CN116826506A - Method for simultaneously transmitting visible and near infrared integrated multi-wavelength laser under single pump - Google Patents
Method for simultaneously transmitting visible and near infrared integrated multi-wavelength laser under single pump Download PDFInfo
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- CN116826506A CN116826506A CN202310262823.0A CN202310262823A CN116826506A CN 116826506 A CN116826506 A CN 116826506A CN 202310262823 A CN202310262823 A CN 202310262823A CN 116826506 A CN116826506 A CN 116826506A
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000011521 glass Substances 0.000 claims abstract description 195
- 239000004005 microsphere Substances 0.000 claims abstract description 116
- 239000002131 composite material Substances 0.000 claims abstract description 77
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 53
- -1 rare earth ions Chemical class 0.000 claims abstract description 49
- 239000011159 matrix material Substances 0.000 claims abstract description 40
- 229910001428 transition metal ion Inorganic materials 0.000 claims abstract description 38
- 239000013078 crystal Substances 0.000 claims abstract description 21
- 238000005086 pumping Methods 0.000 claims abstract description 16
- 239000004065 semiconductor Substances 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims description 21
- 230000008018 melting Effects 0.000 claims description 21
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- 239000000843 powder Substances 0.000 claims description 18
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- 229910052723 transition metal Inorganic materials 0.000 claims description 12
- 150000003624 transition metals Chemical class 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 5
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
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- 229910000480 nickel oxide Inorganic materials 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- QGJSAGBHFTXOTM-UHFFFAOYSA-K trifluoroerbium Chemical compound F[Er](F)F QGJSAGBHFTXOTM-UHFFFAOYSA-K 0.000 claims description 4
- 229940105963 yttrium fluoride Drugs 0.000 claims description 4
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 claims description 4
- OKOSPWNNXVDXKZ-UHFFFAOYSA-N but-3-enoyl chloride Chemical compound ClC(=O)CC=C OKOSPWNNXVDXKZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 claims description 3
- XRADHEAKQRNYQQ-UHFFFAOYSA-K trifluoroneodymium Chemical compound F[Nd](F)F XRADHEAKQRNYQQ-UHFFFAOYSA-K 0.000 claims description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 2
- AATUHDXSJTXIHB-UHFFFAOYSA-K trifluorothulium Chemical compound F[Tm](F)F AATUHDXSJTXIHB-UHFFFAOYSA-K 0.000 claims description 2
- XASAPYQVQBKMIN-UHFFFAOYSA-K ytterbium(iii) fluoride Chemical compound F[Yb](F)F XASAPYQVQBKMIN-UHFFFAOYSA-K 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims 1
- 229910000423 chromium oxide Inorganic materials 0.000 claims 1
- 229910001195 gallium oxide Inorganic materials 0.000 claims 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 10
- 238000001514 detection method Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 38
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 22
- 239000002159 nanocrystal Substances 0.000 description 15
- 238000002360 preparation method Methods 0.000 description 13
- 230000008901 benefit Effects 0.000 description 7
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000013307 optical fiber Substances 0.000 description 5
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 4
- 238000005090 crystal field Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 238000004020 luminiscence type Methods 0.000 description 4
- 238000010309 melting process Methods 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 3
- JQMFQLVAJGZSQS-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JQMFQLVAJGZSQS-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910017768 LaF 3 Inorganic materials 0.000 description 2
- 230000005679 Peltier effect Effects 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
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- 239000000047 product Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 230000010354 integration Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
- H01S3/16—Solid materials
- H01S3/17—Solid materials amorphous, e.g. glass
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/05—Construction or shape of optical resonators; Accommodation of active medium therein; Shape of active medium
- H01S3/08—Construction or shape of optical resonators or components thereof
- H01S3/08086—Multiple-wavelength emission
- H01S3/0809—Two-wavelenghth emission
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- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
- H01S3/16—Solid materials
- H01S3/1601—Solid materials characterised by an active (lasing) ion
- H01S3/1603—Solid materials characterised by an active (lasing) ion rare earth
- H01S3/1608—Solid materials characterised by an active (lasing) ion rare earth erbium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
- H01S3/16—Solid materials
- H01S3/1601—Solid materials characterised by an active (lasing) ion
- H01S3/1603—Solid materials characterised by an active (lasing) ion rare earth
- H01S3/1616—Solid materials characterised by an active (lasing) ion rare earth thulium
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- H—ELECTRICITY
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- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
- H01S3/16—Solid materials
- H01S3/1601—Solid materials characterised by an active (lasing) ion
- H01S3/1603—Solid materials characterised by an active (lasing) ion rare earth
- H01S3/1618—Solid materials characterised by an active (lasing) ion rare earth ytterbium
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- H—ELECTRICITY
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- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
- H01S3/16—Solid materials
- H01S3/1601—Solid materials characterised by an active (lasing) ion
- H01S3/162—Solid materials characterised by an active (lasing) ion transition metal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
- H01S3/16—Solid materials
- H01S3/169—Nanoparticles, e.g. doped nanoparticles acting as a gain material
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Abstract
The application discloses a method for simultaneously emitting visible and near infrared integrated multi-wavelength laser under single pump. The double-phase nanocrystalline composite glass microsphere co-doped with transition metal ions and rare earth ions is used as a laser, and the simultaneous emission of visible light 450-700nm and laser light of near infrared band 750-2000nm is realized under 980nm semiconductor laser pumping; the double-phase nanocrystalline composite glass microsphere co-doped with transition metal ions and rare earth ions comprises a glass matrix and a luminescence center; the glass matrix comprises a glass network former, a glass network intermediate, and a crystal source; the luminescent center includes rare earth ions and transition metal ions. The glass microsphere prepared by the application can be used in the fields of serving as a low-threshold ultra-wideband multi-wavelength miniature integrated laser light source in a photon chip (integrated optical path), serving as a multi-wavelength display light source in three-dimensional display, preparing a sensor for ultra-sensitive sensing detection and the like.
