Method for preparing all-solid-state photonic crystal fiber preforms by extrusion
11530156 · 2022-12-20
Assignee
Inventors
- Xunsi Wang (Ningbo, CN)
- Youren Dong (Ningbo, CN)
- Shixun Dai (Ningbo, CN)
- Qiuhua Nie (Ningbo, CN)
- Xiange Wang (Ningbo, CN)
- Minghui Zhong (Ningbo, CN)
- Rongping Wang (Ningbo, CN)
- Xiang Shen (Ningbo, CN)
- Zijun Liu (Ningbo, CN)
- Yongxing Liu (Ningbo, CN)
Cpc classification
C03B2201/86
CHEMISTRY; METALLURGY
C03C3/23
CHEMISTRY; METALLURGY
C03C3/321
CHEMISTRY; METALLURGY
C03B2203/42
CHEMISTRY; METALLURGY
International classification
C03B37/012
CHEMISTRY; METALLURGY
C03C3/23
CHEMISTRY; METALLURGY
C03C3/32
CHEMISTRY; METALLURGY
Abstract
A method for preparing all-solid-state photonic crystal fiber preform by extrusion by aligning the center of the first jacking end of the first jacking rod with the center of the core outlet mold. The adverse effect on this part of extruded core glass by oxygen or other impurities in air during the extrusion out of the core outlets can be avoided. The defects on the core glass surface and the cladding glass surface can be effectively removed, and the purity and quality of the core component in the obtained fiber preform can be improved.
Claims
1. A method for preparing all-solid-state photonic crystal fiber preform by extrusion, comprising: Step-1: preparing an extrusion container, an extrusion chamber, a core outlet mold, a first jacking rod having a first jacking end, a second jacking rod having a second jacking end, an extrusion head and a fiber preform outlet mold, wherein the extrusion container has an opening and a preform outlet respectively on the top and the bottom of the extrusion container; the extrusion chamber has a top opening and a bottom opening respectively on the top and the bottom of the extrusion chamber; the core outlet mold has a plurality of core outlets; the bottom opening of the extrusion chamber communicates with the plurality of core outlets on the core outlet mold; the size of the top opening of the extrusion chamber is smaller than the diameter of the first jacking end of the first jacking rod, and the size of the top opening is greater than the diameter of the second jacking end of the second jacking rod; Step-2: preparing a core glass ingot and a cladding glass ingot which are rinsed with alcohol and dried, wherein the core glass ingot has an outer diameter matched with an inner diameter of the extrusion chamber; and the cladding glass ingot has an outer diameter matched with an inner diameter of the extrusion container; Step-3: placing the cladding glass ingot inside the bottom of the extrusion container, placing the core glass ingot and the extrusion head inside the extrusion chamber, and mounting the core outlet mold at the bottom of the extrusion chamber, the core outlet mold is located above the cladding glass ingot and the extrusion head is located on the core glass ingot; Step-4: putting the extrusion chamber with the core glass ingot into the extrusion container, and resting the first jacking end of the first jacking rod against the top surface of the extrusion chamber, aligning the center of the first jacking end of the first jacking rod with the center of the core outlet mold; Step-5: heating the extrusion container with the extrusion chamber of Step-4 until the temperature in the extrusion container reaches a preset temperature T, so as to make the core glass ingot and the cladding glass ingot in the extrusion container soft to obtain softened core glass and cladding glass; wherein the preset temperature T is higher than Tg and lower than Tx; Tg is defined as the highest one of the core glass transition temperature and the cladding glass transition temperature, and Tx is defined as the lowest one of the core glass crystallization temperature and the cladding glass crystallization temperature; Step-6: pressing the first jacking rod against the top of the extrusion chamber, and pushing the extrusion chamber into the cladding glass inside the extrusion container, so as to make the bottom of the core outlets of the core outlet mold flush with the bottom of the softened cladding glass or make each bottom of the plurality of core outlets of the core outlet mold lower than the bottom of the softened cladding glass; Step-7: maintaining the temperature inside the extrusion container at the preset temperature T, taking the first jacking rod out of the extrusion container, and putting the second jacking rod into the extrusion container, in such a way that the second jacking end of the second jacking rod runs through the top opening of the extrusion chamber and resists against the extrusion head; Step-8: making the second jacking rod push the extrusion head to press the softened core glass inside the extrusion chamber, so that the softened core glass is extruded out from the plurality of core outlets on the core outlet mold located on the bottom of the extrusion container, obtaining a core array having N cores, where N is the number of cores extruded from the extrusion container when the second jacking rod pushes on the extrusion head; Step-9: uniformly pressing the softened core glass in the extrusion chamber and the softened cladding glass in the extrusion container, so that the softened core glass and softened cladding glass are co-extruded out from the preform outlet on the extrusion container, obtaining an initial product of the fiber preform; and Step-10: annealing the obtained initial product of the fiber preform at the transition temperature Tg for a preset period of time, and cooling the initial product of the fiber preform to room temperature, then a fiber preform is obtained, wherein a top plate is disposed in the extrusion chamber covering the core glass ingot; and the extrusion head has a plurality of extrusion stems corresponding to each core outlet on the core outlet mold and capable of inserting into the corresponding core outlet after passing through the top plate.
