CN112321146A - Pretreatment method for improving radiation resistance of quartz optical fiber prefabricated part - Google Patents
Pretreatment method for improving radiation resistance of quartz optical fiber prefabricated part Download PDFInfo
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- CN112321146A CN112321146A CN202011005341.XA CN202011005341A CN112321146A CN 112321146 A CN112321146 A CN 112321146A CN 202011005341 A CN202011005341 A CN 202011005341A CN 112321146 A CN112321146 A CN 112321146A
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- 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
- C03B37/01853—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
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Abstract
The invention discloses a pretreatment method of a quartz optical fiber prefabricated part, which is characterized in that the optical fiber prefabricated part is sequentially subjected to deuterium loading, pre-radiation and heat treatment with a temperature rise gradient, so that the problem that the optical fiber laser performance is reduced due to deuterium loading treatment is solved, the structure of a quartz optical fiber material is more stable, the operation is simple and convenient, the structural rigidity of the material is ensured, and the radiation resistance and the laser tilt efficiency are improved.
Description
Technical Field
The invention relates to the field of quartz optical fibers, in particular to a pretreatment method for high radiation resistance of a quartz optical fiber prefabricated part.
Background
Silica is used as a main raw material of the silica optical fiber, and the refractive index distribution of a fiber core and a cladding is controlled according to different doping amounts. The quartz (glass) series optical fiber has the characteristics of low consumption and wide band, and is widely applied to cable televisions and communication systems at present. The quartz glass optical fiber has the advantage of low loss, and when the wavelength of light is 1.0-1.7 μm (about 1.4 μm), the loss is only 1dB/km, and is the lowest at 1.55 μm, and is only 0.2 dB/km.
The quartz fiber laser is an important tool for realizing space laser communication due to the advantages of light weight, small volume, high peak power, good beam quality and the like, however, the quartz fiber is subjected to complex ion radiation environments (such as proton, electron, X-and gamma-ray) when performing space tasks. The quartz optical fiber is easy to generate color centers in a radiation environment, can seriously affect the laser performance of the quartz optical fiber, and can greatly increase the transmission loss of the optical fiber in the radiation environment. In the prior art, the generation of color centers is suppressed by hydrogen-loaded, however, 70% or more of hydrogen molecules diffuse out of the core of the optical fiber within 3 months at room temperature. In order to prevent the out-diffusion of gas, the prior art has prevented it by two physical methods, one is to cover the surface of the optical fiber with a sealing coating, and the other is to develop a new optical fiber structure. Although both methods are effective, the process is complicated and not suitable for common silica optical fibers. Therefore, a pretreatment method for improving the radiation resistance of the optical fiber by pretreating the optical fiber preform material to inhibit the outward diffusion of gas is proposed. Patent CN103319085B discloses a treatment method for improving radiation resistance of a quartz optical fiber, which adopts a method of preheating treatment, rapid quenching, pre-irradiation and reheating treatment, and makes the structure of the quartz optical fiber material more stable by using two heat treatments, but the heat treatment steps of the method are complex, and the method is not suitable for industrial production.
Disclosure of Invention
The invention aims to solve the technical problems that the performance of the optical fiber is reduced when the optical fiber works in a radiation environment, the color center of the optical fiber is prevented from being generated when the optical fiber is used in the radiation environment, the transmission loss of the optical fiber in the transmission process is reduced, the optical fiber prefabricated part is subjected to reasonable and sequential pretreatment including heat treatment with a temperature rise gradient, the structure of a quartz optical fiber material is more stable, the operation is simple and convenient, the structural rigidity of the material is ensured, and the radiation resistance is improved.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: the method comprises the following steps of sequentially carrying out deuterium loading, pre-radiation and heat treatment on a quartz optical fiber preform, wherein the pre-treatment method comprises the following steps:
1) carrying out deuterium loading treatment on the quartz optical fiber prefabricated part, wherein the pressure of deuterium atmosphere is 5-30Mpa, the temperature of deuterium loading is 200-400 ℃, and the time of deuterium loading treatment is 600-800 h;
2) pre-radiating the quartz optical fiber preform by adopting gamma rays, wherein the pre-radiation dose is 80-120kGy, and the radiation time is 10-20 hours.