Description
Technical Field
The application relates to the technical field, in particular to a visible and near infrared integrated laser emission method under single pumping.
Background
The transmission level of the optical network is continuously expanded, namely the transmission road width of the optical network is continuously and deeply analyzed, and the low-loss bandwidth resource of the full-wave quartz optical fiber is fully utilized. There is an urgent need to develop novel broadband optical amplification materials. Meanwhile, with the development trend of miniaturization and integration of optoelectronic components in recent years, the micro laser integrates a laser gain medium and a resonant cavity, has the outstanding advantages of small size, compact structure, low cost, low power consumption and the like, and is widely interested in scientific research and industry. The ultra-wideband and low-threshold micro laser with the working wave band positioned in the near infrared low-loss optical wave band (1260-1625 nm) has important application prospect in the fields of on-chip communication light source, high-density information storage, ultrasensitive sensing, optical precision measurement and the like, and the related research becomes the front edge of the photonics field. Especially, the light source on the silicon substrate in the later molar age, which is widely paid attention to in the present stage, provides a great challenge for the micro laser capable of simultaneously realizing the emission of the laser covering the O+E+S+C+L wave bands. The choice of the appropriate high gain medium and the high quality factor of the cavity is critical to achieving a micro laser as described above.
The rare earth ion doped light emitting device can increase the gain spectrum range to a certain extent by changing the matrix or rare earth ion co-doping, but the expected ultra-wideband light emitting device is difficult to obtain due to the limitation of the narrow-line light emitting characteristic of rare earth. Transition metal ions are in a specific coordination field environment in a crystal medium, and broadband luminescence with longer service life is shown in a near infrared band, but the application of the transition metal ions is limited by the preparation method and the processing requirement of the crystal. The glass medium has the advantage of easy processing, but transition metal ions are directly doped in the glass, so that the probability of non-radiative transition is increased due to the distorted coordination field environment in the glass medium. The glass composition is reasonably designed, a bulk glass precursor is prepared by adopting a traditional melting quenching method, and then the glass is subjected to heat treatment, so that crystals can be separated out in the glass, and the nanocrystalline composite glass is obtained. The size of crystal grains precipitated in the glass is generally tens of nanometers, which is far smaller than the wavelength of visible light so as to avoid scattering, so that the nanocrystalline composite glass can still keep good light transmittance and lower loss. Therefore, the transition metal ion doped nanocrystalline composite glass combines the advantages of the crystal and the glass, simultaneously eliminates the defects of the crystal and the glass, and can be used as a gain matrix material of a near infrared ultra-wideband light source.
It is assumed that if rare earth ions and transition metal ions can be doped in a glass system at the same time, luminescence of the rare earth ions and the transition metal ions can be obtained at the same time under a single pump, and the optical bandwidth is definitely greatly widened. The university of south China science and technology Zhou Shifeng in 2010 teaches open work in journal Journal of American Chemical Society of the American society of chemistry, designed SiO 2 /Na 2 O/Ga 2 O 3 /LaF 3 Specific glass system = 51/15/20/14 (mol%) capable of ordered precipitation of LaF 3 And Ga 2 O 3 Two nanocrystals such that Er is co-doped 3+ And Ni 2+ Can enter two kinds of nanocrystals respectively, benefit from the isolation of the distance between two kinds of active ions in physical sense and the change of local crystal field, effectively inhibit the energy transfer of the active ions with two different properties, and realize integrated multicolor visible and near infrared ultra-wideband fluorescence luminescence. Numerous researchers at home and abroad report more rare earth ions and transition metal ions co-doped double-phase nanocrystalline composite glass, but unfortunately, the glass is nanoThe nanocrystalline composite bulk glass is of an open structure, the light field binding capability of the nanocrystalline composite bulk glass is still limited, and laser emission in the double-phase nanocrystalline composite glass co-doped with rare earth ions and transition metal ions is not realized until now. Therefore, there is a need to develop a dual-phase nanocrystalline composite glass microsphere laser that can achieve laser emission with rare earth ions and transition metals co-doped, and can achieve visible and near infrared integrated laser emission with a single pump.