2. The method of claim 1, wherein the plurality of core outlets on the core outlet mold are separated from each other at a fixed distance.
3. The method of claim 1, wherein the extrusion container, the extrusion chamber, the core outlet mold, the first jacking rod, the second jacking rod, the extrusion head, the core glass ingot and the cladding glass ingot are all ultrasonically cleaned and wiped with alcohol before Step-3.
4. The method of claim 1, wherein the pressing process of the first jacking rod onto the extrusion chamber in Step-6 and the push to press process of the second jacking rod onto the extrusion chamber in Step-8 are done in a vacuum chamber.
5. The method of claim 4, wherein the following step is respectively done before the pressing process of the first jacking rod onto the extrusion chamber in Step-6 and the push to press process of the second jacking rod onto the extrusion chamber to press the core glass in Step-8: the vacuum chamber is vacuumized by a vacuum pump, then inert gas is supplemented into the vacuum chamber once the degree of vacuum in the vacuum chamber is lower than 10.sup.−2 Pa to increase the pressure in the vacuum chamber to atmospheric pressure.
6. The method of claim 1, wherein in Step-9, both the softened core glass in the extrusion chamber and the softened cladding glass in the extrusion container are extruded at a constant speed.
7. The method of claim 1, wherein the preset period of time in Step-10 is between 4 h and 6 h.
8. The method of claim 1, wherein both the core glass ingot and the cladding glass ingot are infrared soft glass ingot, and the difference ΔTg between the transition temperatures for the core glass ingot and the cladding glass ingot is less than or equal to 15° C.
9. The method of claim 1, wherein the opening of the extrusion container, the top opening of the extrusion chamber, the center of the core outlet mold, and the preform outlet on the extrusion container are aligned on a straight line.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DETAILED DESCRIPTION OF THE INVENTION
(13) To enable a further understanding of the present invention content of the invention herein, refer to the detailed description of the invention and the accompanying drawings below:
Embodiment 1
(14) In the Embodiment 1, it is set that the all-solid-state photonic crystal fiber preform to be prepared are chalcogenide photonic crystal fiber preform, and both the core glass ingot 5 and the cladding glass ingot 7 to be used are chalcogenide glass ingot. Specifically, the core glass ingot 5 are As.sub.2Se.sub.3 and the cladding glass ingot 7 are As.sub.2S.sub.3. As shown in
(15) Step-1: preparing an extrusion equipment, which includes an extrusion container 1, an extrusion chamber 2, an extrusion head 4, a core outlet mold 6, a fiber preform outlet mold 8, a first jacking rod 3 and a second jacking rod 12.
(16) Wherein the extrusion container 1 has an opening and a preform outlet 10 respectively on the top and the bottom of the extrusion container 1; the extrusion chamber 2 has a top opening 9 and a bottom opening respectively on the top and the bottom of the extrusion chamber 2, and the bottom opening of the extrusion chamber 2 communicates with core outlets 60 on the core outlet mold 6. The size of the top opening 9 of the extrusion chamber 2 is smaller than the diameter of the first jacking end of the first jacking rod 3, to ensure that the first jacking end of the first jacking rod can run into the extrusion chamber 2 from the top opening. The size of the top opening 9 is greater than the diameter of the second jacking end of the second jacking rod 12. Herein, the core outlet mold 6 has N core outlets 60, N≥2. In this embodiment, the top opening of the extrusion chamber 2 is preferably circular, and similarly, the core outlets 60 on the core outlet mold 6 are also preferably circular. The N core outlets 60 in this embodiment are distributed regularly, that is, they form a regular array of core outlets. The core outlet mold 6 is shown in
(17) The extrusion container, the extrusion chamber, the outlet molds, the first jacking rod, the second jacking rod and the extrusion head, which are prepared in the Step-1, are all ultrasonically cleaned and wiped with alcohol before use. Due to the design that the size of the top opening is greater than the diameter of the first jacking end of the first jacking rod, it can be ensured that the first jacking end of the first jacking rod is always located on the outer side of the top of the extrusion chamber when the top of the extrusion chamber is extruded by the first jacking end of the first jacking rod, in order to ensure that the whole extrusion chamber is extruded downward by the first jacking end of the first jacking rod. Correspondingly, due to the design that the size of the top opening of the extrusion chamber is greater than the diameter of the second jacking end of the second jacking rod, it can be ensured that the second jacking end of the second jacking rod can run into the extrusion chamber from the top opening of the extrusion chamber during the subsequent extrusion process, to facilitate the extrusion of the corresponding As.sub.2Se.sub.3 chalcogenide core glass ingot by the extrusion head. Of course, when the extrusion container, the extrusion chamber, the first jacking rod, the second jacking rod and the extrusion head are ultrasonically cleaned and wiped with alcohol, they may be further cleaned with distilled water or deionized water.
(18) Step-2: As.sub.2Se.sub.3 chalcogenide core glass ingot and As.sub.2S.sub.3 chalcogenide cladding glass ingot which are rinsed with alcohol and dried, wherein the As.sub.2Se.sub.3 chalcogenide core glass ingot has an outer diameter matched with the inner diameter of the extrusion chamber; and the As.sub.2S.sub.3 chalcogenide cladding glass ingot has an outer diameter matched with the inner diameter of the extrusion container.
