CN110255882B - Tm/Tb co-doped quartz optical fiber for 1.7 mu m optical fiber laser and preparation method thereof - Google Patents
Tm/Tb co-doped quartz optical fiber for 1.7 mu m optical fiber laser and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
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- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
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- H01S3/063—Waveguide lasers, i.e. whereby the dimensions of the waveguide are of the order of the light wavelength
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- 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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- H—ELECTRICITY
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- 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
- H01S3/06708—Constructional details of the fibre, e.g. compositions, cross-section, shape or tapering
- H01S3/06729—Peculiar transverse fibre profile
- H01S3/06733—Fibre having more than one cladding
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Abstract
The invention provides a Tm/Tb co-doped quartz optical fiber for a 1.7 mu m optical fiber laser and a preparation method thereof, wherein the optical fiber has the characteristics of uniform doping of rare earth ions, proper fluorescence center wavelength, high signal gain and the like. The optical fiber consists of a core layer, an inner cladding layer and an outer cladding layer, and is prepared by utilizing a chemical vapor deposition Method (MCVD) and combining a Chelate Precursor Doping Technology (CPDT), wherein the core layer comprises the following formula components: tm (thd)3：0.5～2％、SiCl4：30～50％、GeCl4：5～20％、SiF4：10～20％、POCl3：10～20％、AlCl3: 5-10%, the inner cladding formula component is: tb (thd)3：0.5～2％、SiCl4：30～50％、GeCl4：5～20％、SiF4：10～20％、POCl3：10～20％、AlCl3：5～10％。
Description
Technical Field
The invention belongs to the technical field of optical fibers, and relates to a quartz optical fiber for a 1.7-micrometer optical fiber laser and a preparation method thereof.
Background
The 1.7 mu m wave band is just positioned at the wave trough position between two strong absorption wave bands (1400-1600 nm and 1900-2200 nm) of water, so that the absorption of water molecules to the wave bands is very small. In addition to this, the 1.7 μm band is exactly the strongest absorption band of C-H bonds in the polymer molecule. The unique characteristics of the 1.7 mu m wave band enable the wave band ultrafast laser to have excellent application prospect in the fields of Optical Coherence Tomography (OCT), laser medical treatment, femtosecond photon microscopic imaging, laser processing, femtosecond optical frequency comb, multiphoton microscopy (MPM) and the like.
At present, thulium-doped silica fiber is the main gain matrix in a 1.7 μm band fiber laser. However, the optical fiber has many defects of too long fluorescent center wavelength, small signal gain and the like, and the phenomena of signal light gain saturation, signal light reabsorption and the like are very easy to occur in the laser operation process of the 1.7-micron optical fiber based on the thulium-doped quartz optical fiber. The absence of this band effective gain fiber greatly limits the increase in laser power and laser efficiency. Therefore, the search for a new type of gain fiber suitable for this band becomes the key point to solve this problem.
Due to Tb3+Has strong absorption effect in the wave band of 1.75-2.0 mu m and passes through Tm3+/Tb3+Co-doping makes it possible to achieve Tm in silica fibers3+The quantitative regulation and control of the fluorescence center wavelength and the gain spectrum have the characteristics of both proper gain spectrum and matching of optical fiber devices, and are the best candidate gain materials for the research of 1.7 mu m optical fiber lasers.
According to different requirements, the codopant ions of the quartz optical fiber are selected differently, but generally only aim at the core layer (codoped into the core layer); due to the limitation of a plurality of factors such as preparation technology, doping technology and the like, how to realize controllable uniform doping becomes a difficult point. Perhaps, at present, there is no Tm in connection with the world3+/Tb3+The structure of the co-doped silica optical fiber and the related report of the preparation.
Disclosure of Invention
In order to solve the problem of the deletion of a proper gain optical fiber for a 1.7 mu m optical fiber laser, the invention provides a Tm/Tb co-doped quartz optical fiber for the 1.7 mu m optical fiber laser and a preparation method thereof, wherein the optical fiber has the characteristics of uniform doping of rare earth ions, proper fluorescence center wavelength, high signal gain and the like, and is particularly suitable for being used as a 1.7 mu m waveband gain optical fiber.
