CN114268013A - Saturable absorber manufacturing method, saturable absorber and laser - Google Patents
Saturable absorber manufacturing method, saturable absorber and laser Download PDFInfo
- Publication number
- CN114268013A CN114268013A CN202111592914.8A CN202111592914A CN114268013A CN 114268013 A CN114268013 A CN 114268013A CN 202111592914 A CN202111592914 A CN 202111592914A CN 114268013 A CN114268013 A CN 114268013A
- Authority
- CN
- China
- Prior art keywords
- optical fiber
- tin
- saturable absorber
- fiber
- micro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
The invention discloses a saturable absorber manufacturing method, a saturable absorber and a laser. The preparation method of the saturable absorber comprises synthesizing TiO2(ii) a According to TiO2Preparing TiN modified by Au; mixing TiN and isopropanol, and sequentially performing ultrasonic treatment and centrifugal treatment to obtain a centrifugal liquid; taking out the centrifugate and preparing TiN isopropanol dispersion liquid; preparing the single mode optical fiber into a micro-nano optical fiber through tapering equipment; and (3) dropping the TiN isopropanol dispersion liquid in the beam waist area of the micro-nano optical fiber, and introducing continuous laser into one end of the micro-nano optical fiber to prepare the saturable absorber deposited on the micro-nano optical fiber by TiN. The embodiment of the invention has the advantages that the saturable absorber is manufactured, the structure is simple, the stability is good, the cost is lower, and the saturable absorber can be applied to a harmonic mode-locked fiber laser to obtain stable high-repetition-frequency ultrashort pulses; the high repetition frequency mode-locked fiber laser based on TiN has simple structure, convenient operation, stability and reliability, and can generate stableThe fundamental frequency pulse, and can realize the ultrashort pulse output with high repetition frequency.
Description
Technical Field
The invention relates to the technical field of laser, in particular to a manufacturing method of a saturable absorber, the saturable absorber and a laser.
Background
Laser is one of the greatest inventions of human beings, has the advantages of good coherence, high energy density, strong stability and the like, and has become one of the most important tools in scientific research and industrial production.
With the development of the technology, the fiber laser can generate ultrashort pulses with high peak power, narrow pulse width and wide spectrum. Especially, the high repetition frequency ultrashort pulse fiber laser has been widely applied to the fields of optical frequency comb, optical communication, laser ranging, high-speed optical sampling, nonlinear optical biological imaging and the like, and is a introduction direction and research hotspot of laser technology development.
At present, there are three methods for obtaining high repetition frequency pulses: active mode locking, ultra-short cavity mode locking and passive harmonic mode locking. The active mode locking requires a high-frequency signal generator or other additional equipment outside a resonant cavity, so that the system cost and the structural complexity are increased; the ultra-short cavity mode locking can also obtain high repetition frequency pulse, but is limited by the physical length of the cavity, and further increase of the repetition rate is difficult. In contrast, passive harmonic mode locking is considered to be one of the simpler and more efficient methods of generating high repetition frequency pulses.
On the other hand, passive harmonic mode locking is one of the main techniques for generating ultrashort pulses in fiber lasers. The technology is that a saturable absorber is added into a laser resonant cavity, and ultrashort pulses are realized by utilizing the nonlinear absorption characteristic of the saturable absorber. Therefore, the core of the passive mode locking technology is to find a stable and reliable saturable absorber.
At present, the saturable absorber commonly used in the passive mode-locked laser mainly has two types, namely an equivalent saturable absorber and a true saturable absorber. Wherein equivalent saturable absorbers mainly include nonlinear polarization rotating and nonlinear amplifying ring mirrors, and at present, the actual commercial saturable absorbers are mainly semiconductor saturable absorbers. However, the nonlinear polarization rotation mode locking device has very high dependence on polarization, is particularly easily influenced by external factors such as optical fiber bending, external temperature, stress and vibration, and has poor stability; the mode locking threshold of the nonlinear amplification annular mirror device is high, and self-starting is difficult; the semiconductor saturable absorption mirror mode locking device has the advantages of complex manufacturing process, higher cost and narrow working wavelength range. Therefore, there is a great need to continuously search for a stable and reliable saturable absorber material, and to explore its application potential in high repetition frequency passive mode-locked fiber lasers.
Disclosure of Invention
The invention aims to provide a saturable absorber manufacturing method, a saturable absorber and a laser, and aims to solve the problem that saturable absorber materials are insufficient in stability and reliability in the prior art.
