CN108265330A - A kind of double-doped yttrium aluminate novel near-infrared laser crystal of bismuth potassium and preparation method thereof - Google Patents
A kind of double-doped yttrium aluminate novel near-infrared laser crystal of bismuth potassium and preparation method thereof Download PDFInfo
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- CN108265330A CN108265330A CN201810057892.7A CN201810057892A CN108265330A CN 108265330 A CN108265330 A CN 108265330A CN 201810057892 A CN201810057892 A CN 201810057892A CN 108265330 A CN108265330 A CN 108265330A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/24—Complex oxides with formula AMeO3, wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. ortho ferrites
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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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
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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
- H01S3/163—Solid materials characterised by a crystal matrix
- H01S3/1631—Solid materials characterised by a crystal matrix aluminate
- H01S3/1638—YAlO3 (YALO or YAP, Yttrium Aluminium Perovskite)
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Abstract
The invention discloses double-doped yttrium aluminate novel near-infrared laser crystal of a kind of bismuth potassium and preparation method thereof, belong to near-infrared laser gain material field, wherein, bismuth ion and potassium ion are mixed in the double-doped yttrium aluminate crystal of bismuth potassium simultaneously, wherein the incorporation of bismuth ion is 0.1~15at.%, and the amount of participating in of potassium ion is 0.1~15at.%.The double-doped crystal of bismuth potassium of the present invention, bismuth ion is as active ions, and potassium ion ion as an optimization, can provide the compensating action of partial charge, the Bi that bismuth potassium easily appraises at the current rate when double-doped3+It will obtain relative to singly mixing Bi3+When obtain more electronics, the bismuth ion of more lower valencies is formed, while improve the segregation coefficient of bismuth ion, so as to effectively improve the near-infrared luminous efficiency of bismuth ion.It realizes enhancing fluorescence output, reduce laser threshold and improves lasing efficiency.The laser crystal has important application prospect in fields such as military, medical treatment, scientific research and communications.
Description
Technical field
The present invention relates to near-infrared laser gain material technical fields, and in particular to a kind of double-doped yttrium aluminate novel of bismuth potassium is near
Infrared laser crystal and preparation method thereof.
Background technology
Near infrared band laser is in optic communication, ultrafast photonic propulsion, laser radar, remote sensing, photoelectronic warfare, medical treatment, section
Grind, etc. fields be with a wide range of applications.Japanese scholars Fujimoto in 2001 et al. reports bismuth doped-glass for the first time
After near-infrared super-broadband emission, bismuth ion becomes one of effective ion of near-infrared ultra wide wave band laser output.Bismuth ion not only has
There is a broad-band illumination of near infrared band, the also broad-band illumination with middle infrared band, and half-peak breadth is wider, fluorescence lifetime length etc. is excellent
It puts and is concerned.
It is concentrated mainly in glass optical fiber matrix about the research of bismuth ion both at home and abroad at present, is mainly used in fiber optic communication
Field, and the research in laser crystal material is considerably less, and it is low, luminous to be primarily due to bismuth ion near-infrared fluorescent emission effciency
The weak problems such as low with segregation coefficient.Moreover, bismuth ion has the emission spectrum of signature unlike rare earth ion, shine
By many factors, such as covalent bond, coordination environment, lattice symmetry and acid-base value influence.The origin one of bismuth ion infraluminescence
It does not come to a conclusion directly, the reason is that the valence state of bismuth ion is complicated, can be Bi0、Bi+1、Bi+2、Bi+3、Bi+4And Bi+5, and bismuth ion can
To form a series of cluster.Recent domestic to bismuth ion near-infrared super-broadband emission research shows that, in near-infrared luminous
The heart is the bismuth ion of lower valency, how to obtain the bismuth ion of lower valency, and it is allowed to be stabilized, is the research for mixing bismuth luminescent material
Emphasis.
Therefore the research double-doped yttrium aluminate near-infrared laser crystalline material of bismuth potassium has weight to the output of near-infrared wide spectrum laser
Want meaning.At present, at home and abroad there is no the relevant reports about the double-doped yttrium aluminate crystal of bismuth potassium.