Annealing the quartz optical fiber prefabricated part, wherein during annealing, the temperature rise process comprises three times of constant temperature rise, and the temperature rise to 200-300 ℃ in the first stageoC, raising the temperature to 500-600 ℃ in the second stageoC, raising the temperature to 800-1000 in the third stageoC, the temperature rising speed is 10 to 15oC/min, cooling rate of 5-10oC/min。
Further, deuterium carrying treatment is carried out on the quartz optical fiber in the step (1), wherein the pressure of a deuterium atmosphere is 15Mpa, the temperature of the deuterium is 320 ℃, and the time of the deuterium carrying treatment is 680 h. Further, the pre-radiation in the step (2) is carried out in a vacuum environment, the vacuum pressure is 80-110Pa, and the vacuum temperature is 400-780 ℃.
Further, the annealing process of the quartz optical fiber in the step (3) is carried out in an annealing furnace, the annealing furnace is vacuumized before annealing, and the vacuum state of the annealing furnace is kept until the annealing is finished.
Further, in the step (2), the pre-radiation is carried out in a vacuum environment, the vacuum pressure is 98Pa, the vacuum temperature is 500 ℃, the pre-radiation treatment adopts 105Gy of pre-radiation dose, the dose rate is 6.2kG/h, and the radiation time is 18 hours.
Further, in the step (3), the quartz optical fiber preform is annealed, the temperature of the quartz optical fiber is raised to 900 ℃, and then the annealing is carried out for 9.5 hours.
Compared with the prior art, the invention has the advantages that: when the optical fiber prefabricated member is pretreated, deuterium carrying and pre-irradiation treatment are firstly carried out, and through the annealing process of gradient temperature rise, on one hand, the color center formed in the pre-irradiation process is bleached, and residual deuterium molecules which are not chemically combined with core glass are released, so that the radiation resistance is enhanced, on the other hand, the structural rigidity of the quartz optical fiber is greatly enhanced, and the laser skew efficiency is improved.
Drawings
FIG. 1 is a graph of loss spectra and laser slope efficiency for optical fibers drawn from preforms of examples 3 and 4 under different temperature ramp mechanisms.
Detailed Description
The present invention is further illustrated by the following specific examples, which should not be construed as limiting the scope of the invention.
Example 1:
a pretreatment method for improving radiation resistance of a quartz optical fiber prefabricated part sequentially carries out deuterium loading, pre-radiation and heat treatment on the quartz optical fiber prefabricated part, and comprises the following steps: 1) And carrying out deuterium loading treatment on the quartz optical fiber preform, wherein the deuterium atmosphere pressure is 5Mpa, the deuterium loading temperature is 400 ℃, the deuterium loading treatment time is 600h, the specific deuterium atmosphere pressure is 15Mpa, the deuterium loading temperature is 320 ℃, and the deuterium loading treatment time is 680 h. 2) The method comprises the steps of pre-radiating a quartz optical fiber prefabricated part by gamma rays, wherein the pre-radiation treatment is carried out by placing the quartz optical fiber prefabricated part in a vacuum environment, the vacuum pressure is 95Pa, the vacuum temperature is 450 ℃ and pre-radiating the quartz optical fiber prefabricated part in the vacuum environment, the pre-radiation dosage is 105Gy, the dose rate is 6.2kG/h, the radiation time is 18 hours. 3) Annealing the quartz optical fiber prefabricated part, firstly heating the quartz optical fiber to 850 ℃, then annealing for 9 hours, putting the quartz optical fiber annealing process into an annealing furnace, vacuumizing the annealing furnace before annealing, keeping the vacuum state of the annealing furnace until the annealing is finished, wherein the quartz optical fiber heating process comprises three times of constant temperature rise, the first stage of temperature rise to 200 ℃, the second stage of temperature rise to 500 ℃, the third stage of temperature rise to 800 ℃, and the temperature rise speed is 15 DEG, the temperature rise is performed in the first stage of temperature rise to 200 DEG, the second stage of temperature riseoC/min, and the cooling speed is 5 ℃/min.