Disclosure of Invention
The application aims to provide a visible and near infrared integrated laser emission method under a single pump. The rare earth ion and transition metal co-doped diphase nanocrystalline composite glass microsphere laser resonant cavity prepared by the application has extremely high quality factor (more than or equal to 10) 5 ) And extremely small mode volumes (. Ltoreq.10) 3 μm 3 ) The interaction between the light and the substance can be enhanced by fully exerting the Peltier effect, and the simultaneous emission of the visible light with the wavelength of 450-700nm and the laser with the wavelength of 750-2000nm in the near infrared band can be realized under a single pumping light source.
In order to achieve the above purpose, the application adopts the following technical scheme:
in a first aspect of the present application, a method for implementing visible and near infrared integrated laser emission under a single pump is provided, where the method is: the double-phase nanocrystalline composite glass microsphere co-doped with transition metal ions and rare earth ions is used as a laser, and the laser of visible light and near infrared wave bands is emitted simultaneously under 980nm semiconductor laser pumping;
the double-phase nanocrystalline composite glass microsphere co-doped with transition metal ions and rare earth ions comprises a glass matrix and a luminescence center; the glass matrix comprises a glass network former, a glass network intermediate, and a crystal source; the luminescent center comprises rare earth ions and transition metal ions;
the wavelength of the visible light is 450-700nm; the wavelength of the near infrared band is 750-2000nm.
Preferably, the glass network former is silicate SiO 2 Or germanate GeO 2 The method comprises the steps of carrying out a first treatment on the surface of the The glass network intermediate is sodium oxide (Na 2 O), alumina(Al 2 O 3 ) At least one of zinc oxide (ZnO) and lithium fluoride (LiF); the crystal source is gallium oxide (Ga 2 O 3 ) Yttrium Fluoride (YF) 3 ) Lanthanum fluoride (LaF) 3 ) At least one of (a) and (b); the rare earth ion is erbium fluoride (ErF) 3 ) Thulium fluoride (TmF) 3 ) Ytterbium fluoride (YbF) 3 ) Holmium fluoride (HoF) 3 ) Neodymium fluoride (NdF) 3 ) At least one of (a) and (b); the transition metal ion is nickel oxide (NiO), chromium oxide (Cr 2 O 3 ) At least one of manganese oxide (MnO).
Preferably, the biphase nanocrystalline composite glass microsphere laser is prepared by the following method:
(1) Mixing a glass network former, a glass network intermediate, and a crystal source as a glass matrix; taking rare earth ions and transition metal ions as luminous centers, and uniformly ball-milling a glass substrate and the luminous centers to obtain a glass batch; melting the glass batch to obtain molten liquid, pouring the molten liquid onto a die, quenching the molten liquid to form glass, and annealing the glass to obtain bulk glass;
(2) Grinding the bulk glass obtained in the step (1) into glass powder, melting the glass powder, and forming glass microspheres with smooth surfaces under the action of surface tension after the glass powder is melted;
(3) And (3) performing heat treatment on the glass microspheres obtained in the step (2) to obtain the rare earth ion and transition metal co-doped biphasic nanocrystalline composite glass microsphere laser.
Preferably, in the step (1), the molar ratio of the glass network former, the glass network intermediate and the crystal source is (50-60): (10-15): (10-20); the molar quantity of the luminescent center doped is 0.1-1.5% of the total molar quantity of the glass matrix.
The amount of the luminescent center added is 0.1 to 1.5% of the sum of the molar amounts of the glass network former, the glass network intermediate and the crystal source.
Preferably, in the step (1), the ball milling time is 10-30 mins; the melting temperature is 1200-1600 ℃, and the melting time is 20-40mins; the annealing temperature is 400-500 ℃, and the annealing time is 3-5h.
Annealing at this temperature, on the one hand, eliminates internal glass stresses and, on the other hand, the annealing temperature is lower than the precipitation temperature of the crystals, ensuring that nanocrystals do not precipitate during this step.
Preferably, in the step (2), the particle size of the glass powder is 0.1-0.3mm; the melting is to lead the glass powder into the furnace body for melting after being fully atomized and dispersed from the upper charging hole of the vertical tube furnace.
Preferably, the melting temperature is 1100-1500 ℃, the charging air pressure in the melting process is 1.0Pa, and the negative pressure of the collecting system is 1.2Pa.