Invention content
The purpose of the present invention is to solve drawbacks described above of the prior art, provide a kind of double-doped yttrium aluminate novel of bismuth potassium
Near-infrared laser crystal and preparation method thereof.
According to disclosed embodiment, the first aspect of the present invention proposes a kind of double-doped yttrium aluminate novel near-infrared of bismuth potassium and swashs
Luminescent crystal, the near-infrared laser crystal include crystal substrate, bismuth ion and potassium ion, and the crystal substrate is yttrium aluminate
Crystal, to mix the yttrium aluminate simultaneously brilliant for ion as an optimization as active ions and the potassium ion for the bismuth ion
In body.
Further, the molecular formula of the double-doped yttrium aluminate near-infrared laser crystal of the bismuth potassium is Bi/K:YAlO3, skeleton symbol
For：Bi/K:YAP.
Further, the doping concentration of the bismuth ion ranging from 0.1~15at.%, the doping of the potassium ion
Concentration range is 0.1~15at.%.
Further, the near-infrared laser crystal is used to implement 900nm~1700nm band broadband all-solid state lasers
Output.
According to disclosed embodiment, the second aspect of the present invention proposes a kind of double-doped yttrium aluminate novel near-infrared of bismuth potassium and swashs
The preparation method of luminescent crystal, the preparation method include the following steps：
S1, by purity be 99.999% Bi2O3、K2CO3、Y2O3And Al2O3As raw material, during dispensing [Y] and [Al] mole
Than being 1:1, the incorporation of bismuth ion is 0.1~15at.%, and the amount of participating in of potassium ion is 0.1~15at.%, and raw material is mixed through grinding
Briquetting sintering after uniformly；
S2, the raw material sintered is fitted into iridium crucible, is replaced in single crystal growing furnace completely with high pure nitrogen or inert gas
Air, crystal oven is warming up to 1850~2050 DEG C, and crystal pull speed is 0.5~1.5mm/h, and rotating speed is 6~16r/min；
After S3, crystal growth, need slowly to cool down near growth temperature, 40~50 DEG C/h of falling temperature gradient.
Further, the step S1 processes are as follows：
By the Bi that purity is 99.99%2O3、K2CO3、Y2O3And Al2O3It matches and mixes according to materials, then in batch mixer
Mix 5~20 hours；
Raw material is pressed into columned material cake under the pressure of 1-5Gpa；
Material cake is put into Muffle furnace, 5~10 hours are warming up to 1000~1200 DEG C, small in the sintering 20~30 of this temperature
When, room temperature is down to 10~15 hours, makes batch mixing that solid phase reaction fully occur, you can obtains the double-doped yttrium aluminate crystal powder of bismuth potassium
Material.
Further, the step S2 processes are as follows：
Above-mentioned raw materials are put into Iridium Crucible, using Frequency Induction Heating, using YAP crystal as seed crystal；
It is grown using Czochralski czochralski methods along b axis or a axis directions, according to seeding, necking down, shouldering, isometrical, ending
Program growth the double-doped yttrium aluminate crystal of bismuth potassium.
Further, crystal cooling rate is 20~30 DEG C/h in the step S2.
Further, the step S3 processes are as follows：
It will obtain crystal to anneal in air, annealing temperature is 1100~1200 DEG C, and soaking time is 10~30 hours.
The present invention is had the following advantages relative to the prior art and effect：
Present invention firstly provides a kind of double-doped yttrium aluminate crystal of bismuth potassium and preparation methods.Bismuth ion is as active ions, potassium
Ion, potassium ion can provide the compensating action of partial charge, the Bi that bismuth potassium easily appraises at the current rate when double-doped in crystal to ion as an optimization3+
It will obtain relative to singly mixing Bi3+When obtain more electronics, form the bismuth ion of more lower valencies, it made to be stable in the presence of crystal
In, while the segregation coefficient of bismuth ion is improved, so as to which the laser for effectively improving bismuth ion activation near-infrared laser crystal exports effect
Rate.The crystal has important application prospect in fields such as communication, medical treatment, scientific research and military affairs.