Example 2:
a pretreatment method for improving radiation resistance of a quartz optical fiber prefabricated part sequentially carries out deuterium loading, pre-radiation and heat treatment on the quartz optical fiber prefabricated part, and comprises the following steps: 1) And carrying out deuterium loading treatment on the quartz optical fiber preform, wherein the deuterium atmosphere pressure is 30Mpa, the deuterium loading temperature is 300 ℃, the deuterium loading treatment time is 700h, the specific deuterium atmosphere pressure is 15Mpa, the deuterium loading temperature is 320 ℃, and the deuterium loading treatment time is 680 h. 2) Pre-radiating the quartz optical fiber preform by adopting gamma rays, wherein the pre-radiation treatment adopts the pre-radiation dosage of 105Gy, the dosage rate of 6.2kG/h and the radiation time length of 18 hours, and the pre-radiation is put on a vacuum furnaceThe pre-irradiation is carried out in a vacuum environment at the vacuum pressure of 100Pa and the vacuum temperature of 600 ℃ and is carried out in the vacuum environment. 3) Annealing the quartz optical fiber prefabricated part, firstly heating the quartz optical fiber to 900 ℃, then annealing for 10 hours, putting the quartz optical fiber annealing process into an annealing furnace, vacuumizing the annealing furnace before annealing, keeping the vacuum state of the annealing furnace until the annealing is finished, wherein the quartz optical fiber heating process comprises three times of constant temperature rise, the first stage of temperature rise to 250 ℃, the second stage of temperature rise to 550 ℃, the third stage of temperature rise to 900 ℃, and the temperature rise speed is 12 DEG CoC/min, and the cooling speed is 8 ℃/min.
Example 3:
a pretreatment method for improving radiation resistance of a quartz optical fiber prefabricated part sequentially carries out deuterium loading, pre-radiation and heat treatment on the quartz optical fiber prefabricated part, and comprises the following steps: 1) And carrying out deuterium loading treatment on the quartz optical fiber preform, wherein the deuterium atmosphere pressure is 15Mpa, the deuterium loading temperature is 200 ℃, the deuterium loading treatment time is 800h, the specific deuterium atmosphere pressure is 15Mpa, the deuterium loading temperature is 320 ℃, and the deuterium loading treatment time is 680 h. 2) The method comprises the steps of pre-radiating a quartz optical fiber preform by gamma rays, wherein the pre-radiation treatment is carried out by placing the quartz optical fiber preform in a vacuum environment at the vacuum pressure of 110Pa and the vacuum temperature of 700 ℃ under the condition that the pre-radiation dosage is 105Gy, the dosage rate is 6.2kG/h and the radiation time is 18 hours. 3) Annealing the quartz optical fiber prefabricated part, firstly heating the quartz optical fiber to 1000 ℃, then annealing for 12 hours, putting the quartz optical fiber annealing process into an annealing furnace, vacuumizing the annealing furnace before annealing, keeping the vacuum state of the annealing furnace until the annealing is finished, wherein the quartz optical fiber heating process comprises three times of constant temperature rise, the first stage of temperature rise to 300 ℃, the second stage of temperature rise to 600 ℃, the third stage of temperature rise to 1000 ℃, and the temperature rise speed is 10oC/min, and the cooling speed is 10 ℃/min.
Example 4:
a pretreatment method for improving radiation resistance of a quartz optical fiber prefabricated part sequentially carries out deuterium loading, pre-radiation and heat treatment on the quartz optical fiber prefabricated part, and comprises the following steps: 1) to quartzAnd carrying out deuterium loading treatment on the optical fiber preform, wherein the deuterium atmosphere pressure is 15Mpa, the deuterium loading temperature is 200 ℃, the deuterium loading treatment time is 600-800h, the specific deuterium atmosphere pressure is 15Mpa, the deuterium loading temperature is 320 ℃, and the deuterium loading treatment time is 680 h. 2) The method comprises the steps of pre-radiating a quartz optical fiber preform by gamma rays, wherein the pre-radiation treatment is carried out by placing the quartz optical fiber preform in a vacuum environment at the vacuum pressure of 110Pa and the vacuum temperature of 700 ℃ under the condition that the pre-radiation dosage is 105Gy, the dosage rate is 6.2kG/h and the radiation time is 18 hours. 3) Annealing the quartz optical fiber prefabricated part, firstly heating the quartz optical fiber to 1200 ℃, then preserving heat for 12 hours, putting the quartz optical fiber annealing process into an annealing furnace, vacuumizing the annealing furnace before annealing, keeping the vacuum state of the annealing furnace until the annealing is finished, wherein the quartz optical fiber heating process comprises three times of constant temperature rise, the first stage of temperature rise to 300 ℃, the second stage of temperature rise to 600 ℃, the third stage of temperature rise to 1000 ℃, and the temperature rise speed is 20oC/min, and the cooling speed is 10 ℃/min.
