CN1402028A - Rare earth element doped glass double-clad optical fiber and preparation method thereof - Google Patents
Rare earth element doped glass double-clad optical fiber and preparation method thereof Download PDFInfo
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- CN1402028A CN1402028A CN 02136859 CN02136859A CN1402028A CN 1402028 A CN1402028 A CN 1402028A CN 02136859 CN02136859 CN 02136859 CN 02136859 A CN02136859 A CN 02136859A CN 1402028 A CN1402028 A CN 1402028A
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- 239000011521 glass Substances 0.000 title claims abstract description 62
- 239000013307 optical fiber Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 19
- 238000005253 cladding Methods 0.000 claims abstract description 102
- 239000000835 fiber Substances 0.000 claims abstract description 69
- 239000000463 material Substances 0.000 claims abstract description 49
- 239000005365 phosphate glass Substances 0.000 claims abstract description 22
- 239000005368 silicate glass Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 23
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 8
- 230000007704 transition Effects 0.000 claims description 8
- 238000005491 wire drawing Methods 0.000 claims description 7
- 229910052787 antimony Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 230000004927 fusion Effects 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 238000005352 clarification Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 5
- 229920003023 plastic Polymers 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000003723 Smelting Methods 0.000 claims description 4
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 150000002910 rare earth metals Chemical class 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 235000019628 coolness Nutrition 0.000 claims description 2
- OENIXTHWZWFYIV-UHFFFAOYSA-N 2-[4-[2-[5-(cyclopentylmethyl)-1h-imidazol-2-yl]ethyl]phenyl]benzoic acid Chemical compound OC(=O)C1=CC=CC=C1C(C=C1)=CC=C1CCC(N1)=NC=C1CC1CCCC1 OENIXTHWZWFYIV-UHFFFAOYSA-N 0.000 claims 1
- 210000003050 axon Anatomy 0.000 claims 1
- 238000009472 formulation Methods 0.000 claims 1
- 239000011162 core material Substances 0.000 abstract description 95
- -1 rare earth ions Chemical class 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- 238000012681 fiber drawing Methods 0.000 abstract 1
- 239000010453 quartz Substances 0.000 description 22
- 239000000758 substrate Substances 0.000 description 21
- 238000005516 engineering process Methods 0.000 description 10
- 238000005086 pumping Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
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- 230000009286 beneficial effect Effects 0.000 description 2
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- 238000003825 pressing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 2
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
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Abstract
A rare-earth element doped glass double-clad optical fiber and a preparation method thereof are disclosed, wherein the periphery of a fiber core of the optical fiber is coated with an inner cladding and an outer cladding on the same central axis. The material of the core is a phosphate glass system. The material of the inner cladding is a phosphate glass system or a silicate glass system that matches the core material in terms of refractive index, expansion coefficient, and softening temperature. Selecting glass raw materials of the fiber core and the inner cladding according to the matching relation, melting, preparing a prefabricated rod to form a core-cladding combination body, and finally carrying out the specific steps of optical fiber drawing to obtain the glass double-clad optical fiber. Compared with the prior art, the glass double-clad fiber has the advantages of higher concentration of doped rare earth ions, larger stimulated emission cross section, larger tunable range and larger gain. The preparation method is simple and the production cost is low.
Description
Technical field:
The invention relates to a kind of rare earth doped glass doubly-clad optical fiber and preparation method thereof, being particularly related to optical fiber core material material (abbreviation core material) and inner cladding is the multicomponent glass material of non-quartz substrate, and surrounding layer is doubly clad optical fiber of plastics and preparation method thereof.
