CN114988687A - Preparation method of quartz optical fiber preform - Google Patents
Preparation method of quartz optical fiber preform Download PDFInfo
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- CN114988687A CN114988687A CN202210616880.XA CN202210616880A CN114988687A CN 114988687 A CN114988687 A CN 114988687A CN 202210616880 A CN202210616880 A CN 202210616880A CN 114988687 A CN114988687 A CN 114988687A
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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
- C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
- C03B37/01211—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
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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
- C03B37/01265—Manufacture of preforms for drawing fibres or filaments starting entirely or partially from molten glass, e.g. by dipping a preform in a melt
- C03B37/01268—Manufacture of preforms for drawing fibres or filaments starting entirely or partially from molten glass, e.g. by dipping a preform in a melt by casting
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/045—Silica-containing oxide glass compositions
- C03C13/046—Multicomponent glass compositions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
The invention belongs to the field of optical fiber preforms, and particularly relates to a preparation method of a quartz optical fiber preform. The method comprises the following steps: 1) mixing, curing and molding silicon dioxide powder, alumina powder and resin solution; 2) after pretreatment, firing for degreasing, and then carrying out hole expanding activation to obtain an activated precursor rod; 3) preparing doping treatment liquid for dipping doping treatment, and pre-sintering to obtain a blank; 4) and (5) collapsing to obtain the quartz optical fiber preform. According to the invention, through the matching of components and processes, the actual doping depth and doping uniformity of the gain element are greatly improved, and further the doping effect is improved; the whole process is simple and efficient, and the preparation of the doped silica glass optical fiber preform can be quickly realized.
Description
Technical Field
The invention belongs to the field of optical fiber preforms, and particularly relates to a preparation method of a quartz optical fiber preform.
Background
An optical fiber preform is a preform of material used to draw an optical fiber. And the quartz optical fiber preform is a core raw material for manufacturing the quartz optical fiber.
Doping of silica optical fiber preforms is an effective way to improve their performance. At present, the doped quartz optical fiber plays an irreplaceable role in the fields of optical fiber communication, optical fiber sensing, optical fiber lasers, optical fiber amplifiers and the like.
However, the doping process of the quartz preform has problems of low efficiency, high cost and the like, and the improvement of the doping method of the quartz optical fiber preform is an important research direction.
Disclosure of Invention
The invention provides a preparation method of a quartz optical fiber preform, aiming at solving the problems that the existing doping process of the quartz optical fiber preform is complicated, high in cost and low in efficiency, and most doping processes cannot realize high-depth and high-uniformity doping and the like.
The invention aims to:
firstly, deep and uniform doping can be realized;
and secondly, the process provided by the invention is ensured to have good applicability and can be suitable for doping of most gain elements.
In order to achieve the purpose, the invention adopts the following technical scheme.
A method for preparing a quartz optical fiber prefabricated rod,
the method comprises the following steps:
1) mixing silicon dioxide powder, alumina powder and resin solution, shearing, dispersing and homogenizing to obtain a suspension, controlling the solid content of the suspension to be less than or equal to 80%, then introducing the suspension into a transparent quartz glass mold, and demolding and cleaning after curing and molding to obtain a precursor rod;
2) pretreating the precursor rod, then burning and degreasing, placing in a phosphoric acid solution for dipping treatment, and carrying out reaming activation to obtain an activated precursor rod;
3) preparing a salt solution and/or a salt dispersion solution as a doping treatment solution, placing the activated precursor rod in the doping treatment solution for impregnation doping treatment, and then taking out the activated precursor rod for presintering to obtain a blank;
4) and (3) placing the blank in a quartz glass sleeve mold, placing the quartz glass sleeve mold on rotary heating equipment, carrying out uniform heat treatment at 1600-1800 ℃ until the blank is completely transparent and vitrified, heating to 2200-2400 ℃ and carrying out rotary heat treatment under the condition of low pressure until the sleeve collapses to be completely attached to the surface of the blank, thus obtaining the quartz optical fiber preform.
As a preference, the first and second liquid crystal compositions are,
the dosage of the alumina powder in the step 1) is 0.0015-0.00200 wt% of that of the silicon dioxide powder.