In a first aspect, an embodiment of the present invention provides a method for manufacturing a saturable absorber, including:
synthesis of TiO2；
According to the TiO2Preparing TiN modified by Au;
mixing the TiN and the isopropanol, and sequentially performing ultrasonic treatment and centrifugal treatment to obtain a centrifugal liquid;
taking out the centrifugate and preparing TiN isopropanol dispersion liquid;
preparing the single mode optical fiber into a micro-nano optical fiber through tapering equipment;
and dropping the TiN isopropanol dispersion liquid in a beam waist area of the micro-nano optical fiber, and introducing continuous laser into one end of the micro-nano optical fiber to prepare the saturable absorber deposited on the micro-nano optical fiber by TiN.
In a second aspect, an embodiment of the present invention provides a saturable absorber, which is manufactured by the above saturable absorber manufacturing method.
In a third aspect, an embodiment of the present invention provides a high repetition frequency mode-locked laser, including the saturable absorber, where the saturable absorber is connected in the laser, and further including a pump source, an optical fiber wavelength division multiplexer, a gain fiber, an optical fiber coupler, an optical fiber isolator, a polarization controller, and a single mode fiber, which are sequentially connected in an optical fiber fusion mode, where the saturable absorber is connected to the single mode fiber and the optical fiber wavelength division multiplexer, the gain fiber, the optical fiber coupler, the optical fiber isolator, the polarization controller, the single mode fiber, and the saturable absorber constitute a closed-loop cavity laser.
The embodiment of the invention has the advantages that the saturable absorber is manufactured, the structure is simple, the stability is good, the cost is lower, and the saturable absorber can be applied to a harmonic mode-locked fiber laser to obtain stable high-repetition-frequency ultrashort pulses;
the TiN-based high repetition frequency mode-locked fiber laser has the advantages of simple structure, convenience in operation, stability and reliability, and can generate stable fundamental frequency pulse and realize high repetition frequency ultrashort pulse output.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for manufacturing a saturable absorber according to an embodiment of the present invention;
FIG. 2 is a non-linear optical absorption curve of a saturable absorber of the present invention;
fig. 3 is a schematic structural diagram of a full fiber laser provided by the present invention;
FIG. 4 is a diagram of a fundamental frequency pulse spectrum of a high repetition frequency mode-locked laser provided by the present invention;
FIG. 5 is a timing diagram of the fundamental frequency pulse of the high repetition frequency mode-locked laser provided by the present invention;
FIG. 6 is a diagram of the fundamental frequency pulse RF of the high repetition frequency mode-locked laser provided by the present invention;
FIG. 7 is a fundamental frequency pulse autocorrelation diagram of a high repetition frequency mode-locked laser provided by the present invention;
FIG. 8 is a timing diagram of the high repetition frequency pulse of the high repetition frequency mode-locked laser provided by the present invention;
FIG. 9 is a high repetition frequency pulse spectrum of the high repetition frequency mode-locked laser provided by the present invention;
fig. 10 is a graph showing the variation of the harmonic order and the output power with the pump power in the high repetition frequency mode-locked laser provided by the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that the terms "comprises" and/or "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in the specification of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be further understood that the term "and/or" as used in this specification and the appended claims refers to and includes any and all possible combinations of one or more of the associated listed items.
Referring to fig. 1, a method for manufacturing a saturable absorber includes:
s101, synthesizing TiO2；
S102, according to the TiO2Preparing TiN modified by Au;
s103, mixing the TiN and the isopropanol, and sequentially performing ultrasonic treatment and centrifugal treatment to obtain a centrifugal liquid;
s104, taking out the centrifugate and preparing TiN isopropanol dispersion liquid;
s105, preparing the single-mode optical fiber into a micro-nano optical fiber through tapering equipment;
s106, dripping the TiN isopropanol dispersion liquid in a beam waist area of the micro-nano optical fiber, and introducing continuous laser into one end of the micro-nano optical fiber to prepare a saturable absorber deposited on the micro-nano optical fiber by TiN;
in the embodiment, the manufactured saturable absorber has the advantages of simple structure, good stability and lower cost, and can be applied to a harmonic mode-locked fiber laser to obtain stable high-repetition-frequency ultrashort pulses.
In one embodiment, the synthetic TiO2The method comprises the following steps:
dissolving 0.1-5g of tetrabutyl titanate and 0.36-18g of polyether in 3-150mL of ethanol to obtain a first ethanol solution;
adding 0.1-5mL of hydrochloric acid and 0.05-2.5mL of nitric acid into the first ethanol solution to obtain a second ethanol solution;
stirring the second ethanol solution for 24-72 hours, and drying at the constant temperature of 50-80 ℃ to obtain TiO2Prefabricating an object;
subjecting the TiO to a reaction2Placing the prefabricated object in a compressed air flow environment with the flow rate of 10-80mL/min, gradually heating to 300-500 ℃ at the heating rate of 1-10 ℃/min, and keeping for 3-5 hours to separate out TiO2。
In this embodiment, the mass ratio of each component is not particularly limited, and may be arranged as needed.