Background technology:
Fiber laser is that optical fiber and the bulk of optical feedback element by some rare earth element of mixing constitutes laserresonator, under the effect of pump light, produces stimulated emission in the doped fiber medium, and forms the laser of certain wavelength coverage.Have advantages such as low threshold value, high-level efficiency, narrow linewidth, tunability.The characteristics of fiber laser have determined it to have more superiority than semiconductor laser and other large-scale laser.But initial fiber laser is that pump light directly is coupled into the fibre core of diameter less than 10 μ m, causes coupling efficiency low, and the output power of fiber laser is low, has limited its range of application.In order to overcome above-mentioned difficulties, in recent years, developed a kind of doubly clad optical fiber in the world, because it has the inner cladding of larger cross-section and numerical aperture, can effectively absorb the big pump light of the angle of divergence, utilize cladding pumping, overcome the shortcoming of above-mentioned single covering, make output power obtain greatly to improve, promoted the development of high-capacity optical fiber laser greatly.It is single-mode laser that the advantage of double clad pumping is no longer to require pump light, thereby can use the laser pump (ing) of high power multiple die semiconductor, pump energy does not need directly to be coupled in the fibre core, but be coupled in the inner cladding, and constantly excite dopant ion in the fibre core, like this pump light is had higher absorptivity, cause light-light conversion efficiency height, thereby realize high power output.U.S. light torch (SDL) company is (referring to technology [1] V.Dominc formerly, S.MacCormack, R.Waarts.et al.110W fiber Laser.Electronics letters, 1999, Vol35:1158～1160) reported that in 1999 output power is the cladding pumping laser instrument of 110W.The cladding pumping laser instrument just is being widely used in aspects such as communication, military affairs, industrial processes, medical treatment, printing at present.
The material that is used for the fiber amplifier of cladding pumping or doubly clad optical fiber fibre core on the fiber laser and inner cladding at present all is quartz substrate basically.There is following weak point in doubly clad optical fiber for quartz substrate:
(1) rare earth ion doping content in quartz substrate lower (＜2wt%).Because the cluster phenomenon easily takes place in rare earth ion in quartz substrate, cause that fluorescence lifetime sharply reduces, so can only operate under the situation that doping with rare-earth ions concentration is lower in quartz, can cause doubly clad optical fiber lower like this to the pump light absorptivity, to such an extent as to optical fiber must very longly could absorb fully, but length is long more, and its loss is also big more, nor is beneficial to miniaturization of devices.People such as U.S.'s Polaroid (Polaroid) M.Muendel of company are (referring to technology [2] M.Muendel formerly, B.Engstrom, D.Kea, et al.35-Watt CW singlemode Ytterbium FiberLaser.CLEO ' 97, CPD30-2/649) reported that output power is the double-clad laser of 35W, that is adopted mixes Yb
3+The quartz substrate doubly clad optical fiber, its fibre core and inner cladding material adopt modified chemical vapor deposition process (MCVD) (MCVD) preparation, Yb
3+Ion doping concentration only is 1.5wt%, and core diameter is 8 μ m, and xsect is that the inner cladding of rectangle is of a size of 170 * 330 μ m
2, the numerical aperture (NA) that inner cladding and core material constitute is 0.07, and surrounding layer is an organic polymer, and the surrounding layer diameter is 500 μ m, and the numerical aperture (NA) that surrounding layer and inner cladding constitute is 0.48, fully absorbs for making pump light, fiber lengths reaches 50 meters unexpectedly.
(2) gain of rare earth ion in quartz substrate is less.This mainly is because the stimulated emission cross section of rare earth ion in quartz substrate is less.
(3) the doubly clad optical fiber composition adjustable extent of quartz substrate is little.It mainly adds a small amount of other elements (for example: P, Ge etc.) and changes refractive index on pure quartz substrate, the composition variation range is narrower.
(4) the doubly clad optical fiber complicated process of preparation of quartz substrate, cost is higher.This mainly is because the prefabricated rods of the doubly clad optical fiber of quartz substrate is to adopt inside deposition method (for example: MCVD (modified chemical vapor deposition process (MCVD)) and PCVD (chemical vapour deposition technique of plasma-activated) etc.) preparation, the deposition process complexity, the equipment requirements costliness, wire-drawing temperature is higher.As, U.S. Pat 6345141 (referring to technology [3] US6345141 formerly; Date of publication is: Feb.5.2002; Title: Double-clad optical fiber with improvedinner cladding geometry) proposed the doubly clad optical fiber of the quartz substrate of multiple different inner cladding shapes.
In sum, the doubly clad optical fiber of quartz substrate exists that doping concentration of rare earth ion is low, the deficiency of several aspects such as gain is little, the composition variation range is narrow, preparation cost is high, complicated process of preparation.
Summary of the invention:
The object of the present invention is to provide the multicomponent glass of the non-quartz substrate of a kind of usefulness to prepare doubly clad optical fiber, the existing doping concentration of rare earth ion of doubly clad optical fiber that can effectively overcome quartz substrate in the technology formerly of being similar to is low, it is little to gain, the composition variation range is narrow, the preparation cost height, the deficiency of aspects such as complicated process of preparation.
