CN102337591B - Ytterbium-doped potassium triyttrium borate laser crystal, and growing method and application thereof - Google Patents
Ytterbium-doped potassium triyttrium borate laser crystal, and growing method and application thereof Download PDFInfo
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Abstract
The invention relates to a novel ytterbium-doped potassium triyttrium borate laser crystal, and a growing method and application thereof. The laser crystal belongs to a P21/C space group and has low symmetry and multiple substituting sites, so that Yb ions can produce great crystal field splitting, thereby forming a four-level laser operation mechanism. The crystal is grown by adopting a molten salt method based on a Li-K-B-F-O fluxing agent system, the growing temperature is controlled to range between 800 DEG C and 900 DEG C, a middle seed crystal or top seed crystal method is used, the cooling rate is 1-5 DEG C per day, the rotation speed is 5-30 revolutions per minute, and a single crystal having larger size and higher quality can be grown successfully. The crystal can be used as a tunable laser crystal. A laser device manufactured from the crystal can hopefully produce high-efficiency laser or femtosecond laser, thereby having important application in the fields of social production, military, medicine, science and the like.
Description
Technical field
The present invention relates to the optoelectronic functional materials field, be specifically related to a kind of ytterbium-doped potassium triyttrium borate laser crystals and growth method and purposes.
Background technology
In recent years, along with the fast development of laser technology, be used widely at numerous areas such as optics, communication, medical science, military affairs, all solid state laser particularly is little because of its volume, price is low, advantages of simple structure and simple people's attention extremely.All solid state laser generally all is to produce laser by laser diode-pumped laser crystals.So-called laser crystals is exactly to be made up of host crystal and active ions, and its various physics and chemical property all are to be determined by host crystal, and its spectral response curve and fluorescence lifetime then are to have active ions to determine.Up to now, found hundreds of laser crystalss, but really obtain practical application also with regard to tens kinds, still neodymium (Nd mostly wherein
3+) laser crystals that mixes, and ytterbium (Yb
3+) mix have only several.Yb
3+As the laser crystals of active ions than Nd
3+Active ions have following advantage: (1) Yb
3+Absorption band in 0.9 μ m～1.1 mum wavelength scopes, can effectively be coupled with high-power InGaAs laser diode pumping source, and it is wide to absorb bandwidth (FWHM), need not the pumping wavelength that strict temperature control can obtain the LD pumping source of phase matched; (2) level structure is simple, and two electronic states, i.e. ground state are only arranged
2F
7/2And excited state
2F
5/2(Δ E=10000cm
-1).This has been avoided excited state absorption and last conversion, concentration quenching, radiationless relaxation, reduce the quantum defective, improved the efficiency of conversion of laser, reduced the thermal load of pumping threshold power and laser crystals, improved intrinsic laser slope efficiency, quantum yield is up to about 90% in theory; (3) Yb
3+4f
13Electronics has big spin-orbit coupling absorption and causes stronger phonon coupling, therefore has big fluorescence bandwidth, can support short pulse output, and long relatively fluorescence lifetime is conducive to the amplification of ultrashort pulse.And Yb
3+Main drawback as active ions is: because its simple level structure makes the termination energy level of ground state level and transition of electron belong to same energy level multiplicity, at room temperature form the laser operating mechanism of quasi-three-level, this can cause the pumping threshold height, self-absorption is strong and the problems such as bottleneck of macro-energy hot vessel.In order to overcome this shortcoming, realize that quasi-three-level changes to four-level laser operating mechanism, just need make Yb
3+Ground state level produce big as far as possible division.Realize Yb
3+The ground state level method that produces big division mainly be: select a kind of host crystal, will be by Yb in this host crystal structure
3+There is bigger twisted state the position that replaces, and namely there are low symmetry and incoordinate Yb-O bond distance in this position.Satisfy the host crystal of above-mentioned condition, Yb
3+Generally can form four-level laser operating mechanism after the doping, in conjunction with the advantage of above-mentioned Yb ion, generally can produce efficient or high-power laser again.Simultaneously, in order to realize wide absorption and bandwidth of an emission, selecteed host crystal generally also need satisfy: (1) has higher structural disorder degree; (2) have a plurality of substituted positions in the structure.Can satisfy the host crystal of these two or one of them condition simultaneously, pass through Yb
3+After the doping, can obtain efficient or shorter femtosecond laser usually with InGaAs laser diode pump-coupling.It is pumping source that present commercial titanium jewel femto-second laser adopts the Argon ion laser of 515nm or the intracavity frequency doubling laser of 532nm, and this makes the complex structure of femto-second laser, and is expensive, has limited it and has been extensive use of.And with all solid state femto-second laser of InGaAs laser diode pump-coupling Yb doped crystal because of advantages such as it has efficiently, compact construction, volume are little, price is more cheap, therefore by extensive concern.