In a preferred embodiment, the components are prepared in the above-mentioned range, for example, 1g of tetrabutyl titanate and 3.6g of polyether are dissolved in 30mL of ethanol, 5g of tetrabutyl titanate and 18g of polyether are dissolved in 150mL of ethanol, and the preparation can be carried out similarly.
Preferably, the second ethanol solution is stirred for 48 hours.
Preferably, the temperature is gradually raised to 400 ℃ at a temperature raising rate of 1-10 ℃/min and kept for 4 hours.
In one embodiment, the TiO according to the formula2Making a TiN decorated with Au, comprising:
taking 1-5g of the TiO2Adding 20-100mL of water to obtain a first dissolved solution;
adding 0.01-0.05g of precursor salt containing Au into the first solution to obtain a second solution;
adding 0.01-0.1g of sodium hydroxide and 0.002-0.02g of sodium borohydride into the second dissolving solution to obtain a third dissolving solution;
after full reaction, carrying out dialysis treatment to obtain prefabricated powder;
placing the prefabricated powder in an ammonia gas flow environment with the flow rate of 30-100mL/min, gradually heating to 700-1000 ℃ at the heating rate of 1-10 ℃/min, and keeping for 5-8 hours;
after cooling to 150-250 ℃ in the ammonia gas flow environment, placing the prefabricated powder in a nitrogen gas flow environment with the flow rate of 10-60mL/min, cooling to room temperature in the nitrogen gas flow environment, and maintaining for 3-5 hours;
and placing the prefabricated powder in a compressed air flow environment with the flow rate of 10-30mL/min to obtain the Au modified TiN.
In this embodiment, the mass ratio of each component is not particularly limited, and may be arranged as needed.
In a preferred embodiment, the components are arranged in the above-mentioned proportions, for example in the proportion of 1g of the TiO mentioned2Adding into 20mL of water to obtain a first solution, wherein the amount of TiO is 3g2Adding 60mL of water to obtain a first dissolved solution, and preparing the first dissolved solution according to the actual conditions similarly.
Preferably, after cooling to 200 ℃ in the ammonia gas flow environment, the pre-formed powder is placed in a nitrogen gas flow environment with a flow rate of 10-60mL/min, cooled to room temperature in the nitrogen gas flow environment, and maintained for 4 hours.
Specifically, the modification of Au is to increase the optical nonlinear characteristics of TiN material.
In one embodiment, the TiO according to the formula2Making a TiN modified with Au, including：
Taking 1-5g of the TiO2Adding into 20-100mL dichloromethane to obtain a first dissolved solution;
adding 0.01-0.05g of organic complex containing Au into the first dissolved solution to obtain a second dissolved solution;
adding 0.01-0.1g of sodium hydroxide and 0.002-0.02g of sodium borohydride into the second dissolving solution to obtain a third dissolving solution;
after full reaction, carrying out dialysis treatment to obtain prefabricated powder;
placing the prefabricated powder in an ammonia gas flow environment with the flow rate of 30-100mL/min, gradually heating to 700-1000 ℃ at the heating rate of 1-10 ℃/min, and keeping for 5-8 hours;
after cooling to 150-250 ℃ in the ammonia gas flow environment, placing the prefabricated powder in a nitrogen gas flow environment with the flow rate of 10-60mL/min, cooling to room temperature in the nitrogen gas flow environment, and maintaining for 3-5 hours;
and placing the prefabricated powder in a compressed air flow environment with the flow rate of 10-30mL/min to obtain the Au modified TiN.
In this example, the only difference from the previous example is that the aqueous solution is replaced with dichloromethane, while the Au containing precursor salt is replaced with an Au containing organic complex.
In one embodiment, the Au-containing precursor salt is chloroauric acid or a potassium chloroauric acid salt.
In this example, two kinds of Au-containing precursor salts are given, specifically, not only chloroauric acid and potassium chloroaurate, but also other Au-containing precursor salts may be used.
In one embodiment, the Au-containing organic complex is gold acetylacetonate or gold triphenylphosphine chloride.
In this example, two Au-containing organic complexes are shown, specifically, not only gold acetylacetonate and triphenylphosphine chloride, but also other Au-containing organic complexes.