(19) Additionally, in the Step-2, the As.sub.2Se.sub.3 chalcogenide core glass ingot and the As.sub.2S.sub.3 chalcogenide cladding glass ingot are all ultrasonically cleaned and wiped with alcohol before used, to remove impurities on the surfaces of the two kinds of chalcogenide glass ingot, in order to avoid adverse effect on the subsequent preparation of fiber preform by extrusion by those impurities. Of course, when the two kinds of glass ingot are ultrasonically cleaned and wiped with alcohol, they may be further cleaned with distilled water or deionized water.
(20) Here, the expression “the As.sub.2Se.sub.3 chalcogenide core glass ingot and As.sub.2S.sub.3 chalcogenide cladding glass ingot have an outer diameter matched with the inner diameter of the extrusion chamber” means that the As.sub.2Se.sub.3 chalcogenide core glass ingot, as the raw material, can be exactly placed in the extrusion chamber, and the As.sub.2S.sub.3 chalcogenide cladding glass ingot can be closely fitted on the inner sidewall of the extrusion chamber.
(21) Step-3: Placing the As.sub.2S.sub.3 chalcogenide cladding glass ingot inside the bottom of the extrusion container 1, placing the As.sub.2Se.sub.3 chalcogenide core glass ingot and the extrusion head 4 inside the extrusion chamber 2, and mounting the core outlet mold 6 at the bottom of the extrusion chamber 2, the core outlet mold 6 is located above the As.sub.2S.sub.3 chalcogenide cladding glass ingot and the extrusion head 4 is located on the core glass ingot are assembled in such a way that the core outlet mold 6 is located above the As.sub.2S.sub.3 chalcogenide cladding glass ingot. The extrusion head 4 is located above the As.sub.2Se.sub.3 chalcogenide core glass ingot. The extrusion chamber 2 can protect the As.sub.2Se.sub.3 chalcogenide core glass ingot, to ensure that the As.sub.2Se.sub.3 chalcogenide core glass ingot can be wholly extruded into the As.sub.2S.sub.3 chalcogenide cladding glass ingot.
(22) Step-4: Putting the extrusion chamber 2 with the As.sub.2Se.sub.3 chalcogenide core glass ingot into the extrusion container 1, and resting the first jacking end of the first jacking rod 3 against the top surface of the extrusion chamber, aligning the center of the first jacking end of the first jacking rod 3 with the center of the core outlet mold 6.
(23) Step-5: Heating the extrusion container 1 with the extrusion chamber of the step 4 until the temperature in the extrusion container 1 reaches a preset temperature T, so as to make the As.sub.2Se.sub.3 chalcogenide core glass ingot and the As.sub.2S.sub.3 chalcogenide cladding glass ingot in the extrusion container 1 soft to obtain softened As.sub.2Se.sub.3 chalcogenide core glass and As.sub.2S.sub.3 chalcogenide cladding glass.
(24) Wherein the preset temperature T is higher than Tg and lower than Tx; Tg is defined as the highest one of the As.sub.2Se.sub.3 chalcogenide core glass transition temperature and the As.sub.2S.sub.3 chalcogenide cladding glass transition temperature, and the Tx is defined as the lowest one of the As.sub.2Se.sub.3 chalcogenide core glass crystallization temperature and the As.sub.2S.sub.3 chalcogenide cladding glass crystallization temperature. For example, according to the As.sub.2Se.sub.3 chalcogenide core glass ingot and the As.sub.2S.sub.3 chalcogenide cladding glass ingot to be used, the preset temperature T in this embodiment is higher than 185° C. and lower than 370° C. For example, the preset temperature T is 200° C. The state before the extrusion of the extrusion chamber 2 by the first jacking rod 3 starts is shown in
(25) Step-6: Pressing the first jacking rod 3 against the top of the extrusion chamber 2, and pushing the extrusion chamber 2 into the As.sub.2S.sub.3 chalcogenide cladding glass inside the extrusion container 1, so as to make the bottom of the core outlets 60 of the core outlet mold 6 flush with the bottom of the As.sub.2S.sub.3 chalcogenide cladding glass or make the bottom of the core outlets 60 on the core outlet mold 6 is lower than the bottom of the As.sub.2S.sub.3 chalcogenide cladding glass. The application of the pressing process of the first jacking rod 3 onto the extrusion chamber 2 is in a vacuum chamber. That is, the extrusion chamber 2, the extrusion container 1 and the first jacking rod 3 are all put in the vacuum chamber for extrusion.
(26) Specifically, the vacuum chamber is vacuumized by a vacuum pump, inert gas is supplemented into the vacuum chamber when the degree of vacuum in the vacuum chamber is lower than 10.sup.−2 Pa, so as to make the pressure in the vacuum chamber same as the atmospheric pressure, for example, the supplemented inert gas is nitrogen.