The technical scheme adopted by the invention is as follows:
the Tm/Tb co-doped quartz optical fiber for the 1.7 mu m optical fiber laser consists of a core layer, an inner cladding layer and an outer cladding layer, wherein the core layer comprises the following formula components in percentage by mass: tm (thd)3：0.5～2％、SiCl4：30～50％、GeCl4：5～20％、SiF4：10～20％、POCl3：10～20％、AlCl3: 5-10% of inner claddingThe formula comprises the following components: tb (thd)3：0.5～2％、SiCl4：30～50％、GeCl4：5～20％、SiF4：10～20％、POCl3：10～20％、AlCl3: 5-10%, the outer cladding layer comprises the following formula components: SiCl4：40～50％、GeCl4：5～15％、SiF4：20～30％、POCl3：10～15％。
Preferably, the cross-sectional shapes of the core layer, the inner cladding and the outer cladding are three concentric circles/rings (the whole concentric structure is a cylindrical structure) from inside to outside, wherein the diameter of the core layer is 6-10 μm, the diameter of the inner cladding is 10-30 μm, and the diameter of the outer cladding is 125-130 μm.
The invention also provides a preparation method of the Tm/Tb co-doped quartz optical fiber for the 1.7 mu m optical fiber laser, which comprises the following steps:
1) tm is measured by chemical vapor deposition (MCVD) combined with Chelate Precursor Doping Technology (CPDT)3+With chelate Tm (thd)3The components of the core layer formula are doped in the form of (1), and the doped components are uniformly introduced into a quartz tube to be deposited to form a prefabricated rod core layer; then Tb is added3+With chelate Tb (thd)3The components of the inner cladding formula are doped in the form of (1), and are uniformly introduced into a quartz tube to deposit on the surface of a core layer of a prefabricated rod to form an inner cladding of the prefabricated rod; uniformly introducing the formula components of the outer cladding layer into a quartz tube, and depositing on the surface of the inner cladding layer of the prefabricated rod to form the outer cladding layer of the prefabricated rod; wherein the size ratio among the core layer, the inner cladding layer and the outer cladding layer is controlled by adjusting the deposition cycle times; finally, forming an optical fiber preform through high-temperature sintering and rod shrinking processes;
2) and drawing the prepared optical fiber preform into the optical fiber with the required size in a quartz optical fiber drawing tower by using a hot drawing method.
Preferably, in the step 1), the deposition temperature is 1300-1450 ℃, and the pressure difference in the deposition tube is kept at 50-120 Pa; the sintering temperature is 1850-1950 ℃; the rod-shrinking temperature is 2050-2150 ℃, and the pressure difference is reduced to 20-40 Pa.
Preferably, in the step 2), the fiber drawing temperature is 1950-2100 ℃, the preform rod feeding speed is 0.2-0.5 mm/min, and the drawn fiber size is 125-130 μm.
The invention has the advantages that:
1. the quartz optical fiber consists of a core layer, an inner cladding and an outer cladding, wherein Tm is doped in the core layer3+Tb is doped in the inner cladding3+Through Tb3+Co-doping to achieve Tm3+Quantitative regulation and control of fluorescence spectrum; the fluorescence gain spectrum range is 1650-1750 nm, and the fluorescence center wavelength is 1700-1730 nm. Compared with the traditional thulium-doped quartz optical fiber, the fluorescence center wavelength of the invention is closer to the 1.7 mu m wave band, the signal gain is high, and the invention is an ideal gain optical fiber for a 1.7 mu m optical fiber laser.
2. The quartz optical fiber is prepared by adopting mature MCVD + CPDT technology, the structure and doping concentration of the optical fiber are controllable, and Tm can be effectively ensured3+And Tb3+The doping concentration of the rare earth ions and the uniformity of the rare earth ions are high, and the method has the advantages of high success rate, good repeatability, simplicity in operation and the like.
3. Compared with the rare earth doped fluoride optical fiber and other soft glass gain optical fiber materials, the quartz optical fiber has high damage-resistant threshold power and low transmission loss of a 1.7 mu m wave band, has a mature optical fiber device matched with the quartz optical fiber, and is more suitable for being used as a gain optical fiber material of a 1.7 mu m optical fiber laser.
Description of the drawings:
FIG. 1 is a schematic end view of an optical fiber; in the figure, 1-core layer, 2-inner cladding layer, 3-outer cladding layer.
FIG. 2 is a graph showing the fluorescence spectrum of the optical fiber obtained in example 1.
Detailed Description
The invention is further described below with reference to examples and figures.