In an embodiment, the preparing of the saturable absorber comprises mixing TiN and isopropanol, sequentially performing ultrasonic treatment and centrifugal treatment to obtain a centrifugate, taking out the centrifugate and preparing a TiN isopropanol dispersion solution, preparing a single mode optical fiber into a micro-nano optical fiber through tapering equipment, dropping the TiN isopropanol dispersion solution in a beam waist region of the micro-nano optical fiber, and introducing continuous laser into one end of the micro-nano optical fiber to obtain the saturable absorber deposited on the micro-nano optical fiber by TiN, and comprises:
adding a plurality of TiN modified by Au into isopropanol, and sequentially carrying out ultrasonic treatment and centrifugal treatment on the obtained solution;
taking out the dispersion liquid obtained by centrifugation, and preparing into 0.1mg/mL-1mg/mL TiN isopropanol dispersion liquid;
preparing the single mode fiber into a micro-nano fiber with the beam waist diameter of 10-20 mu m by tapering equipment, wherein the insertion loss of the micro-nano fiber in a communication waveband is less than or equal to 0.5 dB;
dropping the TiN isopropanol dispersion liquid in a beam waist area of the micro-nano optical fiber;
and continuous laser is introduced into one end of the micro-nano optical fiber, the TiN is deposited on the beam waist surface of the micro-nano optical fiber under the action of the photophoresis force, and a saturable absorber of the TiN deposited micro-nano optical fiber is obtained, wherein the insertion loss of the saturable absorber in a communication waveband is less than or equal to 6 dB.
In this embodiment, the insertion loss of the beam waist region of the micro-nano optical fiber is controlled to be less than or equal to 0.5dB, and the micro-nano optical fiber can be replaced by an optical fiber with a side polishing structure; the concentration of TiN isopropanol dispersion liquid needs to be controlled between 0.1mg/mL and 1 mg/mL.
Sonication is treatment in an ultrasonic instrument and centrifugation is treatment in a centrifuge.
Preferably, the prepared TiN isopropanol dispersion liquid has the concentration of 0.5mg/mL, the beam waist diameter of the micro-nano optical fiber is 10 microns, 0.5mg/mL TiN isopropanol is dispersed and dropped in the beam waist area of the micro-nano optical fiber, and meanwhile, 100mW continuous laser is introduced into one end of the TiN isopropanol dispersion liquid.
A saturable absorber is manufactured by a saturable absorber manufacturing method.
In this embodiment, the saturable absorber can be manufactured by the above-mentioned saturable absorber manufacturing method.
As shown in fig. 2, the characteristics of the saturable absorber of the TiN deposited micro-nano fiber are further studied, and firstly, the nonlinear optical absorption characteristics of the TiN material in the communication waveband are measured by using a Z-scanning technology; it can be seen that the modulation depth is about 33%, which indicates that the TiN material exhibits excellent saturable absorption characteristics and can be used for making mode-locked devices for fiber lasers.
Referring to fig. 3, a high repetition frequency mode-locked laser includes the saturable absorber, the saturable absorber is connected in the laser, and the high repetition frequency mode-locked laser further includes a pump source 1, an optical fiber wavelength division multiplexer 2, a gain optical fiber 3, an optical fiber coupler 4, an optical fiber isolator 5, a polarization controller 6 and a single mode optical fiber 7 which are connected in sequence in an optical fiber fusion mode, the saturable absorber 8 is connected with the single mode optical fiber 7 and the optical fiber wavelength division multiplexer 2, the gain optical fiber 3, the optical fiber coupler 4, the optical fiber isolator 5, the polarization controller 6, the single mode optical fiber 7 and the saturable absorber 8 constitute a closed-loop laser.
In this embodiment, the fiber fusion loss is less than or equal to 0.5 dB;
wherein, the pumping source 1 is a semiconductor laser, the output wavelength is 980nm, and the output power is 0-600 mW;
the optical fiber wavelength division multiplexer 2 is an 980/1550 type optical fiber device, has an insertion loss less than 0.2dB, and can bear 1W of pump power and 300mW of signal power.
The gain fiber 3 is a single-mode erbium-doped fiber, and different lengths can be selected according to different absorption coefficients and dispersion values.
The optical fiber coupler 4 has various options, and can be any one of the optical fiber coupling ratios of 20: 80, 30: 70, 10: 90 and 40: 60.
The optical fiber isolator 5 is an optical fiber polarization-independent isolator, unidirectional transmission of laser in a cavity is guaranteed, the maximum isolation degree is less than or equal to 30dB, the insertion loss is less than 0.5dB, and the maximum bearable power is 300 mW.