The furnace charging air pressure in the melting process is set to be 1.5Pa, so that the residence time of the glass powder in the furnace is prolonged, the glass powder can be ensured to be fully melted, and the glass powder can form glass microspheres with smooth surfaces under the action of the surface tension of a melt. The negative pressure is arranged in the collecting system to reduce the impact force when the glass microspheres fall down, so that the damage to the glass microspheres is avoided. According to the application, by strictly controlling the charging air pressure to be 1.0Pa, the negative pressure of the collecting system to be 1.2Pa and the charging air pressure in the furnace to be 1.5Pa in the melting process, two kinds of nanocrystals which are uniformly distributed in the micron-sized glass microspheres can be formed simultaneously by adopting the strict microsphere preparation conditions.
Preferably, in the step (3), the temperature of the heat treatment is 650-750 ℃, the time of the heat treatment is 5-15h, the heating rate during the heat treatment is 5-10 ℃/min, and the cooling rate after the heat treatment is 3-5 ℃/min.
By heat-treating the prepared glass microspheres under specific temperature conditions, desired nanocrystals can be formed within the glass microspheres. However, due to the smaller size of the glass microspheres, the control requirements for annealing conditions are higher than for bulk glass.
Preferably, the diameter of the biphase nanocrystalline composite glass microsphere laser is 20-200 mu m.
In a second aspect of the application, there is provided the use of a dual phase nanocrystalline composite glass microsphere co-doped with a transition metal ion and a rare earth ion in at least one of the following 1) to 3):
(1) As a low-threshold, wide-broadband multi-wavelength miniature integrated laser source;
(2) As a multi-wavelength display light source;
(3) And preparing an ultrasensitive sensor.
The application has the beneficial effects that:
(1) The glass microsphere prepared by the application can separate out two kinds of nanocrystals in the nanocrystal composite glass microsphere cavity at the same time, and provide excellent crystal field coordination environments for rare earth ions and transition metal ions respectively, so that the laser of visible light 450-700nm and near infrared band 750-2000nm can be emitted at the same time under a single pumping light source. The near infrared band is the widest laser emission report known to date. The method can be used in fields of low-threshold, wide-broadband multi-wavelength miniature integrated laser light sources in photonic chips (integrated optical circuits), multi-wavelength display light sources in three-dimensional stereoscopic display, ultra-sensitive sensing detection sensor preparation and the like.
(2) Compared with the existing nano-crystal composite glass microsphere cavity doped with more rare earth ions, the dual-phase nano-crystal composite glass microsphere laser co-doped with rare earth ions and transition metal prepared by the application has wider laser emission peak and lower threshold. As in Er 3+ : the threshold of the laser with the wavelength of about 1.53 mu m is 282 mu W, which is higher than E reported earlier r3+ Doped NaYF-containing 4 The laser threshold of the single-phase nanocrystalline composite glass microsphere is reduced by 1.24 times when the wavelength of the single-phase nanocrystalline composite glass microsphere is approximately 1.557 mu m and is 350 mu W.
Drawings
FIG. 1 is a schematic diagram of a laser test path of a continuous optical pumping tapered fiber coupled microsphere used in the present application;
FIG. 2 is Ni with a diameter of 24 μm prepared in comparative example 1 2+ /Yb 3+ /Er 3+ /Tm 3+ The co-doped matrix glass microsphere (a) and the biphase nanocrystalline composite glass microsphere (b) prepared in the embodiment are subjected to physical photographs under 980nm pumping;
FIG. 3 is Ni prepared in comparative example 1 2+ /Yb 3+ /Er 3+ /Tm 3+ Co-doped 25 μm matrix glass microsphere (a) and dual-phase nanocrystalline composite glass prepared in 28 μm exampleThe quality factor Q value test result of the glass microsphere product (b);
FIG. 4 is a graph showing different Ni sizes prepared in comparative example 1 2+ /Yb 3+ /Er 3+ /Tm 3+ The co-doped matrix glass microsphere and the biphase nanocrystalline composite glass microsphere prepared in the embodiment have laser output spectrum under 500 mu W pumping of a semiconductor laser with wavelength of 980nm, and threshold and slope efficiency of corresponding wave bands: (a) the diameter of the matrix glass microsphere of the comparative example 1 is 25 μm, the diameter of the composite glass microsphere of the embodiment biphasic nanocrystalline is 28 μm, (b) the diameter of the matrix glass microsphere of the comparative example 1 is 62 μm, the diameter of the composite glass microsphere of the embodiment biphasic nanocrystalline is 58 μm, (c) the diameter of the matrix glass microsphere of the comparative example 1 is 105 μm, and the diameter of the composite glass microsphere of the embodiment biphasic nanocrystalline is 102 μm;
FIG. 5 is 24 μm Ni prepared in comparative example 4 2+ The quality factor Q value test results of the single-doped matrix glass microsphere (a) and the 27 mu m biphase nanocrystalline composite glass microsphere product (b) prepared in comparative example 5;
FIG. 6 is 27 μm Ni prepared in comparative example 5 2+ The single-doped biphase nanocrystalline composite glass microsphere outputs laser spectrum under 500 mu W pumping of a semiconductor laser with wavelength of 980nm, and the threshold value and slope efficiency of corresponding wave bands.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As described in the background section, the size of the crystal grains which can be precipitated in the nanocrystalline composite glass is generally tens of nanometers and is far smaller than the wavelength of visible light so as to avoid scattering, so that the nanocrystalline composite glass can still keep good light transmittance and lower loss. Therefore, the transition metal ion doped nanocrystalline composite glass combines the advantages of the crystal and the glass, simultaneously eliminates the defects of the crystal and the glass, and can be used as a gain matrix material of a near infrared ultra-wideband light source. There are reports (e.g. research progress of doped diphase nanocrystalline composite photon glass, gao Zhigang, et al, month 8 of 2021, laser)With optoelectronics development, volume 58, phase 15) mentions that co-doping of rare earth and transition metal ions in a dual-phase nanocrystalline composite glass, which is Au/gamma-Ga, is capable of retaining the respective luminescence characteristics 2 O 3 The biphase nanocrystalline composite glass realizes optical amplification in 1310nm wave band of optical fiber communication after rare earth and transition metal ions are co-doped. The nanocrystalline composite bulk glass is of an open structure, the light field binding capability of the nanocrystalline composite bulk glass is still limited, and laser emission in the double-phase nanocrystalline composite glass co-doped with rare earth ions and transition metal ions is not realized until now.