Example 1
1) Tm is measured by chemical vapor deposition method and chelate precursor doping technology3+And Tb3+With chelate Tm (thd)3Tb (thd) is mixed into the deposited layer in the quartz tube in turn to form prefabricated rod core layer and inner cladding layer, then the formula composition of adjacent deposited layer is regulated to form outer cladding layer structure, finally the high-temp. sintering and rod-reducing process are implemented to form optical fibre prefabricated rod. Wherein the core layerThe formula comprises the following components: tm (thd)3：0.5％、SiCl4：35％、GeCl4：20％、SiF4：18％、POCl3：20％、AlCl3: 6.5%, the formula of the inner cladding comprises the following components: tb (thd)3：2％、SiCl4：35％、GeCl4：20％、SiF4：18％、POCl3：20％、AlCl3: 5%, the outer cladding formula comprises the following components: SiCl4：40％、GeCl4：15％、SiF4：30％、POCl3: 15 percent. Wherein the deposition temperature is 1300 ℃, and the pressure difference in the deposition tube is kept at 50 Pa; the sintering temperature is 1850 ℃; the rod-shrinking temperature is 2050 ℃, and the pressure difference is reduced to 20 Pa.
2) The prepared optical fiber preform is drawn into an optical fiber with the size of 125 μm in a quartz optical fiber drawing tower by a hot drawing method under the conditions that the drawing temperature is 1950 ℃ and the rod feeding speed is 0.2 mm/m. The optical fiber is characterized in that the diameters of a core layer 1, an inner cladding layer 2 and an outer cladding layer 3 are respectively 6, 10 and 125 mu m (as shown in figure 1), and the refractive index difference between the core layer and the inner cladding layer is 0.2 percent.
The optical fiber is pumped by an optical fiber laser with the output wavelength of 1550nm, and the optical fiber fluorescence spectrum (shown in figure 2) is obtained through testing, wherein the gain spectrum range is 1650-1750 nm, and the fluorescence center wavelength is 1707 nm.
Example 2
1) Tm is measured by chemical vapor deposition method and chelate precursor doping technology3+And Tb3+With chelate Tm (thd)3Tb (thd) is mixed into the deposited layer in the quartz tube in turn to form prefabricated rod core layer and inner cladding layer, then the formula composition of adjacent deposited layer is regulated to form outer cladding layer structure, finally the high-temp. sintering and rod-reducing process are implemented to form optical fibre prefabricated rod. Wherein the core layer comprises the following formula components: tm (thd)3：1％、SiCl4：40％、GeCl4：18％、SiF4：17％、POCl3：18％、AlCl3: 6%, the formula of the inner cladding comprises the following components: tb (thd)3：1％、SiCl4：40％、GeCl4：18％、SiF4：17％、POCl3：18％、AlCl3: 6%, the outer cladding formula comprises the following components: SiCl4：45％、GeCl4：13％、SiF4：27％、POCl3: 15 percent. Wherein the deposition temperature is 1350 ℃, and the pressure difference in the deposition tube is kept at 85 Pa; the sintering temperature is 1900 ℃; the rod shrinkage temperature was 2100 ℃ and the pressure difference was reduced to 30 Pa.
2) The prepared optical fiber preform is drawn into an optical fiber with the size of 128 mu m in a quartz optical fiber drawing tower by a hot drawing method under the conditions that the drawing temperature is 2000 ℃ and the rod feeding speed is 0.35 mm/m. The optical fiber is characterized in that the diameters of a core layer 1, an inner cladding layer 2 and an outer cladding layer 3 are respectively 8, 15 and 128 mu m, and the refractive index difference between the core layer and the inner cladding layer is 0.4 percent.
And pumping the optical fiber by adopting an optical fiber laser with the output wavelength of 1550nm, and testing to obtain the optical fiber fluorescence spectrum, wherein the gain spectrum range is about 1660-1760 nm, and the fluorescence center wavelength is 1715 nm.
Example 3
1) Tm is measured by chemical vapor deposition method and chelate precursor doping technology3+And Tb3+With chelate Tm (thd)3Tb (thd) is mixed into the deposited layer in the quartz tube in turn to form prefabricated rod core layer and inner cladding layer, then the formula composition of adjacent deposited layer is regulated to form outer cladding layer structure, finally the high-temp. sintering and rod-reducing process are implemented to form optical fibre prefabricated rod. Wherein the core layer comprises the following formula components: tm (thd)3：2％、SiCl4：50％、GeCl4：15％、SiF4：15％、POCl3：13％、AlCl3: 5%, the formula of the inner cladding comprises the following components: tb (thd)3：0.5％、SiCl4：50％、GeCl4：15％、SiF4：15％、POCl3：13％、AlCl3: 6.5%, the outer cladding formula comprises the following components: SiCl4：50％、GeCl4：10％、SiF4：25％、POCl3: 15 percent. Wherein the deposition temperature is 1450 ℃, and the pressure difference in the deposition tube is kept at 120 Pa; the sintering temperature is 1950 ℃; the rod shrinkage temperature is 2150 ℃, and the pressure difference is reduced to 40 Pa.