In example 4, the temperature rise speed is too high, so that the bubbles cannot be discharged in time, and the stability of the material is reduced, and as can be seen from the attached graph 1, the laser oblique efficiency is reduced to 59% from 75% compared with that of example 3.
The present invention and its embodiments have been described above, and the description is not intended to be limiting, and the drawings are only one embodiment of the present invention, and the actual structure is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A pretreatment method for improving the radiation resistance of a quartz optical fiber preform is characterized by comprising the following steps: the method comprises the following steps of sequentially carrying out deuterium loading, pre-radiation and gradient heat treatment on a quartz optical fiber preform, wherein the pre-treatment method specifically comprises the following steps:
1) deuterium-carrying treatment of quartz optical fiber preformThe atmosphere pressure is 5-30Mpa, and the deuterium-carrying temperature is 200-400oC, deuterium carrying treatment time is 600-800 h;
2) pre-radiating the quartz optical fiber preform by adopting gamma rays, wherein the pre-radiation dose is 80-120kGy, and the radiation time is 10-20 hours;
3) annealing the quartz optical fiber prefabricated part, wherein during annealing, the temperature rise process comprises three times of constant temperature rise, and the temperature rise to 200-300 ℃ in the first stageoC, raising the temperature to 500-600 ℃ in the second stageoC, raising the temperature to 800-1000 in the third stageoC, the temperature rising speed is 10 to 15oC/min, cooling rate of 5-10oC/min。
2. The pretreatment method for improving radiation resistance of a silica optical fiber preform according to claim 1, wherein: the step (1) of deuterium loading treatment of the quartz optical fiber is carried out, wherein the pressure of deuterium atmosphere is 15Mpa, and the temperature of deuterium loading is 320 DEG CoC, deuterium carrying treatment time is 680 h.
3. The pretreatment method for improving radiation resistance of a silica optical fiber preform according to claim 1, wherein: the step (2) is carried out by placing the pre-radiation in a vacuum environment, the vacuum pressure is 80-110Pa, and the vacuum temperature is 400-780oC。
4. The pretreatment method for improving radiation resistance of a silica optical fiber preform according to claim 1, wherein: and (4) putting the quartz optical fiber in the annealing furnace for annealing in the step (3), vacuumizing the annealing furnace before annealing, and keeping the vacuum state of the annealing furnace until the annealing is finished.
5. A pretreatment method for improving a radiation resistance of a silica optical fiber preform according to claim 3, wherein: the step (2) is carried out by placing the pre-radiation in a vacuum environment, the vacuum pressure is 98Pa, and the vacuum temperature is 500 DEG CoAnd C, adopting a pre-radiation dose of 105Gy, a dose rate of 6.2kG/h and a radiation time length of 18 hours for pre-radiation treatment.
6. The pretreatment method for improving radiation resistance of a silica optical fiber preform according to claim 1 or 4, wherein: annealing the quartz optical fiber prefabricated part in the step (3), and heating the quartz optical fiber to 900 DEG firstlyoC, and then keeping the temperature for 9.5 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521079A (en) * | 2022-09-29 | 2022-12-27 | 长飞光纤光缆股份有限公司 | Post-processing method of radiation-resistant optical fiber |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319085A (en) * | 2013-06-04 | 2013-09-25 | 上海大学 | Processing method for improving anti-radiation performance of quartz optical fibers |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103319085A (en) * | 2013-06-04 | 2013-09-25 | 上海大学 | Processing method for improving anti-radiation performance of quartz optical fibers |
Non-Patent Citations (1)
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|---|
| CHONGYUN SHAO: "Enhanced radiation resistance of ytterbium-doped silica fiber by pretreating on a fiber perform", 《OPTICAL MATERIALS EXPRESS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521079A (en) * | 2022-09-29 | 2022-12-27 | 长飞光纤光缆股份有限公司 | Post-processing method of radiation-resistant optical fiber |
| CN115521079B (en) * | 2022-09-29 | 2024-04-19 | 长飞光纤光缆股份有限公司 | Post-treatment method of radiation-resistant optical fiber |
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