As a matter of preference,
the resin in the step 1) comprises the following components in percentage by mass:
80-88 wt% of hydroxyethyl methacrylate, 5-6 wt% of methyl methacrylate, 6-11 wt% of tetraethyleneglycol diacrylate and the balance of hydroquinone, wherein the dosage of hydroquinone is controlled to be less than or equal to 4.5 wt%.
As a preference, the first and second liquid crystal compositions are,
step 2) the pretreatment comprises surface ultrasonic cleaning by adopting ethanol and/or deionized water;
and 2) burning and degreasing at the temperature of 200-600 ℃, and burning and degreasing in an atmosphere with the oxygen content of more than or equal to 12 wt%.
As a matter of preference,
the concentration of the phosphoric acid solution in the step 2) is 2.5-3.5 wt%, the dipping time is 25-35 min, and the dipping temperature is 20-25 ℃.
As a matter of preference,
and 2) carrying out the dipping treatment under the low-pressure condition of 0.3-0.5 atm.
As a preference, the first and second liquid crystal compositions are,
and 3) the doping treatment liquid contains optical fiber gain elements, and the optical fiber gain elements are rare earth ions and/or alkali metal ions.
As a preference, the first and second liquid crystal compositions are,
step 3) the dipping doping treatment is carried out in a high-pressure-low-pressure circulating atmosphere;
the high-low pressure circulating atmosphere is controlled by a vacuum pump and/or a gas booster pump and/or a piston system so as to maintain high pressure once and low pressure once to form a cycle;
in a single cycle: the high pressure is controlled to be 1.15-1.25 atm and maintained for 15-20 s, and the low pressure is controlled to be 100-300 Pa and maintained for 8-10 s.
As a preference, the first and second liquid crystal compositions are,
and 4) controlling the air pressure to be less than or equal to 0.001Pa by using a high vacuum system under the low-pressure condition.
According to the technical scheme, the preparation of the porous quartz glass matrix can be realized by matching the resin with the silicon dioxide powder, and the aluminum oxide powder is doped in the invention, because the aluminum oxide powder and the silicon dioxide powder have good compatibility, a three-dimensional cobweb-shaped continuous glassy interface with large depth and uniform distribution can be formed in the preparation process of the precursor rod, and in the subsequent preparation process, a continuous and large-depth doped pore structure can be realized in a dissolving and reaming manner, and the doping of the benefit elements can be quickly and effectively realized after the activation, so that a blank is obtained. And then processed into a quartz glass prefabricated rod by a conventional process. Compared with the existing doping process, the technical scheme of the invention can improve the doping uniformity and depth and greatly improve the doping effect.
The invention has the beneficial effects that:
1) by matching the components and the process, the doping depth and the doping uniformity of the gain elements are greatly improved, and the doping effect is improved;
2) the whole process is simple and efficient, and the preparation of the doped silica glass optical fiber perform can be quickly realized.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to specific examples. Those skilled in the art will be able to implement the invention based on these teachings. Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Unless otherwise specified, the raw materials used in the examples of the present invention are all commercially available or available to those skilled in the art; unless otherwise specified, the methods used in the examples of the present invention are all those known to those skilled in the art.
Example 1
A method for preparing a quartz optical fiber preform,
the method comprises the following steps:
1) adding silicon dioxide nano powder and 0.0015 wt% of aluminum oxide nano powder into a resin solution together, mixing to prepare a suspension, wherein the resin consists of 82 wt% of hydroxyethyl methacrylate, 5 wt% of methyl methacrylate, 10 wt% of tetraethyleneglycol diacrylate and 3 wt% of hydroquinone, shearing, dispersing and homogenizing to obtain a suspension, controlling the solid content of the suspension to be less than or equal to 80%, then introducing the suspension into a transparent quartz glass mold for UV curing, and demolding and cleaning after curing and forming to obtain a precursor rod;
2) carrying out ethanol ultrasonic cleaning pretreatment on the precursor rod, then burning and degreasing the precursor rod in an air atmosphere at 320 ℃, then placing the precursor rod in 2.5 wt% phosphoric acid solution, carrying out immersion treatment for 25min at 25 ℃ under the condition of low pressure of 0.35atm, and carrying out hole expansion activation to obtain an activated precursor rod;
3) preparing doping treatment liquid, wherein the doping treatment liquid is an ethanol solution containing 0.5mol/L ytterbium trichloride, 2.0mol/L aluminum trichloride and 0.5mol/L erbium trichloride, placing an activation precursor rod into the doping treatment liquid for dipping and doping treatment, and then taking out the activation precursor rod for presintering at 300 ℃ to obtain a blank;
the dipping and doping treatment is carried out in a high-pressure-low-pressure circulating atmosphere;
the high-low pressure circulating atmosphere is controlled by a vacuum pump so as to maintain a primary high pressure and a primary low pressure to form a cycle;
in a single cycle: controlling the high pressure to be 1.15atm and maintaining the pressure for 20s, and controlling the low pressure to be 300Pa and maintaining the pressure for 10 s;
4) and (3) placing the blank in a quartz glass sleeve mold, placing the quartz glass sleeve mold on rotary heating equipment, performing uniform heat treatment at 1600 ℃ until the blank is completely vitrified, heating to 2200 ℃, performing rotary heat treatment after controlling the air pressure to be less than or equal to 0.001Pa by utilizing a high vacuum system until the sleeve is collapsed until the sleeve is completely attached to the surface of the blank, and thus obtaining the quartz optical fiber preform.