The polarization controller 6 may be a polarization controller of a three-ring structure, or may be a polarization controller of a squeeze structure.
The single-mode fiber 7 increases the nonlinear characteristic in the cavity, so that the laser can generate ultrashort pulses more easily, and the length is 5-30 m.
The saturable absorber 8 has a nonlinear optical absorption function in the fiber laser, and can be used as a mode locking device to enable the laser to generate ultrashort pulse output.
In one embodiment, the output end of the pump source 1 is connected to the pump end a of the fiber wavelength division multiplexer 2, and the output end b of the fiber wavelength division multiplexer 2 is connected to one end of the gain fiber 3; the other end of the gain fiber 3 is connected with the input end of the fiber coupler 4, the first output end d of the fiber coupler 4 is used as the output of the laser, the second output end e of the fiber coupler 4 is connected with the input end of the fiber isolator 5, the output end of the fiber isolator 5 is connected with the input end of the polarization controller 6, the output end of the polarization controller 6 is connected with the input end of the single-mode fiber 7, the output end of the single-mode fiber 7 is connected with the input end of the saturable absorber 8, and the output end of the saturable absorber 8 is connected with the signal end c of the fiber wavelength division multiplexer 2.
Preferably, the gain fiber 3 is a single-mode erbium-doped fiber, which is an EDF80 fiber of the OFS, the length of the fiber is 1.2m, and the dispersion coefficient at 1550nm is-48 ps/(nm-km);
preferably, the optical fiber coupler 4 has a coupling ratio of 30: 70, wherein 30% is an output end;
preferably, the single-mode fiber 7 is a common single-mode fiber in a communication waveband, and is a standard G652-type fiber, and the length is 20 m;
preferably, the cavity length of the entire laser is about 32.5 m.
The feasibility of the invention was verified by experimental data as follows:
when the pumping power is dozens of mW, the fiber laser can output continuous laser. As the pump power continues to increase, mode-locked pulses begin to occur.
When the pumping power is increased to 60mW, the polarization state of the cavity is changed by properly adjusting the polarization controller, and then stable fundamental frequency mode-locked pulses can be obtained; referring to FIG. 4, the spectrum of the fundamental frequency pulse at the pump power is shown; clearly, there are some clear sidebands on the spectrum.
The central wavelength of the mode locking pulse is 1558.49nm, and the 3dB spectral bandwidth is 1.96 nm; referring to fig. 5, it can be seen that the adjacent pulses are spaced approximately 162.4ns apart, from which a repetition rate of 6.156MHz, the fundamental frequency, can be calculated.
Referring to fig. 6, the repetition frequency of the mode-locked pulse is 6.156MHz, which is consistent with the cavity length of the fiber laser of 32.5m and the measured pulse timing period of 162.4ns, and the signal-to-noise ratio (SNR) is about 65.8dB, indicating that the mode-locked pulse state has good stability.
Referring to fig. 7, the full-height-at-half-maximum (FWHM) of the fundamental pulse is about 2.25ps, and the pulse width is about 1.46ps by hyperbolic sect (Sech2) formula fitting. Through calculation, the time-bandwidth product (TBP) of the pulse at the moment is about 0.353, which is larger than the transformation limit of the hyperbolic secant pulse by 0.315, and the output mode-locked pulse has certain chirp.
With the pump power being increased, and the angle of the polarization controller being adjusted appropriately, the fundamental mode-locked pulse is converted into a harmonic mode-locked pulse, as shown in fig. 8, the interval between adjacent pulses is about 0.99ns, and the corresponding calculated repetition frequency is about 1.01 GHz; from a repetition rate of 6.156MHz, it can be seen that the mode-locked pulse at 1.01GHz corresponds to 164 th order harmonic mode locking, see fig. 9, with a center wavelength of 1558.28nm and a 3dB spectral bandwidth of 2.28 nm.
Referring to fig. 10, in order to better show the performance of the harmonic mode-locked fiber laser, the harmonic order and the average output power at different pump powers were measured.
Referring to fig. 10, it is clear that as the pump power increases, both the harmonic order and the output power increase substantially linearly with the pump power. When the pump power is increased from 100mW to 580mW, the harmonic mode locking order is increased from 22 to 164, and the average output power is increased from 3.69mW to 29.04 mW.
These findings are consistent with the typical characteristics of harmonic mode-locked fiber lasers.
The high repetition frequency mode-locked fiber laser based on the saturable absorber can obtain stable fundamental frequency pulse and can realize ultrashort pulse with repetition frequency as high as 1 GHz.