Based on the above, the application aims to provide a dual-phase nanocrystalline composite glass microsphere laser integrating visible light and near infrared light under a single pump. By preparing the double-phase nanocrystalline composite glass microsphere co-doped with the transition metal ions and the rare earth ions, two kinds of nanocrystals are simultaneously separated out from the nanocrystalline composite glass microsphere cavity, excellent crystal field coordination environments are respectively provided for the rare earth ions and the transition metal ions, and the laser simultaneous emission of the visible light 450-700nm and the near infrared band 750-2000nm can be realized under a single pumping light source. Compared with the existing nano-crystal composite glass microsphere cavity doped with more rare earth ions, the dual-phase nano-crystal composite glass microsphere laser co-doped with rare earth ions and transition metal prepared by the application has wider laser emission peak and lower threshold. As in Er 3+ : the threshold of the laser with the wavelength of about 1.53 mu m is 282 mu W, which is higher than E reported earlier r3+ Doped NaYF-containing 4 The laser threshold of the single-phase nanocrystalline composite glass microsphere is reduced by 1.24 times when the wavelength of the single-phase nanocrystalline composite glass microsphere is approximately 1.557 mu m and is 350 mu W. Glass microsphere based on whispering gallery mode (Whispering Gallery Mode, WGM) can utilize total reflection principle to restrict light in micrometer-level cavity for a long time, so that it has extremely high quality factor (not less than 10) 5 ) And extremely small mode volumes (. Ltoreq.10) 3 μm 3 ) The interaction between light and substances can be enhanced by fully utilizing the Peltier effect. The luminescent ions are introduced into the microsphere to have gain and feedback, so that the WGM microsphere laser is formed, and the laser threshold is far lower than that of the traditional semiconductor and fiber lasers, and reaches the micro-watt or hundred-nano-watt level.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present application, the technical scheme of the present application will be described in detail with reference to specific embodiments.
The test materials used in the examples of the present application are all conventional in the art and are commercially available.
Examples
Preparation of 45SiO 2 -10Al 2 O 3 -15Ga 2 O 3 -10ZnO-15YF 3 -5LiF-0.15NiO-0.5YbF 3 -0.2TmF 3 -0.2ErF 3 (mol.%) rare earth ion co-doped biphasic nanocrystalline composite glass microspheres:
the glass network forming body is SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the The intermediate of the glass network is Al 2 O 3 ZnO and LiF; the crystal source is Ga 2 O 3 、YF 3 The transition metal ion is NiO, and the rare earth ion is YbF 3 、TmF 3 、ErF 3 。
The preceding values for each compound represent the mole percent incorporated (mol.%) relative to the entire glass matrix.
The preparation method comprises the following steps:
the compound is prepared into a mixture according to the stoichiometric ratio, and the mixture is ball-milled and mixed for 20mins, so that the raw materials are uniformly mixed; transferring the uniformly mixed raw materials into a corundum crucible, and covering to reduce volatilization of the high-temperature melting raw materials, wherein the melting temperature is 1540 ℃ and the melting time is 25mins, so as to obtain a molten liquid; pouring the molten liquid on a copper plate which is heated at 200 ℃ in advance for quenching to form glass; and (3) annealing the glass at 500 ℃ for 3 hours to obtain the initial bulk glass.