(27) During the extrusion of the top of the extrusion chamber 2 by the first jacking rod 3, the opening of the extrusion container 1, the top opening 9 of the extrusion chamber 2, the center of the core outlet mold 6, and the preform outlet 10 on the extrusion container 1 are all located on a same line. This ensures that the fiber preform products prepared by extrusion will not bend. The state when the extrusion of the extrusion chamber 2 by the first jacking rod 3 ends is shown in
(28) Step-7: Maintaining the temperature inside the extrusion container 1 at the preset temperature T, taking the first jacking rod 3 out of the extrusion container 1 and putting the second jacking rod 12 into the extrusion container 1, in such a way that the second jacking end of the second jacking rod 12 runs through the top opening 9 of the extrusion chamber 2 and resists against the extrusion head 4. The state when the extrusion chamber 2 is extruded by the second jacking rod 12 is shown in
(29) Step-8: Making the second jacking rod 12 push the extrusion head 4 to press the As.sub.2Se.sub.3 chalcogenide core glass inside the extrusion chamber 2, so that the As.sub.2Se.sub.3 chalcogenide core glass is extruded out from the core outlets 60 on the core outlet mold 6 located on the bottom of the extrusion container, obtaining a core array having N As.sub.2Se.sub.3 chalcogenide cores. The state when the extrusion of the extrusion chamber 2 by the second jacking rod 12 ends is shown in
(30) Step-9: Uniformly pressing the core glass in the extrusion chamber 2 and the cladding glass in the extrusion container 1, so that the As.sub.2Se.sub.3 chalcogenide core glass and the As.sub.2S.sub.3 chalcogenide cladding glass are co-extruded out from the preform outlet 10 on the extrusion container 1 obtaining an initial product of the fiber preform.
(31) In the Step-9, both the As.sub.2Se.sub.3 chalcogenide core glass in the extrusion chamber 2 and the As.sub.2S.sub.3 chalcogenide cladding glass in the extrusion container 1 are extruded at a constant speed. Thus, the uniformity of purity of the obtained initial products of the fiber preform and the finally obtained fiber preform products can be improved, and the fracture of the obtained initial products of the fiber preform and the finally obtained fiber preform products due to inconstant speed can be avoided. Therefore, the quality of the prepared fiber preform products is improved.
(32) The application of a stress onto the top of the extrusion chamber 2 by the second jacking rod 12 is also done in a vacuum chamber. That is, the extrusion chamber 2, the extrusion container 1 and the second jacking rod 12 are all put in the vacuum chamber for extrusion. Specifically, the vacuum chamber is vacuumized by a vacuum pump, inert gas is supplemented into the vacuum chamber when the degree of vacuum in the vacuum chamber is lower than 10.sup.−2 Pa, so as to make the pressure in the vacuum chamber same as the atmospheric pressure, for example, the supplemented inert gas is nitrogen.
(33) Step-10: Annealing the obtained initial product of the fiber preform at the transition temperature Tg for a preset period of time (here, 4 h), and cooling the initial product of the fiber preform to room temperature, then a fiber preform is obtained.
(34) The cross-section of the fiber preform products prepared in Embodiment 1 is shown in
(35) It can be found from the product structure shown in
(36) Of course, a top plate 16 is disposed in the extrusion chamber 2 covering the core glass ingot 5; and the extrusion head 4 has a plurality of extrusion stems 40 corresponding to each core outlet 60 on the core outlet mold 6 and capable of inserting into the corresponding core outlet 60 after passing through the top plate 16. As shown in
(37) To prepare fiber preform of different requirements, as an improvement to this embodiment, the core glass outlet mold connected to the bottom of the extrusion chamber may be designed to be adjustable according to the actual requirements. That is, by changing the cross-sectional shape of the preform outlet on the fiber preform outlet mold 8, all-solid-state infrared-soft-glass-based photonic crystal fiber preform products having different cross-sectional shapes can be obtained correspondingly.
Embodiment 2
(38) In the Embodiment 2, it is set that the all-solid-state photonic crystal fiber preform to be prepared are heavy metal oxide glass based photonic crystal fiber preform, and both the core glass ingot 5 and the cladding glass ingot 7 to be used are heavy metal oxide glass ingot. Specifically, the core glass ingot 5 are TeO.sub.2—Nb.sub.2O.sub.5—PbO and the cladding glass ingot 7 are TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5. As shown in FIGS. 1-5, the method for preparing all-solid-state photonic crystal fiber preform by extrusion in this embodiment comprises following steps 1-10.
