CN106684676A - Saturable absorber device based on WS2 and preparation method and application of saturable absorber device - Google Patents
Saturable absorber device based on WS2 and preparation method and application of saturable absorber device Download PDFInfo
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- CN106684676A CN106684676A CN201611116292.0A CN201611116292A CN106684676A CN 106684676 A CN106684676 A CN 106684676A CN 201611116292 A CN201611116292 A CN 201611116292A CN 106684676 A CN106684676 A CN 106684676A
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- saturable absorber
- ammonium tungstate
- absorber device
- tetrathio ammonium
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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
- H01S3/10—Controlling the intensity, frequency, phase, polarisation or direction of the emitted radiation, e.g. switching, gating, modulating or demodulating
- H01S3/11—Mode locking; Q-switching; Other giant-pulse techniques, e.g. cavity dumping
- H01S3/1106—Mode locking
- H01S3/1112—Passive mode locking
- H01S3/1115—Passive mode locking using intracavity saturable absorbers
- H01S3/1118—Semiconductor saturable absorbers, e.g. semiconductor saturable absorber mirrors [SESAMs]; Solid-state saturable absorbers, e.g. carbon nanotube [CNT] based
-
- 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
- H01S3/06—Construction or shape of active medium
- H01S3/063—Waveguide lasers, i.e. whereby the dimensions of the waveguide are of the order of the light wavelength
- H01S3/067—Fibre lasers
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- Electromagnetism (AREA)
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- Optics & Photonics (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Lasers (AREA)
- Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)
Abstract
The invention discloses a saturable absorber device based on WS2 and preparation method and application of the saturable absorber device. An ammonium tetrathiotungstate solution is coated on the surface of an optical fiber connector, and then the WS2 is prepared on the surface of a FC head by use of a method for thermally decomposing the ammonium tetrathiotungstate so as to obtain the WS2/FC head saturable absorber device. The transition metal sulfide material (WS2) is directly grown on the FC head end surface, and the WS2 is tightly contacted with the FC head surface. By use of the preparation method disclosed by the invention, not only are the advantages of the transition metal sulfide material saturable absorber inherited, such as high performance and low manufacturing cost, but also the damage caused by the transfer process can be avoided, the optical loss is reduced, an optical-damage resistance threshold value is improved, and the pulse laser output power is improved.
Description
Technical field
It is more particularly to a kind of to be based on transient metal sulfide the present invention relates to a kind of preparation method of saturated absorbing body
(WS2) practical saturable absorption device and preparation method thereof, belong to ultrashort pulse optical-fiber laser saturable absorber and prepare skill
Art field.
Background technology
Saturable absorber passive mode-locking technology is to realize that laser pulse is effective from psec to femtosecond in optical fiber laser
One of method.In recent years, many different types of nonlinear materials had started new era of saturable absorber, caused extensively
Concern.Particularly, two-dimentional transient metal sulfide material such as molybdenum bisuphide (MoS2) and tungsten disulfide (WS2) be subjected to
It is deep to probe into and be considered as a kind of saturated absorbing body material for having very much a development potentiality.
In general, transient metal sulfide material saturated absorbing body is integrated into fiber ring laser system generally with following
Mode:On different substrates, saturated absorbing body material is dissolved in different solvents including by saturated absorption Material growth
Or saturated absorbing body material attachment directly is incorporated into Shu in optical fiber surface dies on field.From a practical point of view, Ren Heyi
The method of kind is all defective, so as to limit the extensive use industrially of saturated absorbing body material.Grown frequently by the method for CVD
By saturated absorbing body Material growth on different substrates.When saturated absorbing body is incorporated into fiber laser cavity, transition
Metal sulfide material needs to be transferred to the surface of optical fiber from substrate, and material passes through weaker Van der Waals with optical fiber surface
Power is combined, and it is not very closely, so as to increase light loss that may so cause saturated absorbing body and optical fiber surface to combine.Saturation is inhaled
The dissolving of acceptor material then needs a kind of solvent of appropriate index of being become estranged with low light loss in a solvent.This sweetening agent is difficult to
Find.Saturated absorbing body is directly attached to the optical fiber that optical fiber surface or Side polishing fiber cross and can also produce extra optical loss.