The quartz optical fiber preform prepared by the invention is detected, the preform is drawn into an optical fiber, the size of the optical fiber is 6 mu m/125 mu m (fiber core/cladding), the loss is 0.6dB/m, and the laser slope efficiency is 40%.
Example 2
A method for preparing a quartz optical fiber prefabricated rod,
the method comprises the following steps:
1) adding silicon dioxide nano powder and 0.00200 wt% of aluminum oxide nano powder into a resin solution together, mixing to prepare a suspension, wherein the resin is composed of 86 wt% of hydroxyethyl methacrylate, 6 wt% of methyl methacrylate, 6 wt% of tetraethyleneglycol diacrylate and 2 wt% of hydroquinone, shearing, dispersing and homogenizing to obtain a suspension, controlling the solid content of the suspension to be less than or equal to 80%, then introducing the suspension into a transparent quartz glass mold for UV curing, and demolding and cleaning after curing and forming to obtain a precursor rod;
2) carrying out ethanol ultrasonic cleaning pretreatment on the precursor rod, then burning and degreasing the precursor rod in an air atmosphere at 550 ℃, then placing the precursor rod in 3.5 wt% phosphoric acid solution, carrying out immersion treatment for 35min under the low pressure condition of 0.5atm and the temperature condition of 20 ℃, and carrying out hole expansion activation to obtain an activated precursor rod;
3) preparing doping treatment liquid, wherein the doping treatment liquid is an ethanol solution containing 0.5mol/L ytterbium trichloride, 2.0mol/L aluminum trichloride and 0.5mol/L erbium trichloride, placing an activation precursor rod in the doping treatment liquid for dipping and doping treatment, and then taking out the activation precursor rod for pre-sintering at 300 ℃ to obtain a blank;
the dipping and doping treatment is carried out in a high-pressure-low-pressure circulating atmosphere;
the high-low pressure circulating atmosphere is controlled by a vacuum pump so as to maintain a primary high pressure and a primary low pressure to form a cycle;
in a single cycle: controlling the high pressure to be 1.25atm and maintaining the pressure for 15s, and controlling the low pressure to be 100Pa and maintaining the pressure for 8 s;
4) and (3) placing the blank in a quartz glass sleeve mold, placing the quartz glass sleeve mold on rotary heating equipment, performing uniform heat treatment at 1750 ℃ until the blank is completely transparent and vitrified, heating to 2400 ℃, performing rotary heat treatment after controlling the air pressure to be less than or equal to 0.001Pa by using a high vacuum system until the sleeve is collapsed until the sleeve is completely attached to the surface of the blank, and thus obtaining the quartz optical fiber preform.
The quartz optical fiber preform prepared by the invention is detected, the preform is drawn into an optical fiber, the size of the optical fiber is 6 mu m/125 mu m (fiber core/cladding), the loss is 0.5dB/m, and the laser slope efficiency is 42%.