Doubly clad optical fiber cross sectional shape of the present invention as depicted in figs. 1 and 2, comprise fibre core 1, surround the inner cladding 2 of fibre core 1 and surrounding layer 3 three parts of surrounding inner cladding 2, three's central axes, fibre core 1 material selection phosphate glass system wherein, its glass formula scope is as shown in table 1, fiber core cross section is circular, fibre core 1 typically have a diameter from φ 5～60 μ m, wherein core diameter be φ 5～12 μ m can be used as fiber laser output single-mode laser bundle, be commonly referred to single-mode fiber, other larger-diameter fibre core is called multimode optical fiber.The material selection phosphate glass system of inner cladding or silicate glass system, its glass formula scope is as shown in table 2, and inner cladding has the refractive index low than fibre core, that is, and n
In＜n
Core, its shape of cross section is square (as Fig. 1) or a rectangle (as Fig. 2), or other polygon.Surrounding layer is made of polymeric material such as plastics, and the surrounding layer shape of cross section is circular, its refractive index n
OutwardBe lower than inner cladding refractive index, n
In, that is, and n
Outward＜n
In
The topmost not only doping content height (than the high at least order of magnitude of quartz substrate) in phosphate glass of fibre core 1 interior rare earth ion that is characterised in that of doubly clad optical fiber of the present invention, and also big than quartz substrate of stimulated emission cross section, the prepared optical fiber unit length gain big (than the high at least order of magnitude of doubly clad optical fiber of quartz substrate) that goes out, superiority of the present invention in addition also is: (a) glass ingredient of the glass ingredient of inner cladding 2 and fibre core is complementary.(b) can select the glass ingredient scope big.(c) among the preparation technology, prefabricated rods preparation and drawing process are simple, and preparation cost is low.
The used multicomponent glass prescription of glass formula table 2 inner cladding that table 1 fibre core is used
| The phosphate glass system | |
| Composition | Content (mol%) |
| ??P 2O 5 | ????55～70 |
| ??Al 2O 3 | ????4～10 |
| ??BaO | ????4～14 |
| ??Na 2O | ????3～8 |
| ??K 2O | ????3.5～15 |
| ??Nb 2O 5 | ????0.4～3.4 |
| ??La 2O 3 | ????0.3～3.0 |
| ??Y 2O 3 | ????0.2～6 |
| ??Sb 2O 3 | ????0～0.2 |
| ??Yb 2O 3Or Er 2O 3Or Nd 2O 3Or Ho 2O 3Or Tm 2O 3Or Dy 2O 3 | ? ? ????0.2～6 ? ? ? |
| The phosphate glass system | The silicate glass system | ||
| Composition | Content (mol%) | Composition | Content (mol%) |
| ??P 2O 5 | ??54.5～71 | ????SiO 2 | ????61.8～74 |
| ??Al 2O 3 | ??4～8 | ????B 2O 3 | ????2～15 |
| ??BaO | ??4～16.5 | ????Na 2O | ????0～8.2 |
| ??Na 2O | ??3～8 | ????K 2O | ????3.7～8.8 |
| ??K 2O | ??5～15.5 | ????CaO | ????0～4.5 |
| ??Nb 2O 5 | ??0.4～2 | ????ZnO | ????0～6.6 |
| ??La 2O 3 | ??0.3～2.8 | ????PbO | ????0～0.6 |
| ??Y 2O 3 | ??0.5～5.3 | ????KHF 2 | ????0～19.5 |
| ??Sb 2O 3 | ??0～0.2 | ????Sb 2O 3 | ????0～0.2 |
The concrete steps of the preparation process of glass doubly-clad optical fiber of the present invention are:
1. the prescription of the first step, fibre core 1 material (being designated hereinafter simply as core material) and inner cladding 2 materials (by mole number percent) is chosen.