(39) Step-1: An extrusion container 1, an extrusion chamber 2, an extrusion head 4, a core outlet mold 6 (the structure of which may be different from that in Embodiment 1), a fiber preform outlet mold 8 (the structure of which may be different from that in Embodiment 1), a first jacking rod 3 and a second jacking rod 12 are prepared in advance. The extrusion container 1 has an opening and a preform outlet 10 respectively on the top and the bottom of the extrusion container 1; the extrusion chamber 2 has a top opening 9 and a bottom opening respectively on the top and the bottom of the extrusion chamber 2 and a the bottom opening of the extrusion chamber 2 communicates with core outlets 60 on the core outlet mold 6. The size of the top opening 9 of the extrusion chamber 2 is smaller than the diameter of the first jacking end of the first jacking rod 3, and the size of the top opening 9 is greater than the diameter of the second jacking end of the second jacking rod 12. Herein, the core outlet mold 6 has N core outlets 60, where N≥2. In this embodiment, the top opening of the extrusion chamber 2 is preferably circular, and similarly, the core outlets 60 on the core outlet mold 6 are also preferably circular. The N core outlets 60 in this embodiment are distributed regularly, that is, they form a regular array of core outlets. The core outlet mold 6 is shown in
(40) The extrusion container, the extrusion chamber, the outlet molds, the first jacking rod, the second jacking rod and the extrusion head, which are prepared in the step 1, are all ultrasonically cleaned and wiped with alcohol before use. Due to the design that the size of the top opening of the extrusion chamber is smaller than the diameter of the first jacking end of the first jacking rod, it can be ensured that the first jacking end of the first jacking rod is always located on the outer side of the top of the extrusion chamber when the top of the extrusion chamber is extruded by the first jacking end of the first jacking rod, in order to ensure that the whole extrusion chamber is extruded downward by the first jacking end of the first jacking rod. Correspondingly, due to the design that the size of the top opening of the extrusion chamber is greater than the diameter of the second jacking end of the second jacking rod, it can be ensured that the second jacking end of the second jacking rod can run into the extrusion chamber from the top opening of the extrusion chamber during the subsequent extrusion process, to facilitate the extrusion of the corresponding TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot by the extrusion head. Of course, when the extrusion container, the extrusion chamber, the first jacking rod and the second jacking rod are ultrasonically cleaned and wiped with alcohol, they may be further cleaned with distilled water or deionized water.
(41) Step-2: TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot and TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass ingot which are rinsed with alcohol and dried, wherein the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot has an outer diameter matched with the inner diameter of the extrusion chamber; and the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass ingot has an outer diameter matched with the inner diameter of the extrusion container.
(42) Additionally, in the Step-2, the TeO2-Nb2O5-PbO core glass ingot and the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass ingot are all ultrasonically cleaned and wiped with alcohol before used, to remove impurities on the surfaces of the two kinds of heavy metal oxide glass ingot, in order to avoid adverse effect on the subsequent preparation of fiber preform by extrusion by those impurities. Of course, when the two kinds of glass ingot are ultrasonically cleaned and wiped with alcohol, they may be further cleaned with distilled water or deionized water.
(43) Here, the expression “the TeO2-Nb.sub.2O5-PbO core glass ingot and TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass ingot have an outer diameter matched with the inner diameter of the extrusion chamber” means that the TeO2-Nb.sub.2O5-PbO core glass ingot, as the raw material, can be exactly placed in the extrusion chamber, and the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass ingot can be closely fitted on the inner sidewall of the extrusion chamber.
(44) Step-3: Placing the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass ingot inside the bottom of the extrusion container 1, placing the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot and the extrusion head 4 inside the extrusion chamber 2, and mounting the core outlet mold 6 at the bottom of the extrusion chamber 2, the core outlet mold 6 is located above the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass ingot and the extrusion head 4 is located on the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot are assembled in such a way that the core outlet mold 6 is located above the TeO.sub.2—Nb.sub.2O.sub.5—PbO cladding glass ingot. The extrusion head 4 is located above the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot. The extrusion chamber 2 can protect the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot, to ensure that the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot can be wholly extruded into the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass ingot.
(45) Step-4: Putting the extrusion chamber 2 with the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot into the extrusion container 1, and resting the first jacking end of the first jacking rod 3 against the top surface of the extrusion chamber, aligning the center of the first jacking end of the first jacking rod 3 with the center of the core outlet mold 6
(46) Step-5: Heating the extrusion container 1 with the extrusion chamber of the step 4 until the temperature in the extrusion container 1 reaches a preset temperature T, so as to make the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot and the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass ingot in the extrusion container 1 soft to obtain softened TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass and TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass.
(47) Wherein the preset temperature T is higher than Tg and lower than Tx; Tg is defined as the highest one of the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass transition temperature and the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass transition temperature, and the Tx is defined as the lowest one of the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass crystallization temperature and the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass crystallization temperature. For example, according to the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass ingot and the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass ingot to be used, the preset temperature T in this embodiment is higher than 185° C. and lower than 370° C. For example, the preset temperature T is 200° C. The state before the extrusion of the extrusion chamber 2 by the first jacking rod 3 starts is shown in
(48) Step-6: Pressing the first jacking rod 3 against the top of the extrusion chamber 2, and pushing the extrusion chamber 2 into the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass inside the extrusion container 1, so as to make the bottom of the core outlets 60 of the core outlet mold 6 flush with the bottom of the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass or make the bottom of the core outlets 60 on the core outlet mold 6 is lower than the bottom of the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass. The application of the pressing process of the first jacking rod 3 onto the extrusion chamber 2 is in a vacuum chamber. That is, the extrusion chamber 2, the extrusion container 1 and the first jacking rod 3 are all put in the vacuum chamber for extrusion.
(49) Specifically, the vacuum chamber is vacuumized by a vacuum pump, inert gas is supplemented into the vacuum chamber when the degree of vacuum in the vacuum chamber is lower than 10.sup.−2 Pa, so as to make the pressure in the vacuum chamber same as the atmospheric pressure, for example, the supplemented inert gas is nitrogen.