Saturated absorbing body membrane process is that a kind of simple and low cost is hopeful to realize the method for practical application.The macromolecule of numerous species
Composite has also been employed that, such as PMMA, makrolon, polyimides and PVA.But, saturated absorbing body material and high score
The optical damage threshold of sub- composite material film is heavily dependent on high molecular polymer.For these reasons, macromolecule
Material is usually a kind of organic material, so has one than relatively low laser damage threshold, thus resisting laser damage ability compared with
It is weak.
The content of the invention
For technical problem present in above-mentioned prior art, WS is based on it is an object of the present invention to provide one kind2's
The preparation method of saturable absorber device, the preparation method is by WS2Film layer growth in situ single-mode fiber FC head surfaces, WS2
Can be combined closely with FC head surfaces, it is to avoid damaged caused by transfer process, reduce light loss, improve threshold for resisting laser damage,
Improve pulsed laser output power.
It is a further object to provide above-mentioned preparation method prepare based on WS2Saturable absorber device
Part.WS should be based on2Saturable absorber device there is the pulse laser that light loss is small, threshold for resisting laser damage is high and higher
Power output.
Third object of the present invention is to provide above-mentioned based on WS2Saturable absorber device application.
In order to solve the above technical problems, the technical scheme is that:
One kind is based on WS2Saturable absorber device preparation method, comprise the following steps:
The metallic sheath of the non-refractory of FC is removed first, is left resistant to elevated temperatures ceramic probe;
Tetrathio ammonium tungstate solution is coated in the surface of ceramic probe, the method using tetrathio ammonium tungstate is thermally decomposed,
WS is prepared on the surface of FC2, during thermal decomposition, hydrogen is passed through in reaction system, obtain WS2/ FC saturated absorbing body device.
Traditional WS2Preparation method be by tetrathio ammonium tungstate carry out Roasting Decomposition prepare WS2But, tetrathio wolframic acid
The sintering temperature of ammonium is too high, and preparing should be based on WS2Saturable absorber device when, temperature higher is inevitably right
Optical fiber causes to damage, and, tetrathio ammonium tungstate easily generates tungstic acid impurity in thermal bake-out, and these can all influence can
The sensitivity of saturated absorbing body units test and accuracy.
Inventor proves by experiment repeatedly, in thermal decomposition, to hydrogen is passed through in reaction system, can avoid three oxygen
Change the generation of tungsten inclusion, while tungsten disulfide can be obtained at lower temperatures, it is to avoid damage optical fiber under high temperature.
Preferably, the solvent in the tetrathio ammonium tungstate solution is ethylene glycol.
Ethylene glycol is a kind of colourless viscous liquid, has good dissolubility for tetrathio ammonium tungstate, because ethylene glycol is molten
The toughness of liquid, preferably absorption, on the surface of ceramic probe, is carried out when to tetrathio ammonium tungstate can to make tetrathio ammonium tungstate
During thermal decomposition, the tungsten disulfide of generation can preferably be grown in the surface of ceramic probe, being closely connected between ceramic probe.
Compared to traditional dimethyl formamide solution, experiment finds that during using ethylene glycol, the saturable absorber device for obtaining has
More preferable sensitivity and the degree of accuracy, this is not accomplished using other organic solvents.Because the species of organic solvent is more,
Select ethylene glycol as solvent in so many organic solvent, be experiment in inventor's years of researches experience and repeatedly
Verified, be non-obvious.
It is further preferred that the concentration of the tetrathio ammonium tungstate solution is 1-1.5%.% at this refers to quality percentage
Number.
Preferably, the fiber connector is the FC connectors of single-mode fiber.
Wherein, glass core is very thin centered on single-mode fiber, can only pass a kind of optical fiber of pattern.Single mode light is compared to multimode
Optical fiber can support more longer transmission distance.
Fiber connector, is to be coupled together by its internal split coupling by connector between optical fiber, to ensure light
Highest switching performance between fine wire jumper.Fiber connector is generally divided into the fiber connectors such as ST, SC, FC and LC, wherein FC light
Fine joint is most commonly seen.Locked mode needs single-mode fiber, and the metallic sheath of the non-refractory of FC can be removed, convenient in optical fiber head
Section direct growth tungsten disulfide.
Preferably, the method for thermally decomposing tetrathio ammonium tungstate, comprises the following steps:
The fiber connector that tetrathio ammonium tungstate solution will be scribbled is heated to 400-800 DEG C under vacuum conditions, while to
Its hydrogen and argon gas that are passed through set amount, is thermally decomposed, and is obtained final product.