The prescription of core material and the prescription of inner cladding should be to mate mutually, when selecting prescription, after at first determining the concrete prescription of core material, determine the component of inner cladding material at the matching relationship of existence aspect three of the refractive indexes, expansion coefficient, softening temperature according to core material and inner cladding material.At first definite core material glass is chosen the phosphate glass system, and concrete compositional range sees Table 1.By mole number percent is 55～70%P
2O
5, 4～10%Al
2O
3, 4～14%BaO, 3～8%Na
2O, 3.5～15%K
2O, 0.4～3.4%Nb
2O
5, 0.3～3%La
2O
3, 0.2～6%Y
2O
3, 0～0.2%Sb
2O
3, 0.2～6%Yb
2O
3, or Er
2O
3, or Nd
2O
3, or Ho
2O
3, or Tm
2O
3, or Dy
2O
3Select the used glass formula of inner cladding that two kinds of glass systems are arranged: to be (pressing mol%): 54.5～71%P (a) for phosphate glass system prescription
2O
5, 4～8%Al
2O
3, 4～16.5%BaO, 3～8%Na
2O, 5～15.5%K
2O, 0.4～2%Nb
2O
5, 0.3～2.8%La
2O
3, 0.5～5.3%Y
2O
3, 0～0.2%Sb
2O
3, be (pressing mol%): 61.8～74%SiO (b) for silicate glass system prescription
2, 2～15%B
2O
3, 0～8.2%Na
2O, 3.7～8.8%K
2O, 0～4.5%CaO, 0～6.6%ZnO, 0～0.6%PbO, 0～19.5%KHF
2, 0～0.2%Sb
2O
3Core material of the invention described above and inner cladding glass are the condition below satisfying aspect three of refractive indexes, expansion coefficient, softening temperature:
(a) core material refractive index n core and inner cladding glass refraction n
InBetween close and to be: n
CoreGreater than n
In, i.e. n
Core＞n
Bag, above-mentioned both refractive indexes of selected prescription differ n
Core-n
InBe 0.15%～3%;
(b) coupling between the expansion coefficient of core material glass expansion coefficient and inner cladding glass does not produce internal compressive stress with Cheng Sihou and is as the criterion, differ generally speaking ± 20 * 10
-7/ ℃.
(c) transition temperature between core material and the inner cladding material differs in 30 ℃, and softening temperature can differ in 50 ℃.
The selection of the prescription of core material of the invention described above and inner cladding glass has not only reached above-mentioned matching relationship each other, and select the general requirement that can reach: the good mechanical property of glass, chemical stability are good, the most important thing is to be difficult for producing under wire-drawing temperature the crystallization phenomenon.
2. the glass smelting of second step, core material and inner cladding.
(a) core material glass is founded: after by the prescription of determining in the above-mentioned first step raw material being mixed, at first be placed in the silica crucible and melt, temperature of fusion is 1200～1300 ℃, after raw material melts fully, logical oxygen dewaters, reach capacity up to fluorescence lifetime, then its grog is poured in the platinum crucible, temperature still remains on 1200～1300 ℃, stir successively, the operation (whole process was greater than 5 hours) of clarification is cast on the swage at last, is moved into to be preheating in the muffle furnace that temperature is material transition temperature (Tg) and anneals, insulation earlier 2 hours, lower the temperature 50～100 ℃ with 2 ℃/hour speed then, and then be cooled to room temperature, take out again after the cooling fully with 5 ℃/hour speed.
(b) inner cladding 2 glass smeltings: according to the inner cladding glass formula of determining in the above-mentioned first step, when selecting the phosphate glass system for use, it is founded, and process is founded process with above-mentioned core material glass, conditionally complete is identical.When selecting the silicate glass system for use, be placed directly in the platinum crucible after mixing by the raw material of above-mentioned first step prescription and melt, stir successively, the operating process of clarification (whole process needs more than 5 hours), temperature of fusion remains on 1300～1450 ℃ always, be cast on the swage at last, be moved in the muffle furnace that preheat temperature is material transition temperature (Tg) and anneal, insulation earlier 2 hours, then with after 50～100 ℃ of 2 ℃/hour the speed coolings, be cooled to room temperature with 5 ℃/hour speed again, take out again after the cooling fully.
3. the 3rd go on foot, prepare prefabricated rods.
According to the size of the xsect of the diameter of the fiber core 1 that will draw and inner cladding and diameter and the length that their length is determined prepared prefabricated rods, for example: can adopt ratio d plug=200～500d between the two
Core, d
The bag rod=(200～500) * (200～500)) d
Bag, d wherein
PlugBe the diameter of fibre core prefabricated rods, d
CoreBe core diameter, d
The bag rodBe the cross-sectional area of inner cladding prefabricated rods, d
BagBe the inner cladding cross-sectional area.