Grinding the prepared bulk glass, and screening and filtering the ground powder sample by using a pore-size sieve with the size of 0.15 mm; the screened powder sample is fully atomized and dispersed in the upper feed inlet of the vertical tube furnace and then is introduced into the furnace body, and the temperature range of the tube furnace is 1480 ℃; in the melting process, nitrogen is introduced to form charging air pressure which is set to be 1.0Pa, so that the residence time of the glass powder in the furnace is prolonged, the glass powder can be fully melted, and the glass powder is enabled to be fully meltedForming glass microspheres with smooth surfaces under the action of melt surface tension; the negative pressure of the collecting system is set to be 1.2Pa, so that the impact force of the glass microspheres in falling is reduced, and the damage to the glass microspheres is avoided; placing the prepared glass microspheres in a culture dish, transferring the culture dish into a precise furnace for heat treatment, wherein the heat treatment speed is 5 ℃/min, heating to 740 ℃, keeping for 12 hours, then cooling to room temperature at 10 ℃/min, and finally preparing the transition metal Ni 2+ With rare earth ion Er 3+ 、Yb 3+ 、Tm 3+ Co-doped gamma-Ga containing 2 O 3 And beta-YF 3 Is a double-phase nanocrystalline composite glass microsphere.
Comparative example 1
Ni 2+ /Yb 3+ /Er 3+ /Tm 3+ Preparation of co-doped matrix glass microspheres: the same raw material proportion and the same preparation method as those of the example are different in that after the glass microspheres are obtained by melting, the glass microspheres are not subjected to heat treatment at 740 ℃.
Comparative example 2
Preparing matrix glass microspheres without adding transition metal ions and rare earth ions:
the raw materials are as follows: 45SiO 2 -10Al 2 O 3 -15Ga 2 O 3 -10ZnO-15YF 3 -5LiF(mol.％)；
The preparation method is the same as the example, except that after the glass microspheres are melted, the glass microspheres are not subjected to heat treatment at 740 ℃.
Comparative example 3:
according to the preparation method of the embodiment, no transition metal ion and rare earth ion are added to prepare 45SiO 2 -10Al 2 O 3 -15Ga 2 O 3 -10ZnO-15YF 3 -5LiF (mol.%) biphasic nanocrystalline composite glass microsphere.
Comparative example 4:
preparing matrix glass microspheres without adding rare earth ions: the raw materials are as follows: 45SiO 2 -10Al 2 O 3 -15Ga 2 O 3 -10ZnO-15YF 3 -5LiF-0.15NiO (mol.%) identical to the preparation of the examples, except that: melting to obtain glassAfter the microspheres, the glass microspheres were not subjected to a heat treatment at 740 ℃.
Comparative example 5
According to the preparation method of the example, no rare earth ion is added to prepare 45SiO 2 -10Al 2 O 3 -15Ga 2 O 3 -10ZnO-15YF 3 -5LiF-0.15NiO (mol.%) rare earth ion doped biphasic nanocrystalline composite glass microspheres.
Comparative example 6
According to the preparation method of the example, 45SiO is prepared without adding transition metal ions 2 -10Al 2 O 3 -15Ga 2 O 3 -10ZnO-15YF 3 -5LiF-0.5YbF 3 -0.2TmF 3 -0.2ErF 3 (mol%) rare earth ion doped biphasic nanocrystalline composite glass microsphere.
Test examples
A narrow linewidth tunable laser is used as a light source, and tapered quartz fiber waveguides with different diameters are prepared through a fiber tapering system to excite and couple WGM laser. During coupling, the microsphere is slowly close to the tapered optical fiber under the precise three-dimensional displacement platform, the equatorial plane of the microsphere cavity is parallel to the tapered optical fiber, and the two are adjusted to a critical coupling state by adjusting the distance between the tapered optical fiber and the microcavity. The WGM resonance signal is measured by a photodetector and an oscilloscope connected thereto. In the process, the scanning frequency of the tunable laser is determined by parameters set by the oscilloscope, and finally the obtained time domain spectrum signal is converted into a corresponding frequency domain spectrum. And researching the change of the quality factor of the microsphere according to the change of the half-width of the resonance peak of the transmission curve. The tunable laser is replaced by a corresponding pump laser, so that the laser performance test can be completed by using the same light path; see fig. 1.
Ni with diameter of 25 μm 2+ /Yb 3+ /Er 3+ /Tm 3+ The physical photographs of the co-doped matrix glass microspheres and the biphase nanocrystalline composite glass microspheres prepared in the embodiment with the diameter of 28 μm under 980nm pumping are shown in figure 2, and the matrix glass and the biphase nanocrystalline composite glass prepared in the embodiment under 980nm semiconductor laser pumping show red, blue and green three primary color compositeWhite light is emitted, and after the nano-crystals are separated out, the luminous intensity can be obviously enhanced by naked eyes;
comparative example 1 Ni prepared 2+ /Yb 3+ /Er 3+ /Tm 3+ The test results of the Q value of the quality factors of the co-doped matrix glass microspheres and the biphasic nanocrystalline composite glass microspheres prepared by the 28 μm example are shown in figure 3, and the quality factor of the biphasic nanocrystalline composite glass microspheres prepared by the example after nanocrystalline precipitation is reduced, but still kept at 10 5 High quality factors.