(50) During the extrusion of the top of the extrusion chamber 2 by the first jacking rod 3, the opening of the extrusion container 1, the top opening 9 of the extrusion chamber 2, the center of the core outlet mold 6, and the preform outlet 10 on the extrusion container 1 are all located on a same line. This ensures that the fiber preform products prepared by extrusion will not bend. The state when the extrusion of the extrusion chamber 2 by the first jacking rod 3 ends is shown in
(51) Step-7: Maintaining the temperature inside the extrusion container 1 at the preset temperature T, taking the first jacking rod 3 out of the extrusion container 1 and putting the second jacking rod 12 into the extrusion container 1, in such a way that the second jacking end of the second jacking rod 12 runs through the top opening 9 of the extrusion chamber 2 and resists against the extrusion head 4. The state when the extrusion chamber 2 is extruded by the second jacking rod 12 is shown in
(52) Step-8: Making the second jacking rod 12 push the extrusion head 4 to press the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass inside the extrusion chamber 2, so that the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass is extruded out from the core outlets 60 on the core outlet mold 6 located on the bottom of the extrusion container, obtaining a core array having N TeO.sub.2—Nb.sub.2O.sub.5—PbO cores. The state when the extrusion of the extrusion chamber 2 by the second jacking rod 12 ends is shown in
(53) Step-9: Uniformly pressing the core glass in the extrusion chamber 2 and the cladding glass in the extrusion container 1, so that the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass and the TeO.sub.2—Nb.sub.2O.sub.5—PbO cladding glass are co-extruded out from the preform outlet 10 on the extrusion container 1 obtaining an initial product of the fiber preform.
(54) In the Step-9, both the TeO.sub.2—Nb.sub.2O.sub.5—PbO core glass in the extrusion chamber 2 and the TeO.sub.2—GeO.sub.2—Nb.sub.2O.sub.5 cladding glass in the extrusion container 1 are extruded at a constant speed. Thus, the uniformity of purity of the obtained initial products of the fiber preform and the finally obtained fiber preform products can be improved, and the fracture of the obtained initial products of the fiber preform and the finally obtained fiber preform products due to inconstant speed can be avoided. Therefore, the quality of the prepared fiber preform products is improved.
(55) The application of a stress onto the top of the extrusion chamber 2 by the second jacking rod 12 is also done in a vacuum chamber. That is, the extrusion chamber 2, the extrusion container 1 and the second jacking rod 12 are all put in the vacuum chamber for extrusion. Specifically, the vacuum chamber is vacuumized by a vacuum pump, inert gas is supplemented into the vacuum chamber when the degree of vacuum in the vacuum chamber is lower than 10.sup.−2 Pa, so as to make the pressure in the vacuum chamber same as the atmospheric pressure, for example, the supplemented inert gas is nitrogen.
(56) Step-10: Annealing the obtained initial product of the fiber preform at the transition temperature Tg for a preset period of time (here, 4 h), and cooling the initial product of the fiber preform to room temperature, then a fiber preform is obtained.
(57) The cross-section of the fiber preform products prepared in Embodiment 2 is shown in
(58) It can be found from the product structure shown in
(59) Of course, a top plate 16 is disposed in the extrusion chamber 2 covering the core glass ingot 5; and the extrusion head 4 has a plurality of extrusion stems 40 corresponding to each core outlet 60 on the core outlet mold 6 and capable of inserting into the corresponding core outlet 60 after passing through the top plate 16. As shown in
(60) To prepare fiber preform of different requirements, as an improvement to this embodiment, the core glass outlet mold connected to the bottom of the extrusion chamber may be designed to be adjustable according to the actual requirements. That is, by changing the cross-sectional shape of the preform outlet on the preform outlet mold 8, all-solid-state infrared-soft-glass-based photonic crystal fiber preform products having different cross-sectional shapes can be obtained correspondingly.
Embodiment 3
(61) In the Embodiment 3, it is set that the all-solid-state photonic crystal fiber preform to be prepared are fluorozirconate glass based photonic crystal fiber preform, and both the core glass ingot 5 and the cladding glass ingot 7 to be used are fluorozirconate glass ingot. Specifically, the core glass ingot 5 are Er.sup.3+-dopedZBLAN glass ingot and the cladding glass ingot 7 are non-doped ZBLAN glass ingot. As shown in FIGS. 1-5, the method for preparing fiber preform by extrusion in this embodiment comprises following steps 1-10.