While the invention has been described with reference to specific embodiments, the invention is not limited thereto, and various equivalent modifications and substitutions can be easily made by those skilled in the art within the technical scope of the invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for manufacturing a saturable absorber is characterized by comprising the following steps:
synthesis of TiO2；
According to the TiO2Preparing TiN modified by Au;
mixing the TiN and the isopropanol, and sequentially performing ultrasonic treatment and centrifugal treatment to obtain a centrifugal liquid;
taking out the centrifugate and preparing TiN isopropanol dispersion liquid;
preparing the single mode optical fiber into a micro-nano optical fiber through tapering equipment;
and dropping the TiN isopropanol dispersion liquid in a beam waist area of the micro-nano optical fiber, and introducing continuous laser into one end of the micro-nano optical fiber to prepare the saturable absorber deposited on the micro-nano optical fiber by TiN.
2. The method of claim 1, wherein the synthetic TiO is selected from the group consisting of2The method comprises the following steps:
dissolving 0.1-5g of tetrabutyl titanate and 0.36-18g of polyether in 3-150mL of ethanol to obtain a first ethanol solution;
adding 0.1-5mL of hydrochloric acid and 0.05-2.5mL of nitric acid into the first ethanol solution to obtain a second ethanol solution;
to the second alcoholStirring the solution for 24-72 hours, and drying at the constant temperature of 50-80 ℃ to obtain TiO2Prefabricating an object;
subjecting the TiO to a reaction2Placing the prefabricated object in a compressed air flow environment with the flow rate of 10-80mL/min, gradually heating to 300-500 ℃ at the heating rate of 1-10 ℃/min, and keeping for 3-5 hours to separate out TiO2。
3. The method of claim 2, wherein the TiO is selected from the group consisting of2Making a TiN decorated with Au, comprising:
taking 1-5g of the TiO2Adding 20-100mL of water to obtain a first dissolved solution;
adding 0.01-0.05g of precursor salt containing Au into the first solution to obtain a second solution;
adding 0.01-0.1g of sodium hydroxide and 0.002-0.02g of sodium borohydride into the second dissolving solution to obtain a third dissolving solution;
after full reaction, carrying out dialysis treatment to obtain prefabricated powder;
placing the prefabricated powder in an ammonia gas flow environment with the flow rate of 30-100mL/min, gradually heating to 700-1000 ℃ at the heating rate of 1-10 ℃/min, and keeping for 5-8 hours;
after cooling to 150-250 ℃ in the ammonia gas flow environment, placing the prefabricated powder in a nitrogen gas flow environment with the flow rate of 10-60mL/min, cooling to room temperature in the nitrogen gas flow environment, and maintaining for 3-5 hours;
and placing the prefabricated powder in a compressed air flow environment with the flow rate of 10-30mL/min to obtain the Au modified TiN.
4. The method of claim 2, wherein the TiO is selected from the group consisting of2Making a TiN decorated with Au, comprising:
taking 1-5g of the TiO2Adding into 20-100mL dichloromethane to obtain a first dissolved solution;
adding 0.01-0.05g of organic complex containing Au into the first dissolved solution to obtain a second dissolved solution;
adding 0.01-0.1g of sodium hydroxide and 0.002-0.02g of sodium borohydride into the second dissolving solution to obtain a third dissolving solution;
after full reaction, carrying out dialysis treatment to obtain prefabricated powder;
placing the prefabricated powder in an ammonia gas flow environment with the flow rate of 30-100mL/min, gradually heating to 700-1000 ℃ at the heating rate of 1-10 ℃/min, and keeping for 5-8 hours;
after cooling to 150-250 ℃ in the ammonia gas flow environment, placing the prefabricated powder in a nitrogen gas flow environment with the flow rate of 10-60mL/min, cooling to room temperature in the nitrogen gas flow environment, and maintaining for 3-5 hours;
and placing the prefabricated powder in a compressed air flow environment with the flow rate of 10-30mL/min to obtain the Au modified TiN.
5. A method of manufacturing a saturable absorber according to claim 3, wherein: the precursor salt containing Au is chloroauric acid or potassium chloroauric acid salt.
6. The method for manufacturing a saturable absorber according to claim 4, wherein: the organic complex containing Au is acetylacetone gold or triphenylphosphine gold chloride.