Comparative example 1 different size Ni prepared 2+ /Yb 3+ /Er 3+ /Tm 3+ The laser output spectrum of the co-doped matrix glass microsphere and the biphasic nanocrystalline composite glass microsphere prepared in the embodiment under 500 mu W pumping of the semiconductor laser with the wavelength of 980nm and the threshold value and slope efficiency of the corresponding wave band are shown in figure 4: the laser output efficiency of rare earth ions in the biphasic nanocrystalline composite glass microsphere prepared in the example is higher than that of Ni prepared in comparative example 1 2+ /Yb 3+ /Er 3+ /Tm 3+ Co-doped matrix glass microspheres are significantly improved and benefit from gamma-Ga 2 O 3 Precipitation of nanocrystals, transition metal Ni was detected in the biphasic nanocrystalline composite glass microspheres prepared in the examples 2+ Laser emission in the 1050-1450nm band, while Ni prepared in comparative example 1 2+ /Yb 3+ /Er 3+ /Tm 3+ No laser was detected in the co-doped matrix glass microspheres at this band.
The quality factor Q value of the matrix glass microsphere prepared in comparative example 2 and without adding transition metal ions and rare earth ions is 8.65X10 5 1576.24nm; the quality factor Q value of the biphase nanocrystalline composite glass microsphere prepared in comparative example 3 is 6.97X10 5 @1569.38nm. From the results, it can be seen that the quality factor Q value of the matrix glass microsphere prepared in comparative example 2 and the nanocrystalline composite glass microsphere prepared in comparative example 3, which are not added with transition metal ions and rare earth ions, is improved compared with that of the matrix glass microsphere prepared in comparative example 1 and the nanocrystalline composite glass microsphere prepared in the examples, which are added with luminescent centers. However, the matrix glass prepared in comparative example 2 without addition of transition metal ions and rare earth ionsIn the laser performance test process of the glass microsphere and the nanocrystalline composite glass microsphere prepared in comparative example 3, no laser emission is detected in the visible light and near infrared light bands.
Ni prepared in comparative example 4 having a diameter of 24. Mu.m 2+ The test results of the quality factor Q values of the single-doped matrix glass microspheres and the biphase nanocrystalline composite glass microspheres prepared in comparative example 5 with the diameter of 27 μm are shown in FIG. 5, and it can be seen from the results that only transition metal Ni is added in the preparation of comparative example 4 2+ The quality factor Q value of the ionic matrix glass microsphere and the nanocrystalline composite glass microsphere prepared in comparative example 5 is slightly improved compared with that of the transition metal ion and rare earth ion co-doped matrix glass microsphere prepared in comparative example 1 and nanocrystalline composite glass microsphere prepared in the example, but the quality factor Q value is kept at 10 5 The order of the high quality factor is shown in figure 3.
Ni prepared in proportion 4 with diameter of 24 μm 2+ The laser output spectrum of the single doped matrix glass microsphere and the dual-phase nanocrystalline composite glass microsphere prepared in comparative example 5 with the diameter of 27 μm under 500 mu W pumping of a semiconductor laser with the wavelength of 980nm and the threshold and slope efficiency of the corresponding wave band are shown in FIG. 6: in the matrix glass microsphere prepared in comparative example 4, we did not detect Ni in the near infrared band due to lack of suitable crystal field environment due to lack of any precipitation of nanocrystals 2+ And (5) laser emission. Benefit from gamma-Ga in the biphasic nanocrystalline composite glass microsphere prepared in comparative example 5 2 O 3 Precipitation of nanocrystalline, transition metal Ni can be detected 2+ Laser emission in the 1150-1450nm band. FIG. 4 shows the rare earth ion and transition metal Ni prepared in the example 2+ Compared with the laser emission spectrum of the ion co-doped nanocrystalline composite glass microsphere, the Ni prepared in comparative example 4 2+ The single doped matrix glass microsphere can not be detected by lasers in the visible light 450-700nm and the near infrared bands 750-1150nm and 1450-2000 nm. At the same time, the same size rare earth ion and transition metal Ni in comparative example 2+ Ion co-doped nanocrystalline composite glass microspheres (FIG. 4 a), ni with diameter of 27 μm prepared in comparative example 5 2+ The laser threshold of the single-doped diphase nanocrystalline composite glass microsphere is improved, the slope efficiency is reduced, and the laser is totalThe body performance is significantly reduced.