2) The prepared optical fiber preform is drawn into an optical fiber with the size of 130 μm in a quartz optical fiber drawing tower by a hot drawing method under the conditions that the drawing temperature is 2100 ℃ and the rod feeding speed is 0.5 mm/m. The optical fiber is characterized in that the diameters of a core layer 1, an inner cladding layer 2 and an outer cladding layer 3 are respectively 10, 30 and 130 mu m, and the refractive index difference between the core layer and the inner cladding layer is 0.6%.
And pumping the optical fiber by adopting an optical fiber laser with the output wavelength of 1550nm, and testing to obtain the optical fiber fluorescence spectrum, wherein the gain spectrum range is about 1675-1770 nm, and the fluorescence center wavelength is 1724 nm.
Claims (5)
1. A Tm/Tb co-doped silica fiber for a 1.7 μm fiber laser, characterized in that: the composite material consists of a core layer, an inner cladding and an outer cladding, wherein the core layer comprises the following formula components in percentage by mass: tm (thd)3：0.5～2％、SiCl4：30～50％、GeCl4：5～20％、SiF4：10～20％、POCl3：10～20％、AlCl3: 5-10%, the formula of the inner cladding comprises the following components: tb (thd)3：0.5～2％、SiCl4：30～50％、GeCl4：5～20％、SiF4：10～20％、POCl3：10～20％、AlCl3: 5-10%, the outer cladding layer comprises the following formula components: SiCl4：40～50％、GeCl4：5～15％、SiF4：20～30％、POCl3：10～15％。
2. The Tm/Tb co-doped silica fiber for a 1.7 μm fiber laser according to claim 1, wherein: the core layer, the inner cladding layer and the outer cladding layer are sequentially and integrally concentric from inside to outside to form a cylindrical structure, wherein the diameter of the core layer is 6-10 mu m, the diameter of the inner cladding layer is 10-30 mu m, and the diameter of the outer cladding layer is 125-130 mu m.
3. The method for preparing a Tm/Tb co-doped silica fiber for a 1.7 μm fiber laser according to claim 1, comprising the steps of:
1) by chemical vapor depositionIntegrating Method (MCVD) and Chelate Precursor Doping Technology (CPDT) are combined to convert Tm into3+With chelate Tm (thd)3The components of the core layer formula are doped in the form of (1), and the doped components are uniformly introduced into a quartz tube to be deposited to form a prefabricated rod core layer; then Tb is added3+With chelate Tb (thd)3The components of the inner cladding formula are doped in the form of (1), and are uniformly introduced into a quartz tube to deposit on the surface of a core layer of a prefabricated rod to form an inner cladding of the prefabricated rod; uniformly introducing the formula components of the outer cladding layer into a quartz tube, and depositing on the surface of the inner cladding layer of the prefabricated rod to form the outer cladding layer of the prefabricated rod; wherein the size ratio among the core layer, the inner cladding layer and the outer cladding layer is controlled by adjusting the deposition cycle times; finally, forming an optical fiber preform through high-temperature sintering and rod shrinking processes;
2) and drawing the prepared optical fiber preform into the optical fiber with the required size in a quartz optical fiber drawing tower by using a hot drawing method.
4. The preparation method according to claim 3, wherein in the step 1), the deposition temperature is 1300-1450 ℃, and the pressure difference in the deposition tube is kept between 50-120 Pa; the sintering temperature is 1850-1950 ℃; the rod-shrinking temperature is 2050-2150 ℃, and the pressure difference is reduced to 20-40 Pa.
5. The preparation method according to claim 3, wherein in the step 2), the fiber drawing temperature is 1950-2100 ℃, the rod feeding speed of the preform is 0.2-0.5 mm/min, and the diameter of the drawn Tm/Tb co-doped silica fiber is 125-130 μm.
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| CN111129924B (en) * | 2019-12-23 | 2021-06-22 | 中国科学院西安光学精密机械研究所 | High-power 1.7-micron all-fiber laser |
| CN112851127B (en) * | 2021-01-16 | 2021-11-02 | 威海长和光导科技有限公司 | High-gain Ho3+/Tm3+/Yb3+Co-doped quartz optical fiber and preparation method thereof |
| CN114349355B (en) * | 2022-01-21 | 2022-11-25 | 广东工业大学 | Rare earth doped multi-component oxide glass optical fiber for 1.7 mu m waveband laser generation and application thereof |
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