7. The method for manufacturing the saturable absorber according to claim 3 or 4, wherein the TiN and isopropanol are mixed and sequentially subjected to ultrasonic treatment and centrifugal treatment to obtain a centrifugate, the centrifugate is taken out and prepared into TiN isopropanol dispersion liquid, a single mode fiber is prepared into a micro-nano fiber through tapering equipment, the TiN isopropanol dispersion liquid is dropped in a beam waist region of the micro-nano fiber, and continuous laser is introduced into one end of the micro-nano fiber to prepare the saturable absorber deposited on the micro-nano fiber by the TiN, and the method comprises the following steps:
adding a plurality of TiN modified by Au into isopropanol, and sequentially carrying out ultrasonic treatment and centrifugal treatment on the obtained solution;
taking out the dispersion liquid obtained by centrifugation, and preparing into 0.1mg/mL-1mg/mL TiN isopropanol dispersion liquid;
preparing the single mode fiber into a micro-nano fiber with the beam waist diameter of 10-20 mu m by tapering equipment, wherein the insertion loss of the micro-nano fiber in a communication waveband is less than or equal to 0.5 dB;
dropping the TiN isopropanol dispersion liquid in a beam waist area of the micro-nano optical fiber;
and continuous laser is introduced into one end of the micro-nano optical fiber, the TiN is deposited on the beam waist surface of the micro-nano optical fiber under the action of the photophoresis force, and a saturable absorber of the TiN deposited micro-nano optical fiber is obtained, wherein the insertion loss of the saturable absorber in a communication waveband is less than or equal to 6 dB.
8. A saturable absorber produced by the method for producing a saturable absorber according to any one of claims 1 to 7.
9. A high repetition frequency mode-locked laser, characterized by, include the saturable absorber of claim 8, the saturable absorber connect in the laser, still include pump source, fiber wavelength division multiplexer, gain fiber, fiber coupler, fiber isolator, polarization controller and the single mode fiber that connect gradually through the mode of fiber fusion, the saturable absorber connect the single mode fiber with fiber wavelength division multiplexer, gain fiber, fiber coupler, fiber isolator, polarization controller, single mode fiber and saturable absorber constitute the closed loop cavity laser.
10. The high repetition frequency mode-locked laser of claim 9, wherein: the output end of the pumping source is connected with the pumping end a of the optical fiber wavelength division multiplexer, and the output end b of the optical fiber wavelength division multiplexer is connected with one end of the gain optical fiber; the other end of the gain optical fiber is connected with the input end of the optical fiber coupler, the first output end d of the optical fiber coupler serves as the output of the laser, the second output end e of the optical fiber coupler is connected with the input end of the optical fiber isolator, the output end of the optical fiber isolator is connected with the input end of the polarization controller, the output end of the polarization controller is connected with the input end of the single-mode optical fiber, the output end of the single-mode optical fiber is connected with the input end of the saturable absorber, and the output end of the saturable absorber is connected with the signal end c of the optical fiber wavelength division multiplexer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111592914.8A CN114268013B (en) | 2021-12-23 | 2021-12-23 | Saturable absorber manufacturing method, saturable absorber and laser |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111592914.8A CN114268013B (en) | 2021-12-23 | 2021-12-23 | Saturable absorber manufacturing method, saturable absorber and laser |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114268013A true CN114268013A (en) | 2022-04-01 |
| CN114268013B CN114268013B (en) | 2022-08-23 |
Family
ID=80829355
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111592914.8A Active CN114268013B (en) | 2021-12-23 | 2021-12-23 | Saturable absorber manufacturing method, saturable absorber and laser |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114268013B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5701319A (en) * | 1995-10-20 | 1997-12-23 | Imra America, Inc. | Method and apparatus for generating ultrashort pulses with adjustable repetition rates from passively modelocked fiber lasers |
| US20110158265A1 (en) * | 2009-12-30 | 2011-06-30 | Industrial Technology Research Institute | Ring or linear cavity of all-fiber-based ultra short pulse laser system and method of operating the same |
| CN103318956A (en) * | 2013-07-11 | 2013-09-25 | 苏州大学 | Titanium dioxide nanowire preparation method |
| CN104475079A (en) * | 2014-12-12 | 2015-04-01 | 青岛润国生态科技发展有限公司 | Preparation method of supported photocatalytic composite material |