The above-mentioned core material glass that makes is cut, the part that the optics good uniformity is all cut out in requirement, be polished into round bar shape, pass through steps such as frosted, polishing then successively, be processed into the prefabricated rods (being designated hereinafter simply as plug) of the fibre core 1 of required size, it is more than 2 grades that mandrel surface polishing smooth finish requires.
The above-mentioned inner cladding glass material that makes is cut, require to cut out the good part of optical homogeneity, be polished into round bar shape, pass through steps such as frosted, polishing then successively, hole in the axial centre that is processed into inner cladding glass pole again.The prefabricated rods of making inner cladding is a cover rod, polishes overlapping excellent bore area, and the profile that hole-drilled inner cladding cover rod is processed into xsect is desired shape at last, and is polygonal bar-shaped as square or rectangle or other.With ultrasound wave or hydrofluorite plug and excellent surface impurity or the pollutant of inner cladding cover that processes cleaned again.The plug that processing is handled well inserts in the center hole of inner cladding cover rod, and guarantees both the tight contacts and the coincidence of both central axis, makes the assembly of plug and inner cladding, is called for short core package zoarium.
4. the 4th the step, fibre-optical drawing.
Above-mentioned core package zoarium is fixed on the wire drawing machine, under 650～700 ℃ temperature, after core package zoarium is drawn into optical fiber, optical fiber is passed be equipped with device to form surrounding layer 3 as the melt liquid plastics of surrounding layer 3, again this doubly clad optical fiber is passed after ultraviolet-curable materials applies, solidify with the xenon lamp irradiation, finally be drawn into the doubly clad optical fiber that meets the demands.Produce qualified fiber lengths with this production technology and can reach 1km at least.
The beneficial effect that the present invention produced is: provide high-capacity optical fiber laser and fiber amplifier employed doubly clad optical fiber, satisfy the requirement of current optical communication development, with Nd
3+Ion doping is an example, is about 2.0 * 10 according to the stimulated emission cross section of doubly clad optical fiber acquisition in the silicate glass system of the invention described above
-20Cm
2, the stimulated emission cross section 3.9 * 10 in the phosphate glass system
-20Cm
2, all the stimulated emission cross section than the quartz substrate of used doping in the technology formerly is big.Compare with the silica fibre of quartz substrate doping with rare-earth ions in the technology formerly, glass doubly-clad optical fiber doping content of the present invention is higher, and tunable range is bigger, and it is bigger to gain, and the preparation method is fairly simple, and production cost is also lower.
Description of drawings:
Fig. 1 is foursquare multicomponent glass doubly clad optical fiber schematic cross-section for inner cladding of the present invention
Fig. 2 is the square multicomponent glass doubly clad optical fiber schematic cross-section of square for inner cladding of the present invention
Embodiment:
The invention will be further described below in conjunction with embodiment.
First-selected definite core material and inner cladding glass formula.Table 3 and table 4 have provided 6 core assembly material and inner cladding glass formula, and wherein the core material and the inner cladding glass of the combination of 3 groups in the table 3 all are the phosphate glass system, and core material is the phosphate glass system in three groups of combinations of table 4, and inner cladding is the silicate glass system.