Before the heat decomposition temperature of tetrathio ammonium tungstate is heated to, the solvent in tetrathio ammonium tungstate solution is in heating
Under the conditions of volatilize, tetrathio ammonium tungstate is brought into close contact in the surface of fiber connector.When thermally decomposing again, two sulphur of generation
Change tungsten to be brought into close contact in the surface of fiber connector, form fine and close curing tungsten layer.Fine and close, undamaged curing tungsten layer can
To avoid light injury, threshold for resisting laser damage is significantly improved, and then improve pulsed laser output power.
Preferably, the time of thermal decomposition is 60-120min.
Preferably, the vacuum of pyrolysis is 1-3 × 10-6Support (torr).Experiment finds, if vacuum is not high
Words, the tungsten disulfide for obtaining may adulterate tungstic acid impurity, influence sensitivity and the accuracy of saturable absorber device,
And the vacuum of reaction system is down to 10-6During support, under the reaction conditions, then more pure tungsten disulfide can be obtained.
Preferably, the container that thermal decomposition occurs is quartz ampoule.
Quartz ampoule is quartz glass tube, is a kind of very excellent basic material.And with high temperature resistant, corrosion-resistant, heat
The good characteristic that good stability, light transmission are good and electrical insulation capability is good.It is coated with the optical fiber of four thio ammonium molybdate solution
Sensing unit be put into quartz ampoule, be easy to sealing after vacuumize.And because quartz ampoule can for a long time be used at 1100 DEG C,
When carrying out pyrolytic reaction, quartz ampoule can be used normally, and the failure of experiment will not be caused because of the destruction of quartz ampoule.
Preferably, after the completion of the above method also includes being pyrolyzed, under argon atmosphere the step of Temperature fall.
Because the temperature for thermally decomposing is higher, when the tungsten disulfide for thermally decomposing to yield exposes in atmosphere, in high temperature action
Under, tungsten disulfide can react with the active gases in air, produce impurity.So, by tungsten disulfide nature under argon atmosphere
Cooling, on the one hand can be by tungsten disulfide and air exclusion, it is ensured that the purity of tungsten disulfide, and then ensures the Fibre Optical Sensor for obtaining
The sensitivity of device probe;On the other hand, the natural cooling process of tungsten disulfide, is also that tungsten disulfide carries out closely knit process, from
Curing tungsten layer packing so after cooling is higher, and the active force between optical fiber is stronger, it is to avoid the damage of Fibre Optical Sensor,
The stability and accuracy of the detection of Fibre Optical Sensor are ensure that simultaneously.
Above-mentioned preparation method prepare based on WS2Saturable absorber device.
It is above-mentioned based on WS2Application of the saturable absorber device in ultra-short pulse laser locked mode.
Beneficial effects of the present invention are:
By transient metal sulfide material (WS2) it is grown directly upon FC end surfaces, WS2It is in close contact with FC head surfaces.It is this
Method not only inherits the advantage of transient metal sulfide material saturated absorbing body, such as high-performance, low cost of manufacture, Er Qieke
To avoid being damaged caused by transfer process, light loss is reduced, improve anti-light injury threshold, improve pulsed laser output power.
Brief description of the drawings
Fig. 1 is WS prepared by the embodiment of the present invention2/ FC the structure chart of fiber saturable absorber;
Fig. 2 is WS prepared by the embodiment of the present invention2/ FC the Raman spectrum of fiber saturable absorber;
Fig. 3 is WS prepared by the embodiment of the present invention2The pulse train that/FC fiber saturable absorber locked mode is produced.
Wherein, 1, the WS of FC head surfaces growth2Film, 2, the optical fiber of ceramic probe parcel.
Specific embodiment
Technical scheme is described further with reference to specific embodiments and the drawings.
Embodiment 1
One kind is based on transient metal sulfide material WS2The preparation method of the practical saturable absorption device of/FC, bag
Include following steps:
1st, the cleaning of FC:
The metallic sheath of the non-refractory of FC is removed first, is left resistant to elevated temperatures ceramic probe, ceramic probe is put into
In acetone, it is cleaned by ultrasonic 15 minutes in ultrasonic machine;After the completion of cleaning, the ceramic probe of FC is put into alcohol in ultrasound
It is cleaned by ultrasonic 15 minutes in machine;After the completion of FC be further put into deionized water be cleaned by ultrasonic 15 points in ultrasonic machine
Clock, the FC heads for being cleaned.
2nd, tetrathio ammonium tungstate solution is equipped with:
The tetrathio ammonium tungstate powder for weighing certain mass using a ten thousandth balance is put into container.Use micropipettor
Take ethylene glycol solvent injection to be placed with the container of tetrathio ammonium tungstate powder, be made into the solution that mass fraction is 1.5%.Afterwards will
Solution is put into ultrasonic machine to be carried out ultrasonically treated 20 minutes, is crushed tetrathio ammonium tungstate powder and is formed uniform solution.
3rd, the dropwise addition of tetrathio ammonium tungstate solution:
FC for cleaning is soaked in the tetrathio ammonium tungstate solution for preparing in step 2.After five minutes by FC from
Taken out in solution, be placed on heating platform and heat 25 minutes, temperature setting is 100 DEG C, tetrathio ammonium tungstate is closely pasted
It is attached to FC head surfaces.
4th, annealing obtains WS2/ FC saturated absorbing body:
The tetrathio ammonium tungstate that will be obtained in step 3/FC is put into CVD tube furnaces center;Vavuum pump is opened by quartz ampoule
Air pressure be evacuated to end vacuum state 3 × 10-6Torr;Argon gas and hydrogen flowing quantity are respectively set as 100sccm and 30sccm, by argon
In gas and hydrogen gas mixture injection vacuum chamber;After tubular type furnace temperature reaches 500 DEG C, constant temperature is made annealing treatment for 80 minutes.Close
Close hydrogen, and by tube furnace slow cooling to room temperature.Taken out from tube furnace, obtain WS2/ FC saturated absorbing body.
Fig. 1 is WS prepared by the embodiment of the present invention2/ FC the structure chart of fiber saturable absorber, wherein, sequence number 1 is made a living
The tungsten disulfide film of the end face in ceramic probe long, 2 is the optical fiber of ceramic probe parcel;After the completion of growth, single-mode fiber end
Face and FC fiber optic protection layer of optical cable end face can all grow WS2/ FC films.WS shown in Fig. 22The Raman figure of/FC saturated absorbing body devices
Picture, 350cm in figure-1And 418cm-1Respectively WS2Raman characteristic peak, it was confirmed that FC head surfaces have successfully wrapped up WS2Film.Figure
By WS shown in 32/ FC fiber saturable absorber accesses the mode locking pulse sequence that light path is obtained, and shows that we grow the WS for obtaining2/
FC fiber saturable absorber can realize laser mode locking.
Embodiment 2
One kind is based on transient metal sulfide material WS2The preparation method of the practical saturable absorption device of/FC, bag
Include following steps:
1st, the cleaning of FC:
The metallic sheath of the non-refractory of FC is removed first, is left resistant to elevated temperatures ceramic probe, ceramic probe is put into
In acetone, it is cleaned by ultrasonic 15 minutes in ultrasonic machine;After the completion of cleaning, the ceramic probe of FC is put into alcohol in ultrasound
It is cleaned by ultrasonic 15 minutes in machine;After the completion of FC be further put into deionized water be cleaned by ultrasonic 15 points in ultrasonic machine
Clock, the FC heads for being cleaned.
2nd, tetrathio ammonium tungstate solution is equipped with:
The tetrathio ammonium tungstate powder for weighing certain mass using a ten thousandth balance is put into container.Use micropipettor
Take ethylene glycol solvent injection to be placed with the container of tetrathio ammonium tungstate powder, be made into the solution that mass fraction is 1%.Afterwards will be molten
Liquid is put into ultrasonic machine to be carried out ultrasonically treated 20 minutes, is crushed tetrathio ammonium tungstate powder and is formed uniform solution.
3rd, the dropwise addition of tetrathio ammonium tungstate solution:
FC for cleaning is soaked in the tetrathio ammonium tungstate solution for preparing in step 2.After five minutes by FC from
Taken out in solution, be placed on heating platform and heat 30 minutes, temperature setting is 130 DEG C, tetrathio ammonium tungstate is closely pasted
It is attached to FC head surfaces.
4th, annealing obtains WS2/ FC saturated absorbing body:
The tetrathio ammonium tungstate that will be obtained in step 3/FC is put into CVD tube furnaces center;Vavuum pump is opened by quartz ampoule
Air pressure be evacuated to end vacuum state 1 × 10-6Torr;Argon gas and hydrogen flowing quantity are respectively set as 120sccm and 40sccm, by argon
In gas and hydrogen gas mixture injection vacuum chamber;After tubular type furnace temperature reaches 800 DEG C, constant temperature is made annealing treatment for 120 minutes.Close
Close hydrogen, and by tube furnace slow cooling to room temperature.Taken out from tube furnace, obtain WS2/ FC saturated absorbing body.
Although above-mentioned be described with reference to accompanying drawing to specific embodiment of the invention, not to invention protection domain
Limitation, one of ordinary skill in the art should be understood that on the basis of technical scheme those skilled in the art are not required to
The various modifications or deformation made by paying creative work are still within the scope of the present invention.
Claims (10)
1. it is a kind of to be based on WS2Saturable absorber device preparation method, it is characterised in that:Comprise the following steps:
The metallic sheath of the non-refractory of FC is removed first, is left resistant to elevated temperatures ceramic probe;
Tetrathio ammonium tungstate solution is coated in the surface of ceramic probe, the method using tetrathio ammonium tungstate is thermally decomposed, in FC
The surface of head prepares WS2, during thermal decomposition, hydrogen is passed through in reaction system, obtain WS2/ FC saturated absorbing body device.
2. preparation method according to claim 1, it is characterised in that:Solvent in the tetrathio ammonium tungstate solution is second
Glycol.
3. preparation method according to claim 2, it is characterised in that:The concentration of the tetrathio ammonium tungstate solution is 1-
1.5%.
4. preparation method according to claim 1, it is characterised in that:The method for thermally decomposing tetrathio ammonium tungstate, including such as
Lower step:
FC that tetrathio ammonium tungstate solution will be scribbled is heated to 400-800 DEG C under vacuum conditions, while being passed through setting to it
The hydrogen and argon gas of amount, are thermally decomposed, and are obtained final product.
5. preparation method according to claim 4, it is characterised in that:The time of thermal decomposition is 60-120min.
6. preparation method according to claim 4, it is characterised in that:The vacuum of pyrolysis is 1-3 × 10-6Support.
7. preparation method according to claim 4, it is characterised in that:It is quartz ampoule to thermally decompose the container for occurring.
8. preparation method according to claim 4, it is characterised in that:After the completion of also including being pyrolyzed, under argon atmosphere certainly
So the step of cooling.
9. any preparation methods of claim 1-8 prepare based on WS2Saturable absorber device.
10. WS is based on described in claim 92Application of the saturable absorber device in ultra-short pulse laser locked mode.
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Cited By (4)
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CN107229138A (en) * | 2017-07-17 | 2017-10-03 | 上海交通大学 | Full light opens the light device and its operating method |
CN109842013A (en) * | 2019-04-16 | 2019-06-04 | 西北工业大学 | A kind of saturable absorption device, preparation method and fiber pulse laser |
CN111689519A (en) * | 2020-05-15 | 2020-09-22 | 杭州电子科技大学 | Method for preparing two-dimensional transition metal chalcogenide by adopting precursor thermal decomposition |
CN114552354A (en) * | 2022-02-24 | 2022-05-27 | 郑州轻工业大学 | Ethylene glycol-based saturable absorber, preparation method and application thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107229138A (en) * | 2017-07-17 | 2017-10-03 | 上海交通大学 | Full light opens the light device and its operating method |
CN109842013A (en) * | 2019-04-16 | 2019-06-04 | 西北工业大学 | A kind of saturable absorption device, preparation method and fiber pulse laser |
CN111689519A (en) * | 2020-05-15 | 2020-09-22 | 杭州电子科技大学 | Method for preparing two-dimensional transition metal chalcogenide by adopting precursor thermal decomposition |
CN114552354A (en) * | 2022-02-24 | 2022-05-27 | 郑州轻工业大学 | Ethylene glycol-based saturable absorber, preparation method and application thereof |
CN114552354B (en) * | 2022-02-24 | 2024-01-12 | 郑州轻工业大学 | Ethylene glycol-based saturable absorber, preparation method and application thereof |
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