Example 3
A method for preparing a quartz optical fiber prefabricated rod,
the method comprises the following steps:
1) adding silicon dioxide nano powder and 0.00175 wt% of aluminum oxide nano powder into a resin solution together, mixing to prepare a suspension, wherein the resin is composed of 81 wt% of hydroxyethyl methacrylate, 6 wt% of methyl methacrylate, 9 wt% of tetraethyleneglycol diacrylate and 4 wt% of hydroquinone, shearing, dispersing and homogenizing to obtain a suspension, controlling the solid content of the suspension to be less than or equal to 80%, then introducing the suspension into a transparent quartz glass mold for UV curing, and demolding and cleaning after curing and forming to obtain a precursor rod;
2) carrying out ethanol ultrasonic cleaning pretreatment on the precursor rod, then burning and degreasing the precursor rod in an air atmosphere at 550 ℃, then placing the precursor rod in 3.5 wt% phosphoric acid solution, carrying out immersion treatment for 35min under the low pressure condition of 0.5atm and the temperature condition of 20 ℃, and carrying out hole expansion activation to obtain an activated precursor rod;
3) preparing doping treatment liquid, wherein the doping treatment liquid is an ethanol solution containing 0.5mol/L ytterbium trichloride, 2.0mol/L aluminum trichloride and 0.5mol/L erbium trichloride, placing an activation precursor rod into the doping treatment liquid for dipping and doping treatment, and then taking out the activation precursor rod for presintering at 300 ℃ to obtain a blank;
the dipping doping treatment is carried out in a high-pressure-low-pressure circulating atmosphere;
the high-low pressure circulating atmosphere is controlled by a vacuum pump so as to maintain a primary high pressure and a primary low pressure to form a cycle;
in a single cycle: controlling the high pressure to be 1.25atm and maintaining for 15s, controlling the low pressure to be 100Pa and maintaining for 8 s;
4) and (3) placing the blank in a quartz glass sleeve mold, placing the quartz glass sleeve mold on rotary heating equipment, performing uniform heat treatment at 1750 ℃ until the blank is completely transparent and vitrified, heating to 2400 ℃, performing rotary heat treatment after controlling the air pressure to be less than or equal to 0.001Pa by using a high vacuum system until the sleeve is collapsed until the sleeve is completely attached to the surface of the blank, and thus obtaining the quartz optical fiber preform.
The quartz optical fiber preform prepared by the invention is detected, the preform is drawn into an optical fiber, the size of the optical fiber is 6 mu m/125 mu m (fiber core/cladding), the loss is 0.6dB/m, and the laser slope efficiency is 41%.
Comparative example 1
A method for preparing a quartz optical fiber prefabricated rod,
the method comprises the following steps:
1) adding silicon dioxide nano powder into a resin solution, mixing to prepare a suspension, wherein the resin consists of 82 wt% of hydroxyethyl methacrylate, 5 wt% of methyl methacrylate, 10 wt% of tetraethyleneglycol diacrylate and 3 wt% of hydroquinone, shearing, dispersing and homogenizing to obtain a suspension, controlling the solid content of the suspension to be less than or equal to 80%, then introducing the suspension into a transparent quartz glass mold for UV curing, and demolding and cleaning after curing and forming to obtain a precursor rod;
2) carrying out ethanol ultrasonic cleaning pretreatment on the precursor rod, then burning and degreasing the precursor rod in an air atmosphere at 320 ℃, then placing the precursor rod in 2.5 wt% phosphoric acid solution, carrying out immersion treatment for 25min at 25 ℃ under the condition of low pressure of 0.35atm, and activating to obtain an activated precursor rod;
3) preparing doping treatment liquid, wherein the doping treatment liquid is an ethanol solution containing 0.5mol/L ytterbium trichloride, 2.0mol/L aluminum trichloride and 0.5mol/L erbium trichloride, placing an activation precursor rod into the doping treatment liquid for dipping and doping treatment, and then taking out the activation precursor rod for presintering at 300 ℃ to obtain a blank;
the dipping and doping treatment is carried out in a high-pressure-low-pressure circulating atmosphere;
the high-low pressure circulating atmosphere is controlled by a vacuum pump so as to maintain a primary high pressure and a primary low pressure to form a cycle;
in a single cycle: controlling the high pressure to be 1.15atm and maintaining for 20s, and controlling the low pressure to be 300Pa and maintaining for 10 s;
4) and (3) placing the blank in a quartz glass sleeve mold, placing the quartz glass sleeve mold on rotary heating equipment, performing uniform heat treatment at 1600 ℃ until the blank is completely vitrified, heating to 2200 ℃, performing rotary heat treatment after controlling the air pressure to be less than or equal to 0.001Pa by utilizing a high vacuum system until the sleeve is collapsed until the sleeve is completely attached to the surface of the blank, and thus obtaining the quartz optical fiber preform.