The 1st group of material of specific embodiment 1-
Table 3
| The 1st group | The 2nd group | The 3rd group | ||||
| Component (mol%) | Fibre core | Inner cladding | Fibre core | Inner cladding | Fibre core | Inner cladding |
| P 2O 5 | ????60.0 | ??61.0 | ????55.0 | ??54.5 | ????70 | ????71 |
| Al 2O 3 | ????4.0 | ??4 | ????5.0 | ??5.0 | ????7 | ????8 |
| BaO | ????10.0 | ??10.0 | ????14.0 | ??16.5 | ????4 | ????4 |
| Na 2O | ????4.0 | ??4.5 | ????3.0 | ??3.0 | ????8 | ????8 |
| K 2O | ????15.0 | ??15.5 | ????13.0 | ??13.0 | ????5.6 | ????5 |
| Nb 2O 5 | ????0.4 | ??0.4 | ????2 | ??2 | ????0.5 | ????0.5 |
| La 2O 3 | ????0.3 | ??0.3 | ????1.5 | ??1.5 | ????0.3 | ????2.8 |
| Y 2O 3 | ????0.2 | ??5.3 | ????4.5 | ??4.4 | ????0.5 | ????0.5 |
| The 1st group | The 2nd group | The 3rd group | ||||
| Component (mol%) | Fibre core | Inner cladding | Fibre core | Inner cladding | Fibre core | Inner cladding |
| Sb 2O 3 | ????0.1 | ???0 | ????0 | ???0.1 | ????0.1 | ???0.2 |
| Yb 2O 3 | ????6 | ???- | ????2 | ???- | ????4 | ???- |
| Stimulated emission cross section (* 10 -20cm 2) | ????1.69 | ???- | ????1.72 | ???- | ????1.65 | ???- |
| Fluorescence lifetime (ms) | ????2.2 | ???- | ????2.3 | ???- | ????2.3 | ???- |
| Fiber core diameter (μ m) | ????10μm | ????????6μm | ?????????30μm | |||
| The core glass refractive index n Core | ????1.530 | ????????1.528 | ?????????1.511 | |||
| Numerical aperture | ????0.10 | ????????0.08 | ?????????0.12 | |||
By above-mentioned specific practice.The first step: choose glass formula, press table 3.The 1st assembly side that at first chooses in the table 3 is the core material refractive index n that satisfies above-mentioned conditional request
CoreGreater than inner cladding glass refraction n
In, both poor (n
Core-n
In) between 0.15%～3%.
In second step, it is identical with inner cladding glass melting rule to found core material, that is: core material takes by weighing about 2500 grams of mixed material of above-mentioned prescription, takes by weighing about 5000 grams of inner cladding glass mixed material.At first melt raw material in 1.5 liter silica crucibles, temperature of fusion is 1250 ℃, and after raw material melted fully, logical oxygen dewatered, and reaches capacity up to fluorescence lifetime.Grog is poured in the platinum crucible of 1.2 liters then, stirred successively, operations such as clarification, whole process needs 5 hours approximately.Be cast at last on the swage that is of a size of 150mm * 70mm * 60mm, immigration is preheating to material transition temperature T g and anneals in 430 ℃ the muffle furnace, is incubated 2 hours, is cooled to 380 ℃ with 2 ℃/hr speed then, reduce to room temperature with 5 ℃/hr again, take out the cooling back fully.
Test result shows: the refractive index of prepared core material glass is 1.530, Yb
3+Ion stimulated emission cross section in core material glass is 1.6 * 10
-20Cm
2
The 3rd step: the preparation prefabricated rods, at first consider will do single-mode fiber, core diameter d
Core＜12 μ m, single-mode fiber must meet the following conditions:
Wherein a is the radius of fibre core, and λ is a transmission light wavelength in the optical fiber, n
CoreBe the refractive index of core fibre 1, n
InRefractive index for inner cladding.So selecting the core material preform core to be processed into diameter is 2mm (d
Plug=200d
Core), length is 60mm, and glass surface is polished to 3 grades of smooth finish.The prefabricated rods processing dimension of inner cladding is 25mm * 25mm * 80mm (d
The bag rod=(200 * 200) d
Bag), positive center, upper and lower end face drill diameter is the endoporus of 2mm, and the degree of depth is 60mm, and bore area will polish.With ultrasound wave plug and surrounding layer are overlapped excellent surface and carry out the decontamination cleaning treatment.Plug is inserted inner cladding overlap in the excellent center pit, constitute both core package zoariums.
The 4th step, fibre-optical drawing.Above-mentioned core package zoarium is put into the wire drawing machine heating furnace.Making temperature slowly rise to 650 ℃ (rises to 650 ℃ from normal temperature and needs 1.5hr at least, in room temperature to 250 ℃ following scope, heating rate is slower), the prefabricated rods stub bar falls down, with wire drawing machine with its drawing optic fibre, wire drawing speed is 10m/min, become fibre after, pass at once and form surrounding layer after the device that dissolves liquid plastics is housed.Then this doubly clad optical fiber is passed again and solidify with the xenon lamp irradiation after ultraviolet-curable materials applies, finally being drawn into the fibre core numerical aperture is NA=0.100, core diameter is 10 μ m, the inner cladding cross-sectional shape is that the square length of side is 125 μ m, the surrounding layer diameter be φ 170 μ m mix the ytterbium glass doubly-clad optical fiber, produce qualified fiber lengths with above-mentioned preparation method and can reach 1km at least.