At present, all actively seeking various physics, chemistry and mechanical property excellence both at home and abroad, and be easy to grow the large-sized novel laser crystal of high quality.Exactly because ytterbium doped crystal also above-mentioned reason becomes the focus of research especially.
Substrate material K
3Y
3(BO
3)
4Be contriver's a kind of new compound synthetic in 2007, though its powder synthesis method and structural performance report (Materials Reseach Bulletin 43 (2008), 882-888).But up to the present yet there are no the growth of its large-size crystals growth and its relevant laser crystals.This material belongs to oblique system, and spacer is P2
1/ c has the Y atom of six cases in the single cell structure, the Y atom of these six cases, and wherein 2 and 8 oxygen coordinations, 4 and 7 oxygen coordinations, symmetry is C
1, their Y-O bond distance's variation range is all bigger, is respectively to Y (6) from Y (1):
As seen, the position that is replaced by Yb in this compound (Y atom case) has bigger torsion resistance, and has 6 and be substituted case.According to the argumentation of front, this makes ytterbium (Yb
3+) K that mixes
3Y
3(BO
3)
4To have laser activity preferably.
Summary of the invention
One object of the present invention is, a kind of ytterbium-doped potassium triyttrium borate laser crystals is provided.
Another object of the present invention provides the growth method of above-mentioned ytterbium-doped potassium triyttrium borate laser crystals.
According to experimental results show that, the ytterbium-doped potassium triyttrium borate laser crystals of the present invention's preparation, can be in all solid state laser, femto-second laser as the application of gain media, perhaps photoflash lamp or laser diode-pumped under be created in tunable laser or ultrashort Application of Spectral Laser in 950nm～1100nm interval.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of ytterbium-doped potassium triyttrium borate laser crystals is characterized in that, the chemical formula of this ytterbium-doped potassium triyttrium borate laser crystals is K
3Y
(3-x)Yb
x(BO
3)
4, can count Yb:K
3Y
3(BO
3)
4, belong to oblique system, spacer P2
1/ C.Wherein, the Yb ion is dopant ion, replaces the crystallographic site of Y atom, and the Yb ionic concn is at 0.05at%-100at%, and the Yb ionic concn is when 10at%, and fluorescence lifetime (τ) is 2.9ms, and its life-span is the function of Yb ionic concn.It can absorb the light of 900nm～1000nm wave band, the infrared laser of exportable 950nm～1100nm, and highest peak is positioned at 1011nm.
The growth method of above-mentioned ytterbium-doped potassium triyttrium borate laser crystals, it is characterized in that this method adopts molten-salt growth, selects the fusing assistant system that contains Li-K-B-F-O for use, in 800 ℃～900 ℃ temperature range, adopt top-seeded solution growth or bubble to give birth to the growth of (middle part seed crystal) method.
Yb:K of the present invention
3Y
3(BO
3)
4Crystal can go out the monocrystalline of better quality large-size with molten-salt growth, after this crystal is made into device, can be applicable in all solid state laser, the femto-second laser as gain media, under photoflash lamp or the pumping of laser secondary light, can be created in tunable laser or ultrashort femtosecond laser in the 950-1100nm interval, in fields such as social production, military affairs, medical science, science important use be arranged.
Embodiment
The present invention relates to a kind of new ytterbium-doped potassium triyttrium borate laser crystals, belong to P2
1/ C spacer has low symmetry, and therefore polysubstituted case, can make the Yb ion produce bigger crystal field splitting, thereby forms four-level laser operating mechanism.The fusing assistant system of Li-K-B-F-O is selected in this crystal by adopting molten-salt growth for use, and growth temperature is controlled between 800-900 ℃, adopt the method for middle part seed crystal or top seed crystal, rate of temperature fall is 1-5 ℃/day, and rotating speed is 5-30 rev/min, and the monocrystalline of large-size better quality can successfully be grown.