The quartz optical fiber preform prepared by the invention is detected, the preform is drawn into an optical fiber, and the size of the optical fiber is as follows: 6 μm/125 μm (core/cladding), 1.0dB/m loss, and a laser slope efficiency of 36%.
Comparative example 2
A method for preparing a quartz optical fiber prefabricated rod,
the method comprises the following steps:
1) adding silicon dioxide nano powder into a resin solution, mixing to prepare a suspension, wherein the resin consists of 82 wt% of hydroxyethyl methacrylate, 5 wt% of methyl methacrylate, 10 wt% of tetraethyleneglycol diacrylate and 3 wt% of hydroquinone, shearing, dispersing and homogenizing to obtain a suspension, controlling the solid content of the suspension to be less than or equal to 80%, then introducing the suspension into a transparent quartz glass mold for UV curing, and demolding and cleaning after curing and forming to obtain a precursor rod;
2) carrying out ethanol ultrasonic cleaning pretreatment on the precursor rod, and then burning and degreasing the precursor rod in an air atmosphere at 320 ℃ to obtain an activated precursor rod;
3) preparing doping treatment liquid, wherein the doping treatment liquid is an ethanol solution containing 0.5mol/L ytterbium trichloride, 2.0mol/L aluminum trichloride and 0.5mol/L erbium trichloride, placing an activation precursor rod in the doping treatment liquid for dipping and doping treatment, and then taking out the activation precursor rod for pre-sintering at 300 ℃ to obtain a blank;
the dipping and doping treatment is carried out in a high-pressure-low-pressure circulating atmosphere;
the high-low pressure circulating atmosphere is controlled by a vacuum pump so as to maintain a primary high pressure and a primary low pressure to form a cycle;
in a single cycle: controlling the high pressure to be 1.15atm and maintaining for 20s, and controlling the low pressure to be 300Pa and maintaining for 10 s;
4) and (3) placing the blank in a quartz glass sleeve mold, placing the quartz glass sleeve mold on rotary heating equipment, performing uniform heat treatment at 1600 ℃ until the blank is completely vitrified, heating to 2200 ℃, performing rotary heat treatment after controlling the air pressure to be less than or equal to 0.001Pa by utilizing a high vacuum system until the sleeve is collapsed until the sleeve is completely attached to the surface of the blank, and thus obtaining the quartz optical fiber preform.
The quartz optical fiber preform prepared by the invention is detected, the preform is drawn into an optical fiber, and the size of the optical fiber is as follows: 6 μm/125 μm (core/cladding), loss 0.9dB/m, laser slope efficiency 38%.
It can be seen from the above examples 1 to 3 and comparative examples 1 to 2 that the technical solution of the present invention is mainly to improve the effectiveness of doping of the gain element, and the effective doping of the gain element can be significantly reflected in the aspect of the loss of the optical fiber. However, under the condition of no alumina nano powder, a cobweb-shaped continuous glass structure cannot be formed, and the doping rate is reduced. Comparing comparative example 1 and comparative example 2, it can be seen that the phosphoric acid treatment is not a treatment directly beneficial to improving the doping effect of the silica optical fiber preform, but needs to be matched with the common mixing of the alumina nano powder.
Therefore, for the technical scheme of the invention, the common blending of the alumina nano powder and the silica nano powder is a key influencing factor influencing the technical effect of the invention. After the usage amount of the alumina nano powder reaches 0.00250 wt% of that of the silica nano powder, a small amount of fine cracks appear on the surface of the obtained precursor rod, which results in the reduction of the quality of the quartz optical fiber preform rod product, and when the usage amount of the alumina nano powder is further increased, the preparation of the preform rod can not be effectively realized easily.
Claims (9)
1. A method for preparing a quartz optical fiber preform is characterized in that,
the method comprises the following steps:
1) mixing silicon dioxide powder, alumina powder and resin solution, shearing, dispersing and homogenizing to obtain suspension, controlling the solid content of the suspension to be less than or equal to 80%, then introducing the suspension into a transparent quartz glass mold, and demolding and cleaning after curing and forming to obtain a precursor rod;
2) pretreating the precursor rod, then burning and degreasing, placing in a phosphoric acid solution for dipping treatment, and carrying out reaming activation to obtain an activated precursor rod;
3) preparing a salt solution and/or a salt dispersion liquid as a doping treatment liquid, placing an activated precursor rod in the doping treatment liquid for dipping and doping treatment, and then taking out the activated precursor rod for pre-sintering to obtain a blank;
4) and (3) placing the blank in a quartz glass sleeve mold, placing the quartz glass sleeve mold on rotary heating equipment, carrying out uniform heat treatment at 1600-1800 ℃ until the blank is completely transparent and vitrified, heating to 2200-2400 ℃ and carrying out rotary heat treatment under the condition of low pressure until the sleeve collapses to be completely attached to the surface of the blank, thus obtaining the quartz optical fiber preform.
2. A method for fabricating a silica optical fiber preform according to claim 1,
the dosage of the alumina powder in the step 1) is 0.0015-0.00200 wt% of that of the silicon dioxide powder.
3. A method of fabricating a silica optical fiber preform according to claim 1 or 2,
the resin in the step 1) comprises the following components in percentage by mass:
80-88 wt% of hydroxyethyl methacrylate, 5-6 wt% of methyl methacrylate, 6-11 wt% of tetraethyleneglycol diacrylate and the balance of hydroquinone, wherein the dosage of hydroquinone is controlled to be less than or equal to 4.5 wt%.
4. A method for fabricating an optical fiber preform according to claim 1,
step 2) the pretreatment comprises surface ultrasonic cleaning by adopting ethanol and/or deionized water;
and 2) burning and degreasing at the temperature of 200-600 ℃, and burning and degreasing in an atmosphere with the oxygen content of more than or equal to 12 wt%.
5. A method for preparing an optical fiber preform according to claim 1 or 4,
the concentration of the phosphoric acid solution in the step 2) is 2.5-3.5 wt%, the dipping time is 25-35 min, and the dipping temperature is 20-25 ℃.
6. A method for fabricating an optical fiber preform according to claim 5,
and 2) carrying out the dipping treatment under the low-pressure condition of 0.3-0.5 atm.
7. A method for fabricating an optical fiber preform according to claim 1,
and 3) the doping treatment liquid contains optical fiber gain elements, and the optical fiber gain elements are rare earth ions and/or alkali metal ions.
8. A method of fabricating an optical fiber preform according to claim 1 or 7,
step 3) the dipping doping treatment is carried out in a high-pressure-low-pressure circulating atmosphere;
the high-low pressure circulating atmosphere is controlled by a vacuum pump and/or a gas booster pump and/or a piston system so as to maintain high pressure once and low pressure once to form a cycle;
in a single cycle: the high pressure is controlled to be 1.15-1.25 atm and maintained for 15-20 s, and the low pressure is controlled to be 100-300 Pa and maintained for 8-10 s.
9. A method for fabricating an optical fiber preform according to claim 1,
and 4) controlling the air pressure to be less than or equal to 0.001Pa by using a high vacuum system under the low-pressure condition.
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| CN104016580A (en) * | 2014-04-28 | 2014-09-03 | 中国科学院上海光学精密机械研究所 | Preparation method of rare earth doped quartz glass rod |
| US20190375672A1 (en) * | 2018-06-08 | 2019-12-12 | Council Of Scientific & Industrial Research | Process of fabrication of erbium and ytterbium-co-doped multi-elements silica glass based cladding-pumped fiber |
| CN112939445A (en) * | 2021-03-30 | 2021-06-11 | 北京工业大学 | Doped quartz optical fiber preform and preparation method thereof |
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| CN116282882A (en) * | 2023-03-05 | 2023-06-23 | 北京工业大学 | Nd 3+ Doped quartz optical fiber preform and preparation method thereof |
| CN116282882B (en) * | 2023-03-05 | 2024-04-19 | 北京工业大学 | Nd3+Doped quartz optical fiber preform and preparation method thereof |
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