The 2nd, 3 groups of materials of specific embodiment 2-
2nd, 3 groups of glass formulas see Table 3, and the melting technology of core material and inner cladding glass is identical with the foregoing description 1.
For the 2nd group, it is 3mm (d that the plug glass processing becomes diameter
Plug=500d
Core), length is the prefabricated rods of 60mm, it is 50mm * 50mm * 80mm (d that the inner cladding prefabricated rods is processed into processing dimension
The bag rod=(400 * 400) d
Bag), positive center, upper and lower end face drill diameter is the endoporus of 2mm, the degree of depth is the inner cladding cover rod of 60mm.Its subsequent step and drawing process are identical with embodiment 1.The final numerical aperture of doubly clad optical fiber that is made of the 2nd core assembly material and inner cladding material is 0.08, and core diameter is 6 μ m, and the inner cladding length of side is 125 μ m, and external diameter is φ 170 μ m.For the 3rd group, it is 6mm (d that the plug glass processing becomes diameter
Plug=200d
Core), length is the 60mm prefabricated rods, it is 25mm * 25mm * 80mm (d that the inner cladding prefabricated rods is processed into processing dimension
The bag rod=(200 * 200) d
Bag), positive center, upper and lower end face drill diameter is the endoporus of 2mm, the degree of depth is the inner cladding cover rod of 60mm.Its subsequent step and drawing process are identical with embodiment 1.The final numerical aperture of doubly clad optical fiber that is made of the 3rd core assembly material and inner cladding material is 0.12, and core diameter is 30 μ m, and the inner cladding cross-sectional shape quadrate length of side is 125 μ m, and whole optical fiber external diameter is φ 170 μ m.
The 4th, 5,6 groups of materials of specific embodiment 3-
The the 4th, 5,6 three group in the table 4 all is that core material is the phosphate glass system, and inner cladding is the silicate glass system.
For the the 4th, the 5th, the 6th group, core material glass found with specific embodiment 1 in identical, the inner cladding glass smelting is to take by weighing 3000 grams according to the synthetic raw material of inner cladding prescription that above-mentioned silicate glass system chooses, can directly in the platinum crucible of 2.0 liters, melt after mixing, temperature of fusion is 1350 ℃, stir successively, processes such as clarification, whole process needs more than 5 hours.Be cast at last on the swage that is of a size of 120mm * 70mm * 50mm, immigration is preheating to material transition temperature T g and anneals in 460 ℃ the muffle furnace, and insulation earlier 2 hours is cooled to 380 ℃ with 2 ℃/hr speed then, reduce to room temperature with 5 ℃/hr again, take out the cooling back fully.The plug of back is also all identical with embodiment 1 with processing of the prefabricated rods of inner cladding and drawing process.
Table 4
| The 4th group | The 5th group | The 6th group | ||||||||||
| Core (mol%) | Inner cladding (mol%) | Core (mol%) | Inner cladding (mol%) | Core (mol%) | Inner cladding (mol%) | |||||||
| P 2O 5 | ??55.0 | ??SiO 2 | ??61.8 | ?P 2O 5 | ??70 | ?SiO 2 | ???72 | ??P 2O 5 | ??60.0 | ??SiO 2 | ???73.4 | |
| Al 2O 3 | ??10.0 | ??B 2O 3 | ??15.0 | ?Al 2O 3 | ??7 | ?B 2O 3 | ???3.3 | ??Al 2O 3 | ??4.0 | ??B 2O 3 | ????2.0 | |
| BaO | ??10.0 | ??Na 2O | ??0 | ?BaO | ??8 | ?Na 2O | ???6.0 | ??BaO | ??10.0 | ??Na 2O | ????8.2 | |
| Na 2O | ??3.0 | ??K 2O | ??3.7 | ?Na 2O | ??6 | ?K 2O | ???8.8 | ??Na 2O | ??4.0 | ??K 2O | ????7.5 | |
| K 2O | ??12.0 | ??CaO | ??0.0 | ?K 2O | ??3.5 | ?CaO | ???2.9 | ??K 2O | ??15.0 | ??CaO | ????4.5 | |
