CN103723758B - Preparation method of polyphyletic terrae rare fluoride nano particles and transparent lighting dispersive solution thereof - Google Patents

Preparation method of polyphyletic terrae rare fluoride nano particles and transparent lighting dispersive solution thereof Download PDF

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CN103723758B
CN103723758B CN201310672482.0A CN201310672482A CN103723758B CN 103723758 B CN103723758 B CN 103723758B CN 201310672482 A CN201310672482 A CN 201310672482A CN 103723758 B CN103723758 B CN 103723758B
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rare earth
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dehydrated alcohol
multielement rare
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CN103723758A (en
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韦玮
段维宽
施宇豪
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Changzhou Chuangneng Three-dimensional Technology Co., Ltd.
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Nanjing Post and Telecommunication University
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Abstract

The invention discloses a preparation method of polyphyletic terrae rare fluoride K5NdLi2F10 nano particles and a transparent lighting dispersive solution thereof. The proportion of raw materials is determined according to a chemical gauging ratio, the K5NdLi2F10 nano particles with good appearance are obtained via a liquid phase gel process, a hydrothermal process and a transient heat treatment process. The transparent lighting dispersive solution of the polyphyletic terrae rare fluoride K5NdLi2F10 nano particle, which has the characteristic of near-infrared lighting, is obtained via a ball milling process and a dispersion process. The preparation method lowers reaction conditions and preparation difficulty and simplifies processing steps; the particle size of the particles is small; the dispersion is uniform; the luminous intensity is high; the service life of fluorescence is long; energy is saved; the quality of the product is improved.

Description

The preparation method of a kind of multielement rare earth fluoride nano granule and transparent luminescent dispersion liquid thereof
Technical field
The present invention relates to a kind of simple method for preparing of a kind of multielement rare earth fluoride nano granule and transparent luminescent dispersion liquid thereof, particularly relate to a kind of multielement rare earth fluorochemical K 5ndLi 2f 10the simple method for preparing of nano particle under liquid-phase condition.
Background technology
Multielement rare earth fluorochemical K 5ndLi 2f 10it is the high density crystal of fluoride obtaining stimulated emission the earliest.Therefore the concern of numerous laserable material investigator is received.As a kind of excellent laser crystals.Have activated ion concentration high, luminous power is strong, and fluorescence lifetime is long, and phonon energy is low waits many merits.But traditional K 5ndLi 2f 10the synthesis of powder mainly adopts fused salt slow cooling method, due to unstable under molten state during fluorochemical high temperature, and very easily etching apparatus, and volatilize toxic gas.Traditional preparation methods require with argon shield, in platinum crucible, relevant fluorochemical is proportionally mixed, 800-1000 DEG C be heated to molten state after, with 9 DEG C/h, be cooled to room temperature gradually.The defects such as it is high that it has equipment requirements, severe reaction conditions, prepares length consuming time, and product reunion caking phenomenon is serious, and dispersion liquid is muddy.
Summary of the invention
The present invention mentions a kind of multielement rare earth fluorochemical K 5ndLi 2f 10a kind of simple method for preparing of nano particle and transparent luminescent dispersion liquid thereof.
The present invention's potassium ethylate, alcohol dissolubility neodymium salt, alcohol dissolubility lithium salts, high concentration of hydrofluoric acid (49wt%), dehydrated alcohol, as starting raw material, by according to element ratio and order of addition(of ingredients), successively by gelation process, water-heat process, calcination process obtains the K in regular pattern 5ndLi 2f 10nano crystal particles.
Concrete steps are:
A, potassium ethylate is dissolved in dehydrated alcohol, is mixed with the ethanolic soln that concentration is the potassium ethylate of 0.01-0.1mol/L, is placed in beaker, stir 15min;
B, alcohol dissolubility neodymium salt is dissolved in dehydrated alcohol, be mixed with concentration be 0.01-0.1mol/L containing neodymium ion ethanolic soln, be placed in beaker, stir 15min;
C, alcohol dissolubility lithium salts is dissolved in dehydrated alcohol, be mixed with concentration be 0.01-0.1mol/L containing lithium ethanolic soln, be placed in beaker, stir 15min;
D, step a, b, c gained solution to be mixed according to suitable proportion, in mixing process, add the tensio-active agent Triton-100 of 1.5mL, stir 30min.
E, by high concentration of hydrofluoric acid (49wt%) under agitation, dropwise instills in steps d gained mixing solutions, makes mixture be gel.
F, gelatinous mixture is transferred to tetrafluoroethylene is in the hydro-thermal reaction device of liner, and react and carry out in air dry oven, temperature of reaction is 150-200 DEG C, and the reaction times is 10-24h.
G, be transferred in centrifuge tube by step f products therefrom, centrifugal speed is 4000-12000r/min, each centrifugal 10-30min, and employing dehydrated alcohol is medium, repeated centrifugation process 5-6 time.
H, by step g products therefrom, dry in vacuum drying oven, drying temperature is 60 DEG C, and time of drying is 24-48h.
I, step h products therefrom to be transferred in agate mortar suitably grinding after, under argon shield, in retort furnace, calcine 0.5-5h at 300-600 DEG C, after naturally cooling to room temperature, product ground in agate mortar, multielement rare earth fluorochemical K can be obtained 5ndLi 2f 10nano particle.
J, take 20g zirconium ball, its quality of different-grain diameter zirconium ball is respectively 3mm × 4g, 1mm × 4g, 0.5mm × 4g, 0.3mm × 4g, 0.1mm × 4g.
The mixing of k, zirconium ball step I products therefrom, step j taken and 40mL dehydrated alcohol is also fully stirred.
L, by step k gained mixture in ball mill with the rotating speed of 600r/min, continuous ball milling 7 days.
M, be transferred in centrifuge tube by step l products therefrom, centrifugal speed is 12000r/min, each centrifugal 30min, and employing dehydrated alcohol is medium, repeated centrifugation process 5-6 time.
N, by step m product, dry in vacuum drying oven, drying temperature is 60 DEG C, and time of drying is 48h.
O, take certain mass step n products therefrom as required, and be dissolved to the poly(oxyethylene glycol) 400 of certain volume, ultrasonic agitation, the multielement rare earth fluorochemical K with near-infrared luminous characteristic can be obtained 5ndLi 2f 10the transparent dispersion liquid of nanocrystal.
In steps d, e, four kinds of described reactant potassium ethylates, alcohol dissolubility rare earth salts, alcohol dissolubility lithium salts, the element contained respectively in high concentration of hydrofluoric acid (49wt%), potassium: neodymium: lithium: fluorine element ratio is 5:1:2:10; Wherein fluorine element can be suitably excessive.
The prepared reaction of step a-g all occurs under liquid-phase condition.
The nano powder product quality added in step k is 1-20g.
The product that the method obtains is regular cubic nanometer particle.
The present invention mentions a kind of multielement rare earth fluorochemical K 5ndLi 2f 10a kind of simple method for preparing of nano particle and transparent luminescent dispersion liquid thereof.By liquid phase gelation process, water-heat process, in short-term heat treatment process, can obtain the K that pattern is good 5ndLi 2f 10nano particle.Reduce reaction conditions and preparation difficulty, simplify treatment step, energy efficient, improve product quality.By mechanical milling process, dispersion process can obtain K 5ndLi 2f 10transparent luminescent dispersion liquid.
Accompanying drawing explanation
Fig. 1 is the multielement rare earth fluorochemical K that the embodiment of the present invention 1 obtains 5ndLi 2f 10the TEM figure of nano particle.
Fig. 2 is the multielement rare earth fluorochemical K that the embodiment of the present invention 1 obtains 5ndLi 2f 10the XRD figure of nano particle.
Fig. 3 is the K that the embodiment of the present invention 1 obtains 5ndLi 2f 10the fluorescence spectrum figure of the transparent dispersion liquid of nanocrystal.
Fig. 4 is the K that the embodiment of the present invention 1 obtains 5ndLi 2f 10the transparent dispersion liquid of nanocrystal through figure.
Fig. 5 is the multielement rare earth fluorochemical K that the embodiment of the present invention 2 obtains 5ndLi 2f 10the TEM figure of nano particle.
Fig. 6 is the multielement rare earth fluorochemical K that the embodiment of the present invention 2 obtains 5ndLi 2f 10the XRD figure of nano particle.
Fig. 7 is the multielement rare earth fluorochemical K that the embodiment of the present invention 3 obtains 5ndLi 2f 10the TEM figure of nano particle.
Fig. 8 is the multielement rare earth fluorochemical K that the embodiment of the present invention 3 obtains 5ndLi 2f 10the XRD figure of nano particle.
Embodiment
Further illustrate method of the present invention below in conjunction with three embodiments, from example 2 key distinction, example 1 is that required element source is different, example 1 mainly uses nitrate, and example 2 mainly uses muriate, the method desired raw material wide material sources.From example 3 key distinction, example 1 is that pyroprocessing condition is different, example 1 adopts comparatively high temps, fast processing, and example 2 adopts thermal treatment temp lower, but the time length is longer, and needed for the method, condition is not harsh, more flexibly.
Embodiment 1:
Concrete implementation step is as follows:
A, potassium ethylate is dissolved in dehydrated alcohol, is mixed with the ethanolic soln that concentration is the potassium ethylate of 0.1mol/L, is placed in beaker, stir 15min;
B, neodymium nitrate is dissolved in dehydrated alcohol, is mixed with the neodymium nitrate ethanolic soln that concentration is 0.1mol/L, is placed in beaker, stir 15min;
C, lithium nitrate is dissolved in dehydrated alcohol, is mixed with the lithium nitrate ethanolic soln that concentration is 0.1mol/L, is placed in beaker, stir 15min;
D, a, b, c gained solution gets 40mL, 8mL, 16mL respectively, is mixed, and adds the tensio-active agent Triton-100 of 1.5mL in mixing process, stirs 30min.
E, by 4mL high concentration of hydrofluoric acid (49wt%) under agitation, dropwise instills in steps d gained mixing solutions, makes mixture be gel.
F, gelatinous mixture is transferred to tetrafluoroethylene is in the hydro-thermal reaction device of liner, and react and carry out in air dry oven, temperature of reaction is 200 DEG C, and the reaction times is 12h.
G, be transferred in centrifuge tube by step f products therefrom, centrifugal speed 10000r/min, each centrifugal 30min, employing dehydrated alcohol is medium, repeated centrifugation process 5-6 time.
H, by step g product, dry in vacuum drying oven, drying temperature is 60 DEG C, and time of drying is 48h.
I, h step products to be transferred in agate mortar suitably grinding after, under argon shield, in retort furnace, calcine 1.5h at 500 DEG C, after naturally cooling to room temperature, product ground in agate mortar, multielement rare earth fluorochemical K can be obtained 5ndLi 2f 10nano particle.
J, take 20g zirconium ball, different-grain diameter zirconium ball and quality thereof are respectively 3mm × 4g, 1mm × 4g, 0.5mm × 4g, 0.3mm × 4g, 0.1mm × 4g.
K, step I products therefrom, step j taken zirconium ball and the mixing of 40mL dehydrated alcohol and fully stir.
L, by step k gained mixture in ball mill with the rotating speed of 600r/min, continuous ball milling 7 days.
M, be transferred in centrifuge tube by step l products therefrom, centrifugal speed is 12000r/min, each centrifugal 30min, and employing dehydrated alcohol is medium, repeated centrifugation process 5-6 time.
N, by step m product, dry in vacuum drying oven, drying temperature is 60 DEG C, and time of drying is 48h.
O, take certain mass step n products therefrom as required, and be dissolved to the poly(oxyethylene glycol) 400 of certain volume, ultrasonic agitation, the multielement rare earth fluorochemical K with near-infrared luminous characteristic can be obtained 5ndLi 2f 10the transparent dispersion liquid of nanocrystal.
As shown in Figure 1, size is homogeneous, is uniformly dispersed for the TEM figure of product.
XRD figure as shown in Figure 2, figure can be seen and confirm that obtaining product is multielement rare earth fluorochemical K further 5ndLi 2f 10nano particle.
Fluorescence spectrum figure as shown in Figure 3, this product mainly near infrared section emitting fluorescence, by Fig. 4 through the known dispersion liquid of spectrum at near-infrared band, there is higher transmitance.
Embodiment 2:
Concrete implementation step is as follows:
A, potassium ethylate is dissolved in dehydrated alcohol, is mixed with the ethanolic soln that concentration is the potassium ethylate of 0.1mol/L, is placed in beaker, stir 15min;
B, Neodymium trichloride is dissolved in dehydrated alcohol, is mixed with the Neodymium trichloride ethanolic soln that concentration is 0.1mol/L, is placed in beaker, stir 15min;
C, lithium chloride is dissolved in dehydrated alcohol, is mixed with the lithium chloride ethanolic soln that concentration is 0.1mol/L, is placed in beaker, stir 15min;
D, a, b, c gained solution gets 40mL, 8mL, 16mL respectively, is mixed, and adds 1.5mL tensio-active agent Triton-100 in mixing process, stirs 30min.
E, by 4mL high concentration of hydrofluoric acid (49wt%) under agitation, dropwise instills in steps d gained mixing solutions, makes mixture be gel.
F, gelatinous mixture is transferred to tetrafluoroethylene is in the hydro-thermal reaction device of liner, and react and carry out in air dry oven, temperature of reaction is 200 DEG C, and the reaction times is 12h.
G, be transferred in centrifuge tube by step f products therefrom, centrifugal speed 10000r/min, each centrifugal 30min, employing dehydrated alcohol is medium, repeated centrifugation process 5-6 time.
H, by step g product, dry in vacuum drying oven, drying temperature is 60 DEG C, and time of drying is 48h.
I, h step products to be transferred in agate mortar suitably grinding after, under argon shield, in retort furnace, calcine 1.5h at 500 DEG C, after naturally cooling to room temperature, product ground in agate mortar, multielement rare earth fluorochemical K can be obtained 5ndLi 2f 10nano particle.
J, take 20g zirconium ball, different-grain diameter zirconium ball and quality thereof are respectively 3mm × 4g, 1mm × 4g, 0.5mm × 4g, 0.3mm × 4g, 0.1mm × 4g.
The mixing of k, zirconium ball step I products therefrom, step j taken and 40mL dehydrated alcohol is also fully stirred.
L, by step k gained mixture in ball mill with the rotating speed of 600r/min, continuous ball milling 7 days.
M, be transferred in centrifuge tube by step l products therefrom, centrifugal speed is 12000r/min, each centrifugal 30min, and employing dehydrated alcohol is medium, repeated centrifugation process 5-6 time.
N, by step m product, dry in vacuum drying oven, drying temperature is 60 DEG C, and time of drying is 48h.
O, take certain mass step n products therefrom as required, and be dissolved to the poly(oxyethylene glycol) 400 of certain volume, ultrasonic agitation, the multielement rare earth fluorochemical K with near-infrared luminous characteristic can be obtained 5ndLi 2f 10the transparent dispersion liquid of nanocrystal.
As shown in Figure 5, size is homogeneous, is uniformly dispersed for the TEM figure of product.
XRD figure as indicated with 6, figure can be seen and confirm further to be produced
Thing is multielement rare earth fluorochemical K 5ndLi 2f 10nano particle.
Embodiment 3:
Concrete implementation step is as follows:
A, potassium ethylate is dissolved in dehydrated alcohol, is mixed with the ethanolic soln that concentration is the potassium ethylate of 0.1mol/L, is placed in beaker, stir 15min;
B, neodymium nitrate is dissolved in dehydrated alcohol, is mixed with the neodymium nitrate ethanolic soln that concentration is 0.1mol/L, is placed in beaker, stir 15min;
C, lithium nitrate is dissolved in dehydrated alcohol, is mixed with the lithium nitrate ethanolic soln that concentration is 0.1mol/L, is placed in beaker, stir 15min;
D, a, b, c gained solution gets 40mL, 8mL, 16mL respectively, is mixed, and adds the tensio-active agent Triton-100 of 1.5mL in mixing process, stirs 30min.
E, by 4mL high concentration of hydrofluoric acid (49wt%) under agitation, dropwise instills in steps d gained mixing solutions, makes mixture be gel.
F, gelatinous mixture is transferred to tetrafluoroethylene is in the hydro-thermal reaction device of liner, and react and carry out in air dry oven, temperature of reaction is 150 DEG C, and the reaction times is 12h.
G, be transferred in centrifuge tube by step f products therefrom, centrifugal speed 10000r/min, each centrifugal 30min, employing dehydrated alcohol is medium, repeated centrifugation process 5-6 times.
H, by step g product, dry in vacuum drying oven, drying temperature is 60 DEG C, and time of drying is 48h.
I, h step products to be transferred in agate mortar suitably grinding after, under argon shield, in retort furnace, calcine 2h at 400 DEG C, after naturally cooling to room temperature, product ground in agate mortar, multielement rare earth fluorochemical K can be obtained 5ndLi 2f 10nano particle.
J, take 20g zirconium ball, different-grain diameter zirconium ball and quality thereof are respectively 3mm × 4g, 1mm × 4g, 0.5mm × 4g, 0.3mm × 4g, 0.1mm × 4g.
The mixing of k, zirconium ball step I products therefrom, step j taken and 40mL dehydrated alcohol is also fully stirred.
L, by step k gained mixture in ball mill with the rotating speed of 600r/min, continuous ball milling 7 days.
M, be transferred in centrifuge tube by step l products therefrom, centrifugal speed is 12000r/min, each centrifugal 30min, and employing dehydrated alcohol is medium, repeated centrifugation process 5-6 time.
N, by step m product, dry in vacuum drying oven, drying temperature is 60 DEG C, and time of drying is 48h.
O, take certain mass step n products therefrom as required, and be dissolved to the poly(oxyethylene glycol) 400 of certain volume, ultrasonic agitation, the multielement rare earth fluorochemical K with near-infrared luminous characteristic can be obtained 5ndLi 2f 10the transparent dispersion liquid of nanocrystal.
As shown in Figure 7, size is homogeneous, is uniformly dispersed for the TEM figure of product
XRD figure as depicted in figure 8, figure can be seen and confirm that obtaining product is multielement rare earth fluorochemical K further 5ndLi 2f 10nano particle.
As can be seen from above several embodiment and accompanying drawing, the preparation method that this invention proposes, reduce reaction conditions and preparation difficulty, treatment step is simple, and energy consumption is low, and product quality is high, and reactant is cheap and easy to get, has greatly expanded the range of application of the method; K in the product obtained 5ndLi 2f 10nano particle size is all comparatively homogeneous, and pattern rule, luminosity is good, and transmitance is high.

Claims (2)

1. a multielement rare earth fluoride nano granule preparation method, it is characterized in that with potassium ethylate, alcohol dissolubility neodymium salt, alcohol dissolubility lithium salts, high concentration of hydrofluoric acid, dehydrated alcohol, as starting raw material, by controlling feed ratio and the order of each raw material, successively pass through gelation process, water-heat process, calcination process obtains the multielement rare earth fluoride nano granule of regular appearance; Concrete operations follow these steps to carry out:
A, potassium ethylate is dissolved in dehydrated alcohol, is mixed with the ethanolic soln that concentration is the potassium ethylate of 0.01-0.1mol/L, is placed in beaker, stir 15min;
B, alcohol dissolubility neodymium salt is dissolved in dehydrated alcohol, is mixed with the ethanolic soln containing neodymium ion that concentration is 0.01-0.1mol/L, is placed in beaker, stirs 15min;
C, alcohol dissolubility lithium salts is dissolved in dehydrated alcohol, be mixed with concentration be 0.01-0.1mol/L containing lithium ethanolic soln, be placed in beaker, stir 15min;
D, step a, b, c gained solution to be mixed according to suitable proportion, in mixing process, add tensio-active agent 1.5mL Triton-100, stir 30min;
E, by the high concentration of hydrofluoric acid of 49wt% under agitation, dropwise instills in steps d gained mixing solutions, makes mixture be gel;
F, gelatinous mixture is transferred to tetrafluoroethylene is in the hydro-thermal reaction device of liner, and react and carry out in air dry oven, temperature of reaction is 150-200 DEG C, and the reaction times is 10-24h;
G, be transferred in centrifuge tube by step f products therefrom, centrifugal speed is 4000-12000r/min, each centrifugal 10-30min, and employing dehydrated alcohol is medium, repeated centrifugation process 5-6 time;
H, by step g products therefrom, dry in vacuum drying oven, drying temperature is 60 DEG C, and time of drying is 24-48h;
I, step h products therefrom to be transferred in agate mortar after grinding, under argon shield, in retort furnace, to calcine 0.5-5h at 300-600 DEG C, after naturally cooling to room temperature, product is ground in agate mortar, multielement rare earth fluorochemical K can be obtained 5ndLi 2f 10nano particle.
2. a kind of multielement rare earth fluoride nano granule preparation method according to claim 1, it is characterized in that in steps d, e, four kinds of reactant potassium ethylates, alcohol dissolubility rare earth salts, alcohol dissolubility lithium salts, the element contained respectively in the high concentration of hydrofluoric acid of 49wt%, potassium: neodymium: lithium: fluorine element ratio is 5:1:2:10; Wherein fluorine element can be suitably excessive.
3. a kind of multielement rare earth fluoride nano granule preparation method according to claim 1, is characterized in that, the prepared reaction of step a-g all occurs under liquid-phase condition.
4. a preparation method for multielement rare earth fluoride nano granule transparent luminescent dispersion liquid, it is characterized in that nano crystal particles claim 1 obtained carries out ball milling, dispersion, obtain transparent luminescent dispersion liquid, concrete operations follow these steps to carry out:
A, take 20g zirconium ball, its quality of different-grain diameter zirconium ball is respectively 3mm × 4g, 1mm × 4g, 0.5mm × 4g, 0.3mm × 4g, 0.1mm × 4g;
B, nano crystal particles claim 1 obtained, step a take zirconium ball and the mixing of 40mL dehydrated alcohol is also fully stirred;
C, by step b gained mixture in ball mill with the rotating speed of 600r/min, continuous ball milling 7 days;
D, be transferred in centrifuge tube by step c products therefrom, centrifugal speed is 12000r/min, each centrifugal 30min, and employing dehydrated alcohol is medium, repeated centrifugation process 5-6 time;
E, by steps d product, dry in vacuum drying oven, drying temperature is 60 DEG C, and time of drying is 48h;
F, take certain mass step e products therefrom as required, and be dissolved to the poly(oxyethylene glycol) 400 of certain volume, ultrasonic agitation, the multielement rare earth fluorochemical K with near-infrared luminous characteristic can be obtained 5ndLi 2f 10the transparent dispersion liquid of nanocrystal.
5. the preparation method of a kind of multielement rare earth fluoride nano granule transparent luminescent dispersion liquid according to claim 4, it is characterized in that in step b, the nano crystal particles product quality added is 1-20g.
CN201310672482.0A 2013-12-12 2013-12-12 Preparation method of polyphyletic terrae rare fluoride nano particles and transparent lighting dispersive solution thereof Expired - Fee Related CN103723758B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4229713A (en) * 1978-12-14 1980-10-21 Gte Laboratories Incorporated Stoichiometric rare earth laser material and laser based thereon

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4229713A (en) * 1978-12-14 1980-10-21 Gte Laboratories Incorporated Stoichiometric rare earth laser material and laser based thereon

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
Luminescence properties of Nd3+ doped LaF3 nanocrystals with a long lifetime in organic solvents;Sun Wenxiu et al.;《JOURNAL OF MATERIALS CHEMISTRY》;20121231;第6990-6993页 *
Rare-Eath-Doped Bifunctional Alkaline-Eath Metal Fluoride Nanocrystals via a Facile Microwave-Assisted Process;Pang Min et al.;《INORGANIC CHEMISTRY》;20110620;全文 *
Spectroscopy and Lasing in K5NdLi2F10;LEMPICKI A et al.;《IEEE JOURNAL OF QUANTUM ELECTRONICS》;19791231;第15卷(第9期);第896-903页 *

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