Description of the drawings
Fig. 1 is a kind of double-doped yttrium aluminate novel near-infrared laser crystal preparation method of bismuth potassium disclosed by the invention.
Specific embodiment
Purpose, technical scheme and advantage to make the embodiment of the present invention are clearer, below in conjunction with the embodiment of the present invention
In attached drawing, the technical solution in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
Part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
All other embodiments obtained without making creative work shall fall within the protection scope of the present invention.
Embodiment one
Present embodiment discloses a kind of double-doped yttrium aluminate near-infrared laser crystal of bismuth potassium, bismuth ion can be allowed to stablize with lower valency
In the presence of, and effectively improve the segregation coefficient of bismuth ion.The crystal can realize near-infrared laser output, communication, medical treatment,
There is important application prospect in the fields such as scientific research and military affairs.
The yttrium aluminate near-infrared laser crystal, it is characterised in that bismuth ion and potassium ion are mixed simultaneously in yttrium aluminate crystal,
The bismuth ion is as active ions, potassium ion ion as an optimization, can provide the compensating action of partial charge, and bismuth potassium is double-doped
The Bi that Shi Yi appraises at the current rate3+It will obtain relative to singly mixing Bi3+When obtain more electronics, form the bismuth ion of more lower valencies, simultaneously
Improve segregation coefficient of the bismuth ion in crystal.
Bismuth ion and potassium ion mix laser crystal, molecular formula simultaneously in the double-doped yttrium aluminate near-infrared laser crystal of the bismuth potassium
For Bi/K:YAlO3, skeleton symbol is：Bi/K:YAP, doping concentration ranging from 0.1~15at.% of bismuth ion, the doping of potassium ion
Concentration range is 0.1~15at.%.
The laser crystal is used to implement the output of 900nm~1700nm band broadbands all-solid state laser.
Embodiment two
As shown in Figure 1, present embodiment discloses a kind of double-doped yttrium aluminate novel near-infrared laser crystal preparation sides of bismuth potassium
Method, the preparation method include the following steps：
By the Bi that purity is 99.999%2O3、K2CO3、Y2O3And Al2O3As raw material, [Y] and [Al] molar ratio during dispensing
It is 1:1, the incorporation of bismuth ion is 0.1~15at.%, and the amount of participating in of potassium ion is 0.1~15at.%, and raw material is mixed through grinding
Briquetting sintering after even；
The raw material sintered is fitted into iridium crucible, replaces the sky in single crystal growing furnace completely with high pure nitrogen or inert gas
Gas, crystal oven are warming up to 1850~2050 DEG C, and crystal pull speed is 0.5~1.5mm/h, and rotating speed is 6~16r/min；
After crystal growth, need slowly to cool down near growth temperature, 40~50 DEG C/h of falling temperature gradient.
Embodiment three
Present embodiment discloses the double-doped yttrium aluminate novel near-infrared laser crystal preparation method of another bismuth potassium, the preparation sides
Method includes the following steps：
By the Bi that purity is 99.99%2O3、K2CO3、Y2O3And Al2O3It matches and mixes according to materials, then in batch mixer
Mix 5~20 hours.
Raw material is pressed into columned material cake under the pressure of 1-5Gpa.
Material cake is put into Muffle furnace, 5~10 hours are warming up to 1000~1200 DEG C, small in the sintering 20~30 of this temperature
When, room temperature is down to 10~15 hours, makes batch mixing that solid phase reaction fully occur, you can obtains the double-doped yttrium aluminate crystal powder of bismuth potassium
Material.
Above-mentioned raw materials are put into Iridium Crucible, using Frequency Induction Heating, using YAP crystal as seed crystal.Using
Czochralski czochralski methods are grown along b axis or a axis directions, grow bismuth according to seeding, necking down, shouldering, isometrical, ending program
The double-doped yttrium aluminate crystal of potassium；Technological parameter is：0.5~1.5mm/h of pulling rate, rotating speed are：6~16r/min, crystal cooling rate are
20~30 DEG C/h.