The quality factor Q value of the rare earth ion doped biphase nanocrystalline composite glass microsphere prepared in comparative example 6 is also kept at 10 5 This order of magnitude, but no laser emission in the near infrared band of 1150-1450nm was detected.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. The method for realizing visible and near infrared integrated laser emission under single pumping is characterized by comprising the following steps of: the double-phase nanocrystalline composite glass microsphere co-doped with transition metal ions and rare earth ions is used as a laser, and the laser of visible light and near infrared wave bands is emitted simultaneously under the single pumping of 980nm semiconductor laser;
the double-phase nanocrystalline composite glass microsphere co-doped with transition metal ions and rare earth ions comprises a glass matrix and a luminescence center; the glass matrix comprises a glass network former, a glass network intermediate, and a crystal source; the luminescent center comprises rare earth ions and transition metal ions;
the wavelength of the visible light is 450-700nm; the wavelength of the near infrared band is 750-2000nm.
2. The laser emission method according to claim 1, wherein the glass network former is silicate or germanate; the glass network intermediate is at least one of sodium oxide, aluminum oxide, zinc oxide and lithium fluoride; the crystal source is at least one of gallium oxide, yttrium fluoride and lanthanum fluoride; the rare earth ions are at least one of erbium fluoride, thulium fluoride, ytterbium fluoride, holmium fluoride and neodymium fluoride; the transition metal ion is at least one of nickel oxide, chromium oxide and manganese oxide.
3. The laser emission method according to claim 1, wherein the dual-phase nanocrystalline composite glass microsphere laser is prepared by the following method:
(1) Mixing a glass network former, a glass network intermediate, and a crystal source as a glass matrix; taking rare earth ions and transition metal ions as luminous centers, and uniformly ball-milling a glass substrate and the luminous centers to obtain a glass batch; melting the glass batch to obtain molten liquid, pouring the molten liquid onto a die, quenching the molten liquid to form glass, and annealing the glass to obtain bulk glass;
(2) Grinding the bulk glass obtained in the step (1) into glass powder, melting the glass powder, and forming glass microspheres with smooth surfaces under the action of surface tension after the glass powder is melted;
(3) And (3) performing heat treatment on the glass microspheres obtained in the step (2) to obtain the rare earth ion and transition metal co-doped biphasic nanocrystalline composite glass microsphere laser.
4. The method of claim 3, wherein in step (1), the molar ratio of the glass network former, the glass network intermediate, and the crystal source is (50-60): (10-15): (10-20); the molar quantity of the luminescent center doped is 0.1-1.5% of the total molar quantity of the glass matrix.
5. The method of claim 3, wherein in step (1), the ball milling time is 10 to 30 minutes; the melting temperature is 1200-1600 ℃, and the melting time is 20-40mins; the annealing temperature is 400-500 ℃, and the annealing time is 3-5h.
6. The laser light emitting method according to claim 3, wherein in the step (2), the particle diameter of the glass powder is 0.1 to 0.3mm; the melting is to lead the glass powder into the furnace body for melting after being fully atomized and dispersed from the upper charging hole of the vertical tube furnace.
7. The laser emission method according to claim 6, wherein the melting temperature is 1100-1500 ℃, the charging air pressure during melting is 1.0Pa, and the negative pressure of the collecting system is 1.2Pa.
8. The laser emission method as claimed in claim 3, wherein in the step (3), the temperature of the heat treatment is 650-750 ℃, the time of the heat treatment is 5-15 hours, the heating rate of the heat treatment is 5-10 ℃/min, and the cooling rate of the heat treatment is 3-5 ℃/min.
9. The laser emitting method according to claim 1, wherein the diameter of the dual-phase nanocrystalline composite glass microsphere laser is 20-200 μm.
10. Use of the biphasic nanocrystalline composite glass microsphere co-doped with a transition metal ion and a rare earth ion according to any one of claims 1 to 9 in at least one of the following 1) to 3):
(1) As a low-threshold ultra-wideband multi-wavelength miniature integrated laser source;
(2) As a multi-wavelength display light source;
(3) And preparing an ultrasensitive sensor.
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| CN113087397A (en) * | 2021-04-13 | 2021-07-09 | 泰山学院 | Double-phase transparent glass ceramic with ultra-wideband fluorescence emission characteristic and preparation method thereof |
| CN115189211A (en) * | 2022-07-15 | 2022-10-14 | 泰山学院 | Nickel-doped transparent microcrystalline glass microsphere laser with O-band laser emission performance |
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| CN113087397A (en) * | 2021-04-13 | 2021-07-09 | 泰山学院 | Double-phase transparent glass ceramic with ultra-wideband fluorescence emission characteristic and preparation method thereof |
| CN115189211A (en) * | 2022-07-15 | 2022-10-14 | 泰山学院 | Nickel-doped transparent microcrystalline glass microsphere laser with O-band laser emission performance |
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| ZHIGANG GAO等: "Transmission electron microscopic and optical spectroscopic studies of Ni2+/Yb3+/Er3+/Tm3+ doped dual-phase glass-ceramics", 《J AM CERAM SOC.》, vol. 101, pages 2868 - 2876 * |
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