(62) Step-1: An extrusion container 1, an extrusion chamber 2, an extrusion head 4, a core outlet mold 6 (the structure of which may be different from that in Embodiment 1 or Embodiment 2), a preform outlet mold 8 (the structure of which may be different from that in Embodiment 1 or Embodiment 2), a first jacking rod 3 and a second jacking rod 12 are prepared in advance. Wherein the extrusion container 1 has an opening and a preform outlet 10 respectively on the top and the bottom of the extrusion container 1; the extrusion chamber 2 has a top opening 9 and a bottom opening respectively on the top and the bottom of the extrusion chamber 2, and the bottom opening of the extrusion chamber 2 communicates with core outlets 60 on the core outlet mold 6. The size of the top opening 9 of the extrusion chamber 2 is smaller than the diameter of the first jacking end of the first jacking rod 3, to ensure that the first jacking end of the first jacking rod can run into the extrusion chamber 2 from the top opening. The size of the top opening 9 is greater than the diameter of the second jacking end of the second jacking rod 12. Herein, the core outlet mold 6 has N core outlets 60, N≥2. In this embodiment, the top opening of the extrusion chamber 2 is preferably circular, and similarly, the core outlets 60 on the core outlet mold 6 are also preferably circular. The N core outlets 60 in this embodiment are distributed regularly, that is, they form a regular array of core outlets. The core outlet mold 6 is shown in
(63) The extrusion container, the extrusion chamber, the outlet molds, the first jacking rod, the second jacking rod and the extrusion head, which are prepared in the step 1, are all ultrasonically cleaned and wiped with alcohol before use. Due to the design that the size of the top opening is greater than the diameter of the first jacking end of the first jacking rod, it can be ensured that the first jacking end of the first jacking rod is always located on the outer side of the top of the extrusion chamber when the top of the extrusion chamber is extruded by the first jacking end of the first jacking rod, in order to ensure that the whole extrusion chamber is extruded downward by the first jacking end of the first jacking rod. Correspondingly, due to the design that the size of the top opening of the extrusion chamber is greater than the diameter of the second jacking end of the second jacking rod, it can be ensured that the second jacking end of the second jacking rod can run into the extrusion chamber from the top opening of the extrusion chamber during the subsequent extrusion process, to facilitate the extrusion of the corresponding Er.sup.3+-doped ZBLAN core glass ingot by the extrusion head. Of course, when the extrusion container, the extrusion chamber, the first jacking rod and the second jacking rod are ultrasonically cleaned and wiped with alcohol, they may be further cleaned with distilled water or deionized water.
(64) Step-2: Er.sup.3+-doped ZBLAN core glass ingot and non-doped ZBLAN cladding glass ingot which are rinsed with alcohol and dried, wherein the Er.sup.3+-doped ZBLAN core glass ingot has an outer diameter matched with the inner diameter of the extrusion chamber; and the non-doped ZBLAN cladding glass ingot cladding glass ingot has an outer diameter matched with the inner diameter of the extrusion container.
(65) Additionally, in the Step-2, the Er.sup.3+-doped ZBLAN core glass ingot and the non-doped ZBLAN cladding glass ingot are all ultrasonically cleaned and wiped with alcohol before used, to remove impurities on the surfaces of the two kinds of fluorozirconate glass ingot, in order to avoid adverse effect on the subsequent preparation of fiber preform by extrusion by those impurities. Of course, when the two kinds of glass ingot are ultrasonically cleaned and wiped with alcohol, they may be further cleaned with distilled water or deionized water.
(66) Here, the expression “the Er.sup.3+-doped ZBLAN core glass ingot and the non-doped ZBLAN cladding glass ingot have an outer diameter matched with the inner diameter of the extrusion chamber” means that the Er.sup.3+-doped ZBLAN core glass ingot, as the raw material, can be exactly placed in the extrusion chamber, and the non-doped ZBLAN cladding glass ingot can be closely fitted on the inner sidewall of the extrusion chamber.
(67) Step-3: Placing the non-doped ZBLAN cladding glass ingot inside the bottom of the extrusion container 1, placing the Er.sup.3+-doped ZBLAN core glass ingot and the extrusion head 4 inside the extrusion chamber 2, and mounting the core outlet mold 6 at the bottom of the extrusion chamber 2, the core outlet mold 6 is located above the non-doped ZBLAN cladding glass ingot and the extrusion head 4 is located above the Er.sup.3+-doped ZBLAN core glass ingot. The extrusion chamber 2 can protect the Er.sup.3+-doped ZBLAN core glass ingot, to ensure that the Er.sup.3+-doped ZBLAN core glass ingot can be wholly extruded into the non-doped ZBLAN cladding glass ingot.
(68) Step-4: Putting the extrusion chamber 2 with the Er.sup.3+-doped ZBLAN core glass ingot into the extrusion container 1, and resting the first jacking end of the first jacking rod 3 against the top surface of the extrusion chamber, aligning the center of the first jacking end of the first jacking rod 3 with the center of the core outlet mold 6.
(69) Step-5: Heating the extrusion container 1 with the extrusion chamber of the step 4 until the temperature in the extrusion container 1 reaches a preset temperature T, so as to make the Er.sup.3+-doped ZBLAN core glass ingot and the non-doped ZBLAN cladding glass ingot in the extrusion container 1 soft to obtain softened Er.sup.3+-doped ZBLAN core glass and non-doped ZBLAN cladding glass.
(70) Wherein the preset temperature T is higher than Tg and lower than Tx; Tg is defined as the highest one of the Er.sup.3+-doped ZBLAN core glass transition temperature and the non-doped ZBLAN cladding glass transition temperature, and the Tx is defined as the lowest one of the Er.sup.3+-doped ZBLAN core glass crystallization temperature and the non-doped ZBLAN cladding glass crystallization temperature. For example, according to the Er.sup.3+-doped ZBLAN core glass ingot and the non-doped ZBLAN cladding glass ingot to be used, the preset temperature T in this embodiment is higher than 185° C. and lower than 370° C. For example, the preset temperature T is 200° C. The state before the extrusion of the extrusion chamber 2 by the first jacking rod 3 starts is shown in
(71) Step-6: Pressing the first jacking rod 3 against the top of the extrusion chamber 2, and pushing the extrusion chamber 2 into the non-doped ZBLAN cladding glass inside the extrusion container 1, so as to make the bottom of the core outlets 60 of the core outlet mold 6 flush with the bottom of the non-doped ZBLAN cladding glass or make the bottom of the core outlets 60 on the core outlet mold 6 is lower than the bottom of the non-doped ZBLAN cladding glass. The application of the pressing process of the first jacking rod 3 onto the extrusion chamber 2 is in a vacuum chamber. That is, the extrusion chamber 2, the extrusion container 1 and the first jacking rod 3 are all put in the vacuum chamber for extrusion.