Concrete growth method is carried out as follows:
(1) with potassium-containing compound, contain yttrium compound, contain ytterbium compound and boron-containing compound and take by weighing by stoichiometric ratio after, grind, mix, put into retort furnace, 500 ℃ of sintering 4 hours, take out the cooling back and grind fully, put into retort furnace again, temperature is raised to 800 ℃ of sintering 10 hours, takes out the cooling back and grinds fully, put into retort furnace again, temperature is raised to 900 ℃ of sintering 24 hours, takes out the cooling back and grinds fully, puts into retort furnace again, 900 ℃ reburn the knot 24 hours, get Yb:K
3Y
3(BO
3)
4The polycrystal powder sample;
(2) with a small amount of Yb:K of gained in the step (1)
3Y
3(BO
3)
4Polycrystal powder sample and respective amount fusing assistant mix, and the little platinum crucible of Sheng Yuyi is raised to 800 ℃～950 ℃ with temperature, makes sample become melt, constant temperature 5 hours; The gained melt is slowly dropped to 600 ℃ with 5 ℃/hour, turn off stove again, from platinum crucible, separate obtaining Yb:K in the crystal of spontaneous crystallization
3Y
3(BO
3)
4Seed crystal;
(3) with a large amount of Yb:K of gained in the step (1)
3Y
3(BO
3)
4Polycrystal powder sample and respective amount fusing assistant mix, and the big platinum crucible of Sheng Yuyi is raised to 800-950 ℃ with temperature, makes sample become melt, stir after 5 hours constant temperature 5 hours with agitator; Then the temperature of melt slowly is down on the temperature of saturation 0.5-3 ℃, fixes a Yb:K preferably with platinum filament then
3Y
3(BO
3)
4Seed crystal (as step 2 gained), seed crystal is lowered to melt, make seed crystal elder generation melt back a bit, drop to saturation point then, slowly lower the temperature with the rate of temperature fall in (1 ℃-5 ℃)/sky again, treat the long liquid level of lifting from during to certain size of crystal, with (5 ℃-30 ℃)/hour rate of temperature fall drop to room temperature, can obtain Yb:K
3Y
3(BO
3)
4Crystal.
The polycrystal powder sample is prepared by following reaction formula described in the step (1):
3K
2O+(3-x)Y
2O
3+xYb
2O
3+4B
2O
3→2K
3Y
(3-x)Yb
x(BO
3)
4
In the formula, K
2O K
2CO
3, KNO
3, K
2C
2O
4, KOH substitutes;
Y
2O
3With Y (NO
3)
3, Y (CH
3COO)
3And it is alternative by the title complex of C, N, O and Y coordination; Yb
2O
3Available Yb (NO
3)
3, Yb (CH
3COO)
3And it is alternative by the title complex of C, N, O and Yb coordination; B
2O
3Can be by H
3BO
3Substitute; The scope of x is: 0～100%.
Above-mentioned surrogate produces CO in heat-processed
2, NO
2, H
2O, and overflow, thereby only generate required composition, and do not bring impurity component into.
Fusing assistant in the above-mentioned steps (2) is: M-B-F-O (M=Li, K) system, and Yb:K
3Y
3(BO
3)
4With the mol ratio of fusing assistant be 1: 2.0～1: 6.0.
(M=Li, K) fusing assistant is to choose Li in molar ratio to described M-B-F-O
2CO
3, H
3BO
3, KF.2H
2O, K
2CO3,3～5 kinds of preparations among the LiF.
The K that the 10%Yb that grows is mixed
3Y
3(BO
3)
4Crystal is by the direction cutting, polishing, carry out absorption spectrum, fluorescence spectrum and fluorescence lifetime analysis, its result is: this crystal has absorption to the light of 900-1000nm wave band, wherein the strongest in the 977nm absorption, peak width at half height 18nm, 917nm absorb and take second place, belong to wide acromion, they all are fit to adopt laser diode-pumped; When adopting 917nm to excite, its emission band is in the 950-1100nm interval, and the strongest emission peak is in 1011nm, and peak width at half height reaches 97nm; Its fluorescence lifetime is 2.9ms.So wide peak width at half height and long life-span, make this crystal have important application prospects at femtosecond laser.
Below be the embodiment that the contriver provides, these embodiment are in order further to understand the present invention, to the invention is not restricted to these embodiment.
Embodiment 1:Yb:K
3Y
3(BO
3)
4The powder solid phase synthesis
Be K in molar ratio
2CO
3: (1-x) Y
2O
3: xYb
2O
3: H
3BO
3=3: 3 (1-x): 3x: 8 take by weighing following reagent:
K
2CO
3: 41.46 grams, Y
2O
3: 65.48 grams, Yb
2O
3: 11.82 grams, H
3BO
3: 49.464 grams.
With claim reagent, in grinding, grind evenly, be transferred in the corundum crucible then, put into retort furnace, 500 ℃ of sintering 4 hours, take out the cooling back and grind fully, put into retort furnace again, temperature is raised to 800 ℃ of sintering 10 hours, takes out the cooling back and grinds fully, put into retort furnace again, temperature is raised to 900 ℃ of sintering 24 hours, takes out the cooling back and grinds fully, puts into retort furnace again, 900 ℃ reburn the knot 24 hours, get Yb:K
3Y
3(BO
3)
4The polycrystal powder sample.
Embodiment 2:Yb:K
3Y
3(BO
3)
4The growth of crystal
Be Yb: K by mass ratio
3Y
3(BO
3)
4: KF.2H
2O=1: (5-9) taking by weighing reagent, the reagent mix that takes by weighing is evenly placed the Pt crucible, is fusion in 900 ℃ the retort furnace in temperature then, put into crystal growing furnace after cooling, temperature is raised to 900 ℃, makes sample become melt, stirs after 5 hours constant temperature 10 hours; Then melt temperature slowly is down on the temperature of saturation 0.5 ℃～3 ℃, then with a Yb:K preferably
3Y
3(BO
3)
4Seed crystal is fixed on the platinum filament, is lowered to melt, makes Yb:K
3Y
3(BO
3)
4Seed crystal elder generation melt back a bit drops to saturation point then, slowly lowers the temperature with the rate of temperature fall in (1 ℃-5 ℃)/sky again, brilliant rotary speed is 5-30 rev/min, treat the long liquid level of lifting from during to certain size of crystal, with (5 ℃-30 ℃)/hour rate of temperature fall drop to room temperature, can obtain Yb:K
3Y
3(BO
3)
4Crystal.
Embodiment 3:Yb:K
3Y
3(BO
3)
4The growth of crystal
Be Yb: K in molar ratio
3Y
3(BO
3)
4: Li
2CO
3: H
3BO
3: K
2CO
3: LiF=1: (1-5): (1-5): (1-5): (1-3) take by weighing reagent, the reagent mix that takes by weighing is evenly placed the Pt crucible, be fusion in 900 ℃ the retort furnace in temperature then, put into crystal growing furnace after cooling, temperature is raised to 900 ℃, make sample become melt, stirred after 5 hours constant temperature 10 hours; Then melt temperature slowly is down on the temperature of saturation 0.5-3 ℃, then with a Yb:K preferably
3Y
3(BO
3)
4Seed crystal is fixed on the platinum filament, is lowered to melt, makes Yb:K
3Y
3(BO
3)
4Seed crystal elder generation melt back a bit drops to saturation point then, slowly lowers the temperature with the rate of temperature fall in (1 ℃-5 ℃)/sky again, brilliant rotary speed is 5-30 rev/min, treat the long liquid level of lifting from during to certain size of crystal, with (5 ℃-30 ℃)/hour rate of temperature fall drop to room temperature, can obtain Yb:K
3Y
3(BO
3)
4Crystal.
Claims (4)
1. a ytterbium-doped potassium triyttrium borate laser crystals is characterized in that, the chemical formula of this ytterbium-doped potassium triyttrium borate laser crystals is K
3Y
(3-x)Yb
x(BO
3)
4, wherein, the scope of x is: 10-100%; Can count Yb:K
3Y
3(BO
3)
4, belong to oblique system, spacer P2
1/ C.
2. the growth method of the described ytterbium-doped potassium triyttrium borate laser crystals of claim 1, it is characterized in that this method adopts molten-salt growth, selects the fusing assistant system that contains Li-K-B-F-O for use, in 800 ℃～900 ℃ temperature range, adopt the growth of top-seeded solution growth or kyropoulos.
3. method as claimed in claim 2 is characterized in that, carries out as follows:
(1) with potassium-containing compound, contain yttrium compound, contain ytterbium compound and boron-containing compound and take by weighing by stoichiometric ratio after, grind, mix, put into retort furnace, 500 ℃ of sintering 4 hours, take out the cooling back and grind fully, put into retort furnace again, temperature is raised to 800 ℃ of sintering 10 hours, takes out the cooling back and grinds fully, put into retort furnace again, temperature is raised to 900 ℃ of sintering 24 hours, takes out the cooling back and grinds fully, puts into retort furnace again, 900 ℃ reburn the knot 24 hours, get Yb:K
3Y
3(BO
3)
4The polycrystal powder sample;
Described polycrystal powder sample is prepared by following reaction formula:
3K
2O+（3-x）Y
2O
3+xYb
2O
3+4B
2O
3→2K
3Y
（3-x）Yb
x（BO
3）
4
In the formula, K
2O K
2CO
3, KNO
3, K
2C
2O
4Or KOH substitutes;
Y
2O
3Use Y(NO
3)
3, Y(CH
3COO)
3Or it is alternative by the title complex of C, N, O and Y coordination;
Yb
2O
3Use Yb(NO
3)
3, Yb(CH
3COO)
3Or it is alternative by the title complex of C, N, O and Yb coordination;
B
2O
3By H
3BO
3Substitute;
The scope of x is: 10-100%;
(2) with a small amount of Yb:K of gained in the step (1)
3Y
3(BO
3)
4Polycrystal powder sample and respective amount fusing assistant mix, and the little platinum crucible of Sheng Yuyi is raised to 800 ℃～950 ℃ with temperature, makes sample become melt, constant temperature 5 hours; The gained melt is slowly dropped to 600 ℃ with 5 ℃/hour, turn off stove again, from platinum crucible, separate obtaining Yb:K in the crystal of spontaneous crystallization
3Y
3(BO
3)
4Seed crystal;
Described fusing assistant is: M-B-F-O, wherein, M=Li, K, and Yb:K
3Y
3(BO
3)
4With the mol ratio of fusing assistant be 1:2.0～1:6.0;
Described M-B-F-O fusing assistant is to choose Li in molar ratio
2CO
3, H
3BO
3, KF.2H
2O, K
2CO3, LiF be 3 ~ 5 kinds of preparations wherein;
(3) with a large amount of Yb:K of gained in the step (1)
3Y
3(BO
3)
4Polycrystal powder sample and respective amount fusing assistant mix, and the big platinum crucible of Sheng Yuyi is raised to 800-950 ℃ with temperature, makes sample become melt, stir after 5 hours constant temperature 5 hours with agitator; Then the temperature of melt slowly is down on the temperature of saturation 0.5 ℃～3 ℃, fixes a Yb:K preferably with platinum filament then
3Y
3(BO
3)
4Seed crystal is lowered to melt to seed crystal, makes seed crystal elder generation melt back a bit, drop to saturation point then, with 1 ℃/day～5 ℃/day rate of temperature fall cooling, lift from liquid level when treating crystal length to certain size again, rate of temperature fall with 5 ℃/hour～30 ℃/hour drops to room temperature, can obtain Yb:K
3Y
3(BO
3)
4Crystal.
The described ytterbium-doped potassium triyttrium borate laser crystals of claim 1 in all solid state laser, femto-second laser as the application of gain media, perhaps photoflash lamp or laser diode-pumped under be created in tunable laser or ultrashort Application of Spectral Laser in 950nm～1100nm interval.
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| CN109763169B (en) * | 2019-03-06 | 2021-03-02 | 中国科学院新疆理化技术研究所 | Potassium lutetium borate nonlinear optical crystal and its preparation method and use |
| CN110484969B (en) * | 2019-09-12 | 2021-01-15 | 合肥学院 | Platinum-containing inorganic crystalline borate and preparation method thereof |
| CN114101901B (en) * | 2021-12-06 | 2024-01-05 | 苏州晶生新材料有限公司 | Processing technology capable of integrating micro-nano optical structure |
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| CN1782144A (en) * | 2004-12-03 | 2006-06-07 | 中国科学院福建物质结构研究所 | Fs laser crystal of ytterbium doped strontium yttrium borate |
| CN101037797A (en) * | 2006-03-17 | 2007-09-19 | 中国科学院福建物质结构研究所 | Erbium ytterbium boracic acid gadolinium strontium doped laser crystal and preparation method and usage thereof |
| CN101089240A (en) * | 2006-06-13 | 2007-12-19 | 中国科学院福建物质结构研究所 | Ytterbium mixed yttrium calcium borate tunable laser crystal and its preparation and application |
| CN101597797A (en) * | 2009-06-30 | 2009-12-09 | 上海硅酸盐研究所中试基地 | Ytterbium-doped lithium gadolinium borate laser crystal and preparation method thereof |
-
2011
- 2011-11-14 CN CN 201110358821 patent/CN102337591B/en not_active Expired - Fee Related
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| CN1782144A (en) * | 2004-12-03 | 2006-06-07 | 中国科学院福建物质结构研究所 | Fs laser crystal of ytterbium doped strontium yttrium borate |
| CN101037797A (en) * | 2006-03-17 | 2007-09-19 | 中国科学院福建物质结构研究所 | Erbium ytterbium boracic acid gadolinium strontium doped laser crystal and preparation method and usage thereof |
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| CN101597797A (en) * | 2009-06-30 | 2009-12-09 | 上海硅酸盐研究所中试基地 | Ytterbium-doped lithium gadolinium borate laser crystal and preparation method thereof |
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|---|
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| J.H.Gao."Preparation structure and luminescent properties of a new potassium yttrium borate K3Y3(BO3)4".《Materials Research Bulletin》.2007 |
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