It will obtain crystal to anneal in air, annealing temperature is 1100~1200 DEG C, and soaking time is 10~30 hours, is risen
Reduction of speed degree is 40~50 DEG C/h.
Example IV
The raw material Y that purity is selected to be more than 99.999% in the present embodiment2O3、Al2O3、Bi2O3And K2CO3, use
Czochralski czochralski methods carry out crystal growth, wherein the doping concentration of bismuth ion be 0.1at.%, the doping concentration of potassium ion
For 0.1at.%.The good raw material mixed grinding of precise is uniform, after tabletting, it is put into 80 × 100mm of Ф3Corundum do pot
In, in 10 hours of 1200 DEG C of solid phase reactions in Muffle furnace.Synthetic sample is put into 60 × 40mm of Ф3Platinum crucible
In, the pulling single crystal in nitrogen atmosphere, crystal rotation 12r/min, pulling rate 1.2mm/h.Successful growth size is Ф 25
×35mm3High quality the double-doped yttrium aluminate near-infrared laser crystal of bismuth potassium.
Embodiment five
The raw material Y that purity is selected to be more than 99.999% in the present embodiment2O3、Al2O3、Bi2O3And K2CO3, use
Czochralski czochralski methods carry out crystal growth, wherein the doping concentration of bismuth ion be 1.50at.mol%, the doping of potassium ion
A concentration of 2.00at.%.The good raw material mixed grinding of precise is uniform, after tabletting, it is put into 100 × 100mm of Ф3Corundum
In dry pot, in 8 hours of 1100 DEG C of solid phase reactions in Muffle furnace.Synthetic sample is put into 60 × 40mm of Ф3Platinum
In crucible, the pulling single crystal in nitrogen atmosphere, crystal rotation 14r/min, pulling rate 1.1mm/h.Successful growth size is
Ф30×35mm3High quality the double-doped yttrium aluminate near-infrared laser crystal of bismuth potassium.
Embodiment six
The raw material Y that purity is selected to be more than 99.999% in the present embodiment2O3、Al2O3、Bi2O3And K2CO3, use
Czochralski czochralski methods carry out crystal growth, and the wherein doping concentration of bismuth ion is 15.00at.mol%, and potassium ion is mixed
Miscellaneous a concentration of 1.00at.%.The good raw material mixed grinding of precise is uniform, after tabletting, it is put into 100 × 100mm of Ф3It is firm
In beautiful dry pot, in 9 hours of 1150 DEG C of solid phase reactions in Muffle furnace.Synthetic sample is put into 60 × 40mm of Ф3Platinum
In golden crucible, the pulling single crystal in nitrogen atmosphere, crystal rotation 13r/min, pulling rate 1.0mm/h.Successful growth size
For 28 × 35mm of Ф3High quality the double-doped yttrium aluminate near-infrared laser crystal of bismuth potassium.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
- A kind of 1. double-doped yttrium aluminate novel near-infrared laser crystal of bismuth potassium, which is characterized in that the near-infrared laser crystal packet Crystal substrate, bismuth ion and potassium ion are included, the crystal substrate is yttrium aluminate crystal, and the bismuth ion is as active ions Ion is mixed in the yttrium aluminate crystal simultaneously as an optimization with the potassium ion.
- 2. a kind of double-doped yttrium aluminate novel near-infrared laser crystal of bismuth potassium according to claim 1, which is characterized in thatThe molecular formula of the double-doped yttrium aluminate near-infrared laser crystal of the bismuth potassium is Bi/K:YAlO3, skeleton symbol is：Bi/K:YAP.
- 3. the double-doped yttrium aluminate novel near-infrared laser crystal of a kind of bismuth potassium according to claim 1, which is characterized in that described Bismuth ion doping concentration ranging from 0.1~15at.%, the doping concentration ranging from 0.1 of the potassium ion~ 15at.%.
- 4. the double-doped yttrium aluminate novel near-infrared laser crystal of a kind of bismuth potassium according to claim 1, which is characterized in that described Near-infrared laser crystal be used to implement 900nm~1700nm band broadbands all-solid state laser output.
- A kind of 5. preparation method of the double-doped yttrium aluminate novel near-infrared laser crystal of bismuth potassium, which is characterized in that the preparation side Method includes the following steps：S1, by purity be 99.999% Bi2O3、K2CO3、Y2O3And Al2O3As raw material, [Y] and [Al] molar ratio is during dispensing 1:1, the incorporation of bismuth ion is 0.1~15at.%, and the amount of participating in of potassium ion is 0.1~15at.%, raw material through grind be mixed it is even Briquetting is sintered afterwards；S2, the raw material sintered is fitted into iridium crucible, replaces the sky in single crystal growing furnace completely with high pure nitrogen or inert gas Gas, crystal oven are warming up to 1850~2050 DEG C, and crystal pull speed is 0.5~1.5mm/h, and rotating speed is 6~16r/min；After S3, crystal growth, need slowly to cool down near growth temperature, 40~50 DEG C/h of falling temperature gradient.
- 6. a kind of preparation method of the double-doped yttrium aluminate novel near-infrared laser crystal of bismuth potassium according to claim 5, special Sign is that the step S1 processes are as follows：By the Bi that purity is 99.99%2O3、K2CO3、Y2O3And Al2O3It matches and mixes according to materials, 5 are then mixed in batch mixer ~20 hours；Raw material is pressed into columned material cake under the pressure of 1-5Gpa；Material cake is put into Muffle furnace, 5~10 hours are warming up to 1000~1200 DEG C, are sintered 20~30 hours in this temperature, Room temperature is down to 10~15 hours, makes batch mixing that solid phase reaction fully occur, you can obtains the double-doped yttrium aluminate crystal powder of bismuth potassium.
- 7. a kind of preparation method of the double-doped yttrium aluminate novel near-infrared laser crystal of bismuth potassium according to claim 5, special Sign is that the step S2 processes are as follows：Above-mentioned raw materials are put into Iridium Crucible, using Frequency Induction Heating, using YAP crystal as seed crystal；It is grown using Czochralski czochralski methods along b axis or a axis directions, according to seeding, necking down, shouldering, isometrical, ending journey Sequence grows the double-doped yttrium aluminate crystal of bismuth potassium.
- 8. a kind of preparation method of the double-doped yttrium aluminate novel near-infrared laser crystal of bismuth potassium according to claim 7, special Sign is that crystal cooling rate is 20~30 DEG C/h in the step S2.
- 9. a kind of preparation method of the double-doped yttrium aluminate novel near-infrared laser crystal of bismuth potassium according to claim 5, special Sign is that the step S3 processes are as follows：It will obtain crystal to anneal in air, annealing temperature is 1100~1200 DEG C, and soaking time is 10~30 hours.
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| CN112851116A (en) * | 2021-01-19 | 2021-05-28 | 吉林师范大学 | High-density terbium/cerium-doped scintillation glass and preparation method thereof |
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| CN102560661A (en) * | 2010-12-16 | 2012-07-11 | 中国科学院福建物质结构研究所 | Chromium and praseodymium co-doped erbium-activated calcium yttrium aluminate novel medium-wave infrared laser crystal |
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| CN107230928A (en) * | 2017-04-20 | 2017-10-03 | 暨南大学 | The infrared double-doped laser crystal of holmium neodymium towards in 3.7 ~ 4.2 microns of all solid lasers |
| CN108233165A (en) * | 2018-01-22 | 2018-06-29 | 暨南大学 | Towards the double-doped laser crystal of near-infrared bismuth tantalum of 0.95~1.65 micron of all solid laser |
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| CN112851116A (en) * | 2021-01-19 | 2021-05-28 | 吉林师范大学 | High-density terbium/cerium-doped scintillation glass and preparation method thereof |
| CN112851116B (en) * | 2021-01-19 | 2022-09-09 | 吉林师范大学 | High-density terbium/cerium-doped scintillation glass and preparation method thereof |
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