigid upconversion luminescent materials, for example, Chinese patent CN106811197A adopts a high-temperature solid-phase method to prepare a fluorosilicate-based upconversion ceramic material; chinese patent CN106905964A adopts a high-temperature solid phase method to prepare a green upconversion luminous material of titanium niobate. The preparation method and the new material related to the invention provide a method foundation and a material foundation for the application of the upconversion luminescent material in the fields of laser, optical communication, flat panel display, fluorescent marking, optoelectronic devices and the like, but the rigidity and the brittleness of the upconversion luminescent material cannot meet the application requirements of novel flexible lasers, flexible optical communication, flexible display and flexible optoelectronic devices.
Disclosure of Invention
The invention aims to provide an all-inorganic flexible up-conversion light-emitting device and a preparation method thereof.
The technical purpose of the invention is realized as follows: an all-inorganic flexible up-conversion luminescent device comprises a flexible ultrathin mica substrate and an inorganic up-conversion luminescent thin film layer, wherein the inorganic up-conversion luminescent thin film layer is Ba doped with 0.75% Er and 0.75% Yb0.85Ca0.15TiO3A thin film (hereinafter referred to as BCTO).
Furthermore, the flexible ultrathin mica substrate adopts any one of various types of mica such as muscovite, phlogopite or fluorine crystal mica.
Further, the thickness of the flexible ultrathin mica substrate is less than 5 micrometers.
The preparation method of the all-inorganic flexible up-conversion luminescent device comprises the following steps:
(1) preparing a target material according to the stoichiometric ratio of the inorganic up-conversion luminescent thin film layer;
(2) peeling the mica substrate along the cleavage plane by a physical method to thin the mica substrate to below 5 microns;
(3) setting the deposition temperature at 500-800 deg.c, oxygen pressure at 0.1-100Pa and laser energy at 50-250mJ, and preparing film through pulse laser deposition process.
Compared with the prior art, the invention has the advantages that:
(1) the invention adopts the ultrathin mica sheet as the flexible substrate, realizes the preparation of the all-inorganic flexible up-conversion device for the first time, has very simple process, does not need subsequent treatments such as substrate corrosion, film transfer and the like, has rich raw material sources and low cost, and can be produced in large batch.
(2) The all-inorganic flexible up-conversion luminescent device has excellent and stable luminescent performance.
(3) The all-inorganic flexible up-conversion luminescent device has good flexibility, and has great significance and wide application in the field of wearable artificial intelligence.
(4) The thickness of the inorganic up-conversion luminescent film layer can be 10-2000nm, the surface is flat, the formed phase is single and has no impure phase, the inorganic up-conversion luminescent film layer has better ferroelectricity and up-conversion luminescent characteristics, and the performance is stable under the bending condition.
Drawings
Fig. 1 is a schematic view of a macroscopic cross-sectional structure of an all-inorganic flexible up-conversion light emitting device.
Fig. 2 is an X-ray diffraction (hereinafter, XRD) spectrum of the BCTO-based all-inorganic flexible up-conversion light emitting device in example 1 of the present invention.
Fig. 3 is an atomic force microscope (hereinafter AFM) surface topography map of the BCTO-based all-inorganic flexible upconversion luminescent device in example 1 of the present invention.
Fig. 4 is an upconversion luminescence spectrum of an all-inorganic flexible upconversion light emitting device based on BCTO in example 1 of the present invention in both flat and bent states.
Detailed Description
The following are merely preferred embodiments of the present invention, which should not be construed as limiting the scope of the invention. All modifications made according to the claims of the present invention are within the scope of the present invention.
In order to make the objects, technical solutions and advantages of the present invention more clear, a full inorganic flexible up-conversion light emitting device of the present invention is described in detail with particular reference to the drawings in the following examples.
The invention relates to an all-inorganic flexible up-conversion luminescent device, and a schematic diagram of a macroscopic cross-sectional structure of the up-conversion luminescent device is shown in figure 1.