| CN109361142A (en) * | 2018-09-06 | 2019-02-19 | 浙江大学 | It is a kind of based on the saturable absorber device of TiN nano material and application |
-
2021
- 2021-12-23 CN CN202111592914.8A patent/CN114268013B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5701319A (en) * | 1995-10-20 | 1997-12-23 | Imra America, Inc. | Method and apparatus for generating ultrashort pulses with adjustable repetition rates from passively modelocked fiber lasers |
| US20110158265A1 (en) * | 2009-12-30 | 2011-06-30 | Industrial Technology Research Institute | Ring or linear cavity of all-fiber-based ultra short pulse laser system and method of operating the same |
| CN103318956A (en) * | 2013-07-11 | 2013-09-25 | 苏州大学 | Titanium dioxide nanowire preparation method |
| CN104475079A (en) * | 2014-12-12 | 2015-04-01 | 青岛润国生态科技发展有限公司 | Preparation method of supported photocatalytic composite material |
| CN109361142A (en) * | 2018-09-06 | 2019-02-19 | 浙江大学 | It is a kind of based on the saturable absorber device of TiN nano material and application |
Non-Patent Citations (6)
| Title |
|---|
| SHIPENG DING: "《Electrostatic stabilization of single atom catalysts by lonic liquids》", 《CELL PRESS》 * |
| YUJIE HAN等: "《Hydrogen evolution reaction in acidic media on single crystalline titanium nitride nanowires》", 《JOURNAL MATERIALS OF CHEMISTRY A 》 * |
| ZHANG BIN等: "《Atomically dispersed pt polyoxometalate catalysts》", 《JOURNAL OF AMERICAN CHEMICAL SOCIETY》 * |
| ZHANG BIN等: "《Gold Nanocluster-Modified Titanium Nitride for Ultrafast Photonics Applications》", 《ADVANCED ELECTRONIC MATERIALS》 * |
| ZHANG BIN等: "《Stabilizing a platinum, single atom catalyst on supported phosphomolybdic acid without compromising hydrogenation activity》", 《ANGEWANDTE CHEMIE》 * |
| ZHANG BIN等: "《Versatile applications of metal single atom 2d material nanoplatforms》", 《ADVANCED SCIENCE》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114268013B (en) | 2022-08-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100452569C (en) | Optical parameter chirp impulse amplification laser system | |
| CN103124044B (en) | Frequency interval adjustable multi-wavelength anti-Stokes four-wave mixing (FWM) fiber laser | |
| Ab Rahman et al. | Ultrashort pulse soliton fiber laser generation with integration of antimony film saturable absorber | |
| CN103151682B (en) | Anti-Strokes Raman fiber laser achieving multi-wavelength output | |
| CN109038191B (en) | Spectrum limited Fourier domain mode-locked fiber laser | |
| CN107302179B (en) | A kind of sub- hundred femtosecond ultra-short pulse generation devices of compact-sized all -fiber | |
| Salman et al. | Multiwavelength Q-switched erbium-doped fibre laser-based aluminum nanoparticles saturable absorber and Sagnac loop filter | |
| CN110589787A (en) | Nickel-phosphorus-sulfur two-dimensional material and synthesis and application thereof | |
| CN107634445B (en) | Mixed mode-locked pulse laser based on nonlinear polarization rotation technology and graphite alkyne | |
| CN114268013B (en) | Saturable absorber manufacturing method, saturable absorber and laser | |
| Rizman et al. | Q-switched and tunable wavelength fiber laser utilizing nickel oxide saturable absorber and sagnac loop mirror filter | |
| Ahmad et al. | All fiber normal dispersion mode locked ytterbium doped double-clad fiber laser using fiber taper with WS2-ZnO saturable absorber | |
| CN109842013A (en) | A kind of saturable absorption device, preparation method and fiber pulse laser | |
| CN109672075A (en) | A kind of preparation method of multi-wavelength optical fiber laser and its curing nickel mode-locking device | |
| CN109787075A (en) | A kind of dual wavelength mode locked fiber laser based on stannic disulfide mode locker | |
| CN111463651A (en) | Tuning method for working wavelength of ultrashort pulse fiber laser | |
| CN111653930A (en) | Saturable absorber based on boron-alkene two-dimensional material, preparation method thereof and mode-locked pulse laser | |
| CN110589782B (en) | Vanadium diselenide two-dimensional material and synthesis and application thereof | |
| CN201054063Y (en) | Optical parametric chirped pulse amplification laser system | |
| CN115632297A (en) | C-waveband passive Q-switched pulse fiber laser and preparation method of saturable absorber based on CsPbBr3 perovskite nanocrystalline | |
| CN109904715A (en) | A kind of 1064nm self-locking mode polarization-maintaining ytterbium-doping optical fiber laser of low repetition | |
| CN115377785A (en) | Preparation method and application of saturable absorber based on carbon nano onion particles | |
| CN110380324B (en) | Ultrashort pulse fiber laser | |
| CN112164971B (en) | Based on delta-MnO2Saturable absorber of nanosheet, preparation method and application in passive Q-switched optical fiber laser | |
| CN114665368A (en) | Ytterbium-doped intracavity cascade Raman fiber laser |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |