CN112751256A - Saturable absorber based on tungsten ditelluride/tungsten disulfide heterojunction, preparation method and mode-locked fiber laser manufactured by saturable absorber - Google Patents

Saturable absorber based on tungsten ditelluride/tungsten disulfide heterojunction, preparation method and mode-locked fiber laser manufactured by saturable absorber Download PDF

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CN112751256A
CN112751256A CN202011547259.XA CN202011547259A CN112751256A CN 112751256 A CN112751256 A CN 112751256A CN 202011547259 A CN202011547259 A CN 202011547259A CN 112751256 A CN112751256 A CN 112751256A
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saturable absorber
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CN112751256B (en
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何朋飞
陶丽丽
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Guangdong University of Technology
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    • H01S3/00Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
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Abstract

The invention belongs to the technical field of passive mode-locked fiber lasers, and discloses a saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction, a preparation method and a mode-locked fiber laser manufactured by the saturable absorber. The method comprises preparing W film on quartz plate as substrate by magnetron sputtering method, and preparing WS on the substrate by CVD method2A film; then in the same way in WS2Top preparation WTE2To form a WTE2/WS2Heterojunction is etched by strong alkaline solution to obtain the WTE2/WS2A heterojunction thin film. The mode-locked fiber laser comprises a pumping source, a wavelength division multiplexer, a doped fiber, a single-mode fiber, an optical isolator, a fiber coupler, a polarization controller and a WTE2/WS2The heterojunction saturable absorber forms a ring cavity laser. The saturable absorber has good stability, is not easy to oxidize, can be used for laser mode locking for a long time, and has stable mode locking laser performance based on the material.

Description

Saturable absorber based on tungsten ditelluride/tungsten disulfide heterojunction, preparation method and mode-locked fiber laser manufactured by saturable absorber
Technical Field
The invention belongs to the technical field of passive mode-locking fiber lasers, and particularly relates to a tungsten ditelluride/tungsten disulfide (WTE) based fiber laser2/WS2) Saturable absorber of heterojunction and preparation method and prepared by saturable absorberA mode-locked fiber laser is provided.
Background
Compared with the traditional long-pulse (microsecond and nanosecond) laser, the ultrashort-pulse (picosecond and femtosecond magnitude) laser basically does not cause any thermal damage to the periphery of a processed material in the using process, and is an ultra-precise nondestructive processing tool, so that the ultrashort-pulse laser has important research and application values in the fields of precision processing, surgical medical treatment, scientific research and the like. Especially, ultrashort pulse fiber laser, it has simple structure, light-emitting performance stability, multiple advantages such as non-maintaining, portable, has become the preferred high-tech instrument of each industry.
The passive mode locking technology utilizes saturable absorption characteristics in a mode locking device to realize continuous narrowing of pulses so as to generate required ultrashort optical pulses. Therefore, the saturable absorber is the most important component of the ultrashort pulse laser. The most widely commercially used saturable absorber is the semiconductor saturable absorber mirror at present, but the saturable absorber mirror has the defects of high price, complex manufacturing process, narrow working wavelength range, low output energy and the like. Therefore, a saturable absorber with the advantages of broadband tunable nonlinear absorption, low loss, high damage threshold, ultra-fast response time, large modulation depth, low cost and the like is very important to be used as a novel material, and the 2D photoelectric material has unique saturable absorption nonlinear optical characteristics and has good application prospect in the aspect of pulse laser generation.
WS2As a new two-dimensional material, it has been widely demonstrated to be able to produce ultrashort pulsed laser as a saturable absorber, but WS2Longer exciton decay times result in inefficient pulse width compression, typically only resulting in pulsed lasers on the order of sub-nanoseconds and picoseconds. Compared with the pure WS2Film, WTE2/WS2The heterojunction film has stronger saturable absorption characteristic, and compared with a pure two-dimensional material, the heterostructure increases the specific surface area and improves the transition efficiency of carriers. Therefore WTE2/WS2High nonlinear absorption characteristics of heterojunction thin films in saturable absorbers and optical modulatorsAnd has great application value in optoelectronic devices such as optical switches and the like.
Disclosure of Invention
To overcome the disadvantages and shortcomings of the prior art, the present invention provides a tungsten ditelluride/tungsten disulfide (WTE) based optical fiber2/WS2) A method for preparing a saturable absorber of a heterojunction.
The invention further aims to provide a saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction, which is prepared by the preparation method.
It is another object of the present invention to provide a method for preparing a tungsten telluride/tungsten disulfide (WTE) based on the above-mentioned tungsten ditelluride2/WS2) A mode-locked fiber laser made of a saturable absorber of a heterojunction.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction comprises the following operation steps:
(1) sputtering of W: preparing a W film on a quartz substrate by a magnetron sputtering method, specifically, taking a W polycrystalline block as a target material, controlling the radio frequency power to be 80W, the sputtering pressure to be 1.2Pa, controlling the Ar flow to be 50sccm, heating the quartz substrate to 100 ℃, and continuously depositing for 5-30 min;
(2)WS2preparing a film: placing the W film prepared by the magnetron sputtering method at the downstream of the double-temperature-zone tubular furnace, introducing Ar as protective gas, wherein the flow rate is 100 sccm; placing high-purity sulfur powder in a low-temperature area at the upstream of the W film, setting the temperature to be 200 ℃, setting the temperature of a high-temperature area at the downstream to be 1050-1200 ℃, keeping the temperature for 3-5 hours, and then naturally cooling to room temperature;
(3) secondary sputtering of W: WS prepared in step (2)2The film is used as a substrate, and the W film is sputtered again by a magnetron sputtering method, wherein the parameters are the same as those in the step (1);
(4)WTe2/WS2preparing a heterojunction thin film: placing the film prepared by the secondary sputtering in the step (3) at the downstream of the double-temperature-zone tubular furnace, introducing Ar as protective gas, wherein the flow rate is 100 sccm; high-purity tellurium powder (mass fraction) is placed in the upstream low-temperature region of the film99.999 percent), the set temperature is 550 ℃, the temperature of a downstream high-temperature area is 1050-1200 ℃, the temperature is kept for 3-5 hours and then is naturally cooled to the room temperature to obtain the WTE2/WS2A heterojunction thin film;
(5)WTe2/WS2and (3) stripping of the heterojunction film: adopting 5 mass percent of PMMA anisole solution to spin-coat the WTE prepared in the step (4)2/WS2The surface of the heterojunction film is dried at 80 ℃ at the spin-coating rotating speed of 1000-3000 rpm for 10-60 s, and then is soaked in a strong alkaline solution, and the film is heated to be separated from the quartz substrate and float on the surface of the strong alkaline solution; and then rinsing with deionized water, and cutting into small pieces to obtain the saturable absorber based on the tungsten ditelluride/tungsten disulfide heterojunction.
The strong alkali solution in the step (5) is NaOH, KOH or a mixed solution of NaOH and KOH, the mass fraction of the strong alkali solution is 10-50%, and the strong alkali solution is heated to 50-90 ℃.
The rinsing times in the step (5) are three times, and the size of the cut small pieces is 2 multiplied by 2 mm.
The saturable absorber based on the tungsten ditelluride/tungsten disulfide heterojunction is prepared by the preparation method.
The mode-locked fiber laser is made of the saturable absorber based on the tungsten ditelluride/tungsten disulfide heterojunction, and comprises the saturable absorber based on the tungsten ditelluride/tungsten disulfide heterojunction, a pumping source, a wavelength division multiplexer, an ytterbium-doped fiber, an optical isolator, a single-mode fiber, a fiber coupler and a polarization controller.
The wavelength division multiplexer comprises a first input end and a second input end; the optical fiber coupler comprises 75% of output ends and 25% of output ends; the pump source, a first input end of the wavelength division multiplexer, the ytterbium-doped optical fiber, the optical isolator, the single-mode optical fiber, 75% of an output end of the optical fiber coupler, the polarization controller and the saturable absorber based on the double tungsten telluride/tungsten disulfide heterojunction are sequentially connected, and the saturable absorber based on the double tungsten telluride/tungsten disulfide heterojunction is connected with a second input end of the wavelength division multiplexer to form an annular cavity structure; the saturable absorber based on the tungsten ditelluride/tungsten disulfide heterojunction is transferred to the end face of the optical fiber jumper, is connected with another optical fiber jumper by using a flange disc, is arranged in an optical fiber flange, and is respectively connected with the second input end of the wavelength division multiplexer and the polarization controller by using single mode fibers at two ends.
The wavelength of the pumping source is 980nm, and the central wavelength of the wavelength division multiplexer is 1064 nm.
Compared with the prior art, the invention has the following advantages and effects:
(1) the invention combines the magnetron sputtering method and the Chemical Vapor Deposition (CVD) method to prepare the WTE2/WS2The film is uniform in distribution, stable in quality and simple in process, and the thickness of the film can be accurately controlled through process parameters such as sputtering time;
(2) the invention is based on WTE2/WS2Saturable absorber of heterojunction, incorporating WTE2And WS2The method has the advantages that ultrafast laser with large modulation depth and narrow pulse width can be obtained;
(3) when in use, only the WTE is required to be connected2/WS2The heterojunction film is transferred to the end face of the optical fiber connector, the operation is convenient, and the whole laser optical path system runs inside the optical fiber and is not interfered by the external environment.
Drawings
FIG. 1 is a schematic structural diagram of a mode-locked fiber laser made of a saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction as in example 1; wherein, 1 is a pumping source, 2 is a wavelength division multiplexer, 3 is an ytterbium doped fiber, 4 is an optical isolator, 5 is a single mode fiber, 6 is a fiber coupler, 7 is a polarization controller, and 8 is based on WTE2/WS2The saturable absorber of the heterojunction, 9 is the first input end of the wavelength division multiplexer, 10 is the second input end of the wavelength division multiplexer, 11 is 75% output end of the optical fiber coupler, and 12 is 25% output end of the optical fiber coupler.
Fig. 2 is a pulse sequence diagram of a mode-locked fiber laser made from a saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction as in example 1.
Fig. 3 is a graph of a single pulse signal for a mode-locked fiber laser made with a saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction as in example 1.
Fig. 4 is a graph of the radio frequency spectrum of a mode-locked fiber laser made from a saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction as in example 1.
Fig. 5 is a graph of the output power versus pump power for a mode-locked fiber laser made with a saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction as in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
The method comprises the following steps: preparing a W film on a quartz substrate by a magnetron sputtering method, specifically, adopting a W polycrystalline block as a target material, the radio frequency power is 80W, the sputtering pressure is 1.2Pa, the Ar flow is 50sccm, heating the quartz substrate to 100 ℃, and continuously depositing for 30 min; placing the W film prepared by the magnetron sputtering method at the downstream of a double-temperature-zone tubular furnace, introducing Ar as protective gas, wherein the flow rate is 100 sccm; placing high-purity sulfur powder in the upper low-temperature region of the W film, setting the temperature to be 200 ℃, setting the temperature in the lower high-temperature region to be 1100 ℃, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain WS2A film;
step two: WS prepared by the above step one2The film is used as a substrate, and the W film is sputtered again by a magnetron sputtering method, wherein the parameters are the same as the steps; then placing the W film prepared by re-sputtering in the center of a tubular furnace, introducing Ar as protective gas, wherein the flow rate is 100 sccm; placing high-purity tellurium powder in an upstream low-temperature region of the film, setting the temperature to be 550 ℃, setting the temperature in a downstream high-temperature region to be 1100 ℃, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain the WTE2/WS2A heterojunction thin film;
step three: adopting 5 mass percent of PMMA anisole solution to spin-coat on the WTE2/WS2Spin coating the surface of the heterojunction film at 2000rpm for 10s, drying at 80 deg.C, and soaking in the solutionHeating in a strong alkali solution of 30 percent KOH to separate the film from the quartz substrate and float on the surface of the strong alkali solution; then rinsing with deionized water for three times, cutting into 2 × 2mm small pieces to obtain WTE-based products2/WS2Saturable absorber of heterojunction.
Based on WTE obtained by adopting the method2/WS2A mode-locked fiber laser is prepared by a saturable absorber of a heterojunction, the fiber pulse laser in the embodiment adopts an annular cavity structure, the wavelength of a pumping source is 980nm, and the central wavelength of a wavelength division multiplexer is 1064 nm. The wavelength division multiplexer 2 comprises a first input 9 and a second input 10, the fibre coupler 6 comprises a 75% output 11 and a 25% output 12; according to the sequence of a figure 1, an optical fiber fusion splicer is used for sequentially connecting a pumping source 1, a first input end 9 of a wavelength division multiplexer 2, an ytterbium-doped optical fiber 3, an optical isolator 4, a single-mode optical fiber 5, a 75% output end 11 of an optical fiber coupler 6, a polarization controller 7 and a saturable absorber 8 based on a tungsten ditelluride/tungsten disulfide heterojunction according to the sequence of the figure 1, and the saturable absorber based on the tungsten ditelluride/tungsten disulfide heterojunction is connected with a second input end 10 of the wavelength division multiplexer to form a cavity structure; the saturable absorber based on the tungsten ditelluride/tungsten disulfide heterojunction is transferred to the end face of an optical fiber jumper, is connected with another optical fiber jumper by using a flange disc and is arranged in an optical fiber flange, and the two ends of the saturable absorber are respectively connected with a second input end of the wavelength division multiplexer and the polarization controller by using single-mode optical fibers; the 25% output end 12 of the fiber coupler is connected with relevant instruments to measure the laser output characteristics of the fiber laser.
FIG. 2 is a WTE-based representation in example 12/WS2The mode-locked fiber laser of the saturable absorber of the heterojunction has a pulse sequence diagram, and the mode-locked pulse in the cavity works in a relatively stable state, and the pulse interval is 126.2 ns.
FIG. 3 is a WTE-based representation in example 12/WS2The pulse width of a single-pulse signal diagram of the mode-locked fiber laser of the saturable absorber of the heterojunction is 945 ps.
FIG. 4 is a WTE-based representation in example 12/WS2Radio frequency spectrum of mode-locked fiber laser of saturable absorber of heterojunctionThe signal-to-noise ratio of the pulse is 51dB, indicating that the pulse signal is very stable.
FIG. 5 is a WTE-based representation in example 12/WS2The output power of the mode-locked fiber pulse laser of the saturable absorber of the heterojunction and the pumping power are in a relation graph. As can be seen from fig. 5, the pulse output power gradually increases with the increase of the pump power, and the two are approximately in a linear relationship.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (7)

1. A preparation method of a saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction is characterized by comprising the following operation steps:
(1) sputtering of W: preparing a W film on a quartz substrate by a magnetron sputtering method, specifically, taking a W polycrystalline block as a target material, controlling the radio frequency power to be 80W, the sputtering pressure to be 1.2Pa, controlling the Ar flow to be 50sccm, heating the quartz substrate to 100 ℃, and continuously depositing for 5-30 min;
(2)WS2preparing a film: placing the W film prepared by the magnetron sputtering method at the downstream of the double-temperature-zone tubular furnace, introducing Ar as protective gas, wherein the flow rate is 100 sccm; placing high-purity sulfur powder in a low-temperature area at the upstream of the W film, setting the temperature to be 200 ℃, setting the temperature of a high-temperature area at the downstream to be 1050-1200 ℃, keeping the temperature for 3-5 hours, and then naturally cooling to room temperature;
(3) secondary sputtering of W: WS prepared in step (2)2The film is used as a substrate, and the W film is sputtered again by a magnetron sputtering method, wherein the parameters are the same as those in the step (1);
(4)WTe2/WS2preparing a heterojunction thin film: placing the film prepared by the secondary sputtering in the step (3) at the downstream of the double-temperature-zone tubular furnace, introducing Ar as protective gas, wherein the flow rate is 100 sccm; high-purity tellurium powder is placed in the upper low-temperature region of the film, and the temperature is set to be 550 ℃ belowSetting the temperature of a free high-temperature area to 1050-1200 ℃, keeping the temperature for 3-5 hours, and then naturally cooling to room temperature to obtain the WTE2/WS2A heterojunction thin film;
(5)WTe2/WS2and (3) stripping of the heterojunction film: adopting 5 mass percent of PMMA anisole solution to spin-coat the WTE prepared in the step (4)2/WS2The surface of the heterojunction film is dried at 80 ℃ at the spin-coating rotating speed of 1000-3000 rpm for 10-60 s, and then is soaked in a strong alkaline solution, and the film is heated to be separated from the quartz substrate and float on the surface of the strong alkaline solution; and then rinsing with deionized water, and cutting into small pieces to obtain the saturable absorber based on the tungsten ditelluride/tungsten disulfide heterojunction.
2. The method of claim 1, wherein the method comprises the following steps: the strong alkali solution in the step (5) is NaOH, KOH or a mixed solution of NaOH and KOH, the mass fraction of the strong alkali solution is 10-50%, and the strong alkali solution is heated to 50-90 ℃.
3. The method of claim 1, wherein the method comprises the following steps: the rinsing times in the step (5) are three times, and the size of the cut small pieces is 2 multiplied by 2 mm.
4. A saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction prepared by the production method according to any one of claims 1 to 3.
5. A mode-locked fiber laser made from the saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction as claimed in claim 4, wherein: the mode-locked fiber laser comprises a saturable absorber based on a tungsten ditelluride/tungsten disulfide heterojunction, a pumping source, a wavelength division multiplexer, an ytterbium-doped fiber, an optical isolator, a single-mode fiber, a fiber coupler and a polarization controller.
6. The mode-locked fiber laser of claim 5, wherein: the wavelength division multiplexer comprises a first input end and a second input end; the optical fiber coupler comprises 75% of output ends and 25% of output ends; the pump source, a first input end of the wavelength division multiplexer, the ytterbium-doped optical fiber, the optical isolator, the single-mode optical fiber, 75% of an output end of the optical fiber coupler, the polarization controller and the saturable absorber based on the double tungsten telluride/tungsten disulfide heterojunction are sequentially connected, and the saturable absorber based on the double tungsten telluride/tungsten disulfide heterojunction is connected with a second input end of the wavelength division multiplexer to form an annular cavity structure; the saturable absorber based on the tungsten ditelluride/tungsten disulfide heterojunction is transferred to the end face of the optical fiber jumper, is connected with another optical fiber jumper by using a flange disc, is arranged in an optical fiber flange, and is respectively connected with the second input end of the wavelength division multiplexer and the polarization controller by using single mode fibers at two ends.
7. The mode-locked fiber laser of claim 5, wherein: the wavelength of the pumping source is 980nm, and the central wavelength of the wavelength division multiplexer is 1064 nm.
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