Example 1:
an all-inorganic flexible upconversion luminescent device based on a BCTO thin film material doped with 0.75% mol Er and 0.75% mol Yb.
(1) And (5) peeling and thinning the mica substrate. Commercial artificial fluorine crystal mica is selected as a raw material, a mechanical thinning method is adopted, and the mica is peeled and thinned to be below 5 microns along the cleavage surface by using an adhesive tape or a blade, so that the mica has very good flexibility.
(2) And (3) preparing a film.
Preparing a target material: according to the chemical formula Ba of the target material0.85Ca0.15TiO3Er 0.75 mol% Yb 0.75 mol% inThe stoichiometric ratio of each element is weighed to obtain BaCO3(99.95%)12.626 g CaCO3(99.99%)1.131 g TiO2(99.8%)6.024 g Er2O3(99.9%)0.011 g Yb2O3(99.9%)0.011 g, mixing the ingredients by ball milling, drying at 80 ℃ ambient temperature, presintering the powder for 3h at 1000 ℃, adding 5% by mass of PVA for granulation, sieving, pressing the powder into a round blank under the pressure of about 100MPa, and sintering in a muffle furnace at 1350 ℃ to prepare the BCTO target material.
Preparation work: cleaning the growth cavity, the sample holder and the substrate, and then fixing the substrate. Mounting a target material, adjusting the target distance to be 70mm, and adjusting the laser energy to be 70 mJ;
and (3) deposition process: setting the deposition temperature to 710 ℃ and the oxygen pressure to 1Pa, vacuumizing, controlling the temperature rise and the atmosphere, pre-sputtering, growing a film, and annealing in situ;
and (4) follow-up work: slowly cooling, taking out the sample, closing the laser and keeping the vacuum cavity in vacuum.
(3) The structure of the prepared BCTO film was tested using an X-ray diffractometer, and as a result, as shown in fig. 2, it can be seen in the XRD spectrum that the film was completely phased and no hetero-phase appeared.
(4) The surface morphology of the BCTO film prepared by AFM test is shown in FIG. 3. The surface flatness of the flexible film sample is visually represented in the figure, the BCTO film surface fluctuation is only 10nm, and the film surface is flat.
(5) The up-conversion luminescence spectrum and the attenuation curve of the BCTO film in a straight state and a bent state are tested by using a fluorescence spectrophotometer and a 980nm near-infrared laser, and the up-conversion luminescence efficiency is measured by using an integrating sphere. The up-conversion luminescence spectra of the BCTO film in the flat and bent states are shown in fig. 4. Under the excitation of an excitation light source of 980nm, the BCTO film emits green light at the wavelength of 550 nm. Under the bending state, the flexible up-conversion light-emitting device still keeps higher luminous intensity, shows the stability of the flexible light-emitting device, and provides a device basis for meeting the application requirements of flexible wearable devices.
Claims (2)
1. The all-inorganic flexible up-conversion luminescent device comprises a flexible ultrathin mica substrate and an inorganic up-conversion luminescent thin film layer, and is characterized in that the inorganic up-conversion luminescent thin film layer is Ba doped with 0.75 mol% Er and 0.75 mol% Yb0.85Ca0.15TiO3The flexible ultrathin mica substrate adopts any one of muscovite, phlogopite or fluorine crystal mica; the thickness of the flexible ultrathin mica substrate is less than 5 micrometers.
2. The method of making an all-inorganic flexible up-conversion light emitting device of claim 1, comprising the steps of:
(1) preparing a target material according to the stoichiometric ratio of the inorganic up-conversion luminescent thin film layer;
(2) peeling the mica substrate along the cleavage plane by a physical method to thin the mica substrate to below 5 microns;
(3) setting the deposition temperature at 500-800 deg.c, oxygen pressure at 0.1-100Pa and laser energy at 50-250mJ, and preparing film through pulse laser deposition process.
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