(72) Specifically, the vacuum chamber is vacuumized by a vacuum pump, inert gas is supplemented into the vacuum chamber when the degree of vacuum in the vacuum chamber is lower than 10.sup.−2 Pa, so as to make the pressure in the vacuum chamber same as the atmospheric pressure, for example, the supplemented inert gas is nitrogen.
(73) During the extrusion of the top of the extrusion chamber 2 by the first jacking rod 3, the opening of the extrusion container 1, the top opening 9 of the extrusion chamber 2, the center of the core outlet mold 6, and the preform outlet 10 on the extrusion container 1 are all located on a same line. This ensures that the fiber preform products prepared by extrusion will not bend. The state when the extrusion of the extrusion chamber 2 by the first jacking rod 3 ends is shown in
(74) Step-7: Maintaining the temperature inside the extrusion container 1 at the preset temperature T, taking the first jacking rod 3 out of the extrusion container 1 and putting the second jacking rod 12 into the extrusion container 1, in such a way that the second jacking end of the second jacking rod 12 runs through the top opening 9 of the extrusion chamber 2 and resists against the extrusion head 4. The state when the extrusion chamber 2 is extruded by the second jacking rod 12 is shown in
(75) Step-8: Making the second jacking rod 12 push the extrusion head 4 to press the Er.sup.3+-doped ZBLAN core glass inside the extrusion chamber 2, so that the Er.sup.3+-doped ZBLAN core glass is extruded out from the core outlets 60 on the core outlet mold 6 located on the bottom of the extrusion container, obtaining a core array having N Er.sup.3+-doped ZBLAN cores. The state when the extrusion of the extrusion chamber 2 by the second jacking rod 12 ends is shown in
(76) Step-9: Uniformly pressing the core glass in the extrusion chamber 2 and the cladding glass in the extrusion container 1, so that the Er.sup.3+-doped ZBLAN core glass and the non-doped ZBLAN cladding glass are co-extruded out from the preform outlet 10 on the extrusion container 1 obtaining an initial product of the fiber preform.
(77) In the Step-9, both the Er.sup.3+-doped ZBLAN core glass in the extrusion chamber 2 and the non-doped ZBLAN cladding glass in the extrusion container 1 are extruded at a constant speed. Thus, the uniformity of purity of the obtained initial products of the fiber preform and the finally obtained fiber preform products can be improved, and the fracture of the obtained initial products of the fiber preform and the finally obtained fiber preform products due to inconstant speed can be avoided. Therefore, the quality of the prepared fiber preform products is improved.
(78) The application of a stress onto the top of the extrusion chamber 2 by the second jacking rod 12 is also done in a vacuum chamber. That is, the extrusion chamber 2, the extrusion container 1 and the second jacking rod 12 are all put in the vacuum chamber for extrusion. Specifically, the vacuum chamber is vacuumized by a vacuum pump, inert gas is supplemented into the vacuum chamber when the degree of vacuum in the vacuum chamber is lower than 10.sup.−2 Pa, so as to make the pressure in the vacuum chamber same as the atmospheric pressure, for example, the supplemented inert gas is nitrogen.
(79) Step-10: Annealing the obtained initial product of the fiber preform at the transition temperature Tg for a preset period of time (here, 4 h), and cooling the initial product of the fiber preform to room temperature, then a fiber preform is obtained.
(80) The cross-section of the fiber preform products prepared in Embodiment 3 is shown in
(81) It can be found from the product structure shown in
(82) Of course, there may be a top plate 16 is disposed in the extrusion chamber 2 covering the core glass ingot 5; and the extrusion head 4 has a plurality of extrusion stems 40 corresponding to each core outlet 60 on the core outlet mold 6 and capable of inserting into the corresponding core outlet 60 after passing through the top plate 16. As shown in
(83) To prepare fiber preform of different requirements, as an improvement to this embodiment, the core glass outlet mold connected to the bottom of the extrusion chamber may be designed to be adjustable according to the actual requirements. That is, by changing the cross-sectional shape of the preform outlet on the preform outlet mold 8, all-solid-state infrared-soft-glass-based photonic crystal fiber preform products having different cross-sectional shapes can be obtained correspondingly.
(84) It is to be noted that the method for preparing all-solid-state photonic crystal fiber preform by extrusion provided in the present invention can be applied to the preparation of infrared-soft-glass-based photonic crystal fiber preform and also to the preparation of other all-solid-state photonic crystal fiber preform.
(85) Although the preferred embodiments of the present invention have been described above in detail, it should be clearly understood that, for those skilled in the art, various changes and variations of the present invention may be possible. Any modifications, equivalent replacements and improvements made within the spirit and principle of the present invention should fall into the protection scope of the present invention.