| Nb 2O 5 | ??3.4 | ??ZnO | ??0 | ?Nb 2O 5 | ??0.5 | ?ZnO | ???6.6 | ??Nb 2O 5 | ??0.4 | ??ZnO | ????2.8 | |
| La 2O 3 | ??3.0 | ??PbO | ??0 | ?La 2O 3 | ??1.4 | ?PbO | ???0.3 | ??La 2O 3 | ??0.2 | ??PbO | ????0.6 | |
| Y 2O 3 | ??2.5 | ??KHF 2 | ??19.5 | ?Y 2O 3 | ??0.5 | ?KHF 2 | ???0 | ??Y 2O 3 | ??6 | ??KHF 2 | ????0.8 | |
| Sb 2O 3 | ??0.1 | ??Sb 2O 3 | ??0 | ?Sb 2O 3 | ??0.1 | ?Sb 2O 3 | ???0.1 | ??Sb 2O 3 | ??0.2 | ??Sb 2O 3 | ????0.2 | |
| Yb 2O 3 | ??1.0 | ?Yb 2O 3 | ??3 | ??Yb 2O 3 | ??0.2 | |||||||
| Refractive index | ??????1.494 | ??????1.488 | ???????1.523 | ??????1.522 | ???????1.520 | ??????1.518 | ||||||
| Expansion coefficient (10 -7/℃) | ??????106 | ??????91 | ???????100 | ??????94 | ???????104 | ??????91 | ||||||
| Softening temperature (℃) | ??????480 | ??????500 | ???????487 | ??????514 | ???????491 | ??????508 | ||||||
Claims (2)
1. rare earth doped glass doubly-clad light, comprise fibre core (1), surround the inner cladding (2) of fibre core (1), surround the surrounding layer (3) of inner cladding (2), the same central axis of three, it is characterized in that said fibre core (1) is that phosphate glass system by doped with rare-earth elements constitutes, concrete prescription by mole number percent is: contain 55～70% P
2O
5, 4～10% Al
2O
3, 4～14% BaO, 3～8% Na
2O, 3.5～15% K
2O, 0.4～3.4% Nb
2O
5, 0.3～3.0% La
2O
3, 0.2～6% Y
2O
3, 0～0.2% Sb
2O
3, 0.2～6% Yb
2O
3, or Er
2O
3, or Nd
2O
3, or Ho
2O
3, or Tm
2O
3, or Dy
2O
3
Said inner cladding (2) is to be made of the phosphate glass system of doped with rare-earth elements or silicate glass system;
System specifically fills a prescription for phosphate glass, by mole number percent is: contain 54.5～71% P
2O
5, 4～8% Al
2O
3, 4～16.5% BaO, 3～8% Na
2O, 5～15.5% K
2O, 0.4～2% Nb
2O
3, 0.3～2.8%La
2O
3, 0.5～5.3% Y
2O
3, 0～0.2% Sb
2O
3
System specifically fills a prescription for silicate glass, by mole number percent is: contain 61.8～74% SiO
2, 2～15% B
2O
3, 0～8.2% Na
2O, 3.7～8.8% K
2O, 0～4.5% CaO, 0～6.6% ZnO, 0～0.6% PbO, 0～19.5% KHF
2, 0～0.2% Sb
2O
3
2. the preparation method of rare earth doped glass doubly-clad optical fiber according to claim 1 is characterized in that the concrete steps of preparation process are:
＜1〉for the formulation selection of fibre core (1) material and inner cladding (2) material:
At first determine the prescription of fibre core (1) material, come to determine the prescription of inner cladding (2) material according to inner cladding (2) material and fibre core (1) material again at the matching relationship that exists aspect three of refractive index, expansion coefficient and the softening temperatures then, the matching relationship of said three aspects is: the 1. refractive index n of fibre core (1) material
CoreRefractive index n greater than inner cladding (2) material
Bag2. the expansion coefficient of fibre core (2) expansion coefficient and inner cladding (2) material differ ± 20 * 10
-7/ ℃ 3. the transition temperature between fibre core (1) material and inner cladding (2) material differs less than 30 ℃, and softening temperature differs less than 50 ℃; For this reason, after fibre core (1) material selection phosphate glass system, inner cladding (2) material selection phosphate glass system or silicate glass system;
＜2〉glass smelting of fibre core (1) and inner cladding (2):
1. founding of fibre core (1) phosphate glass system: according to the above-mentioned raw material of choosing prescription, after raw material mixed, at first be placed in the silica crucible and melt, temperature of fusion is 1200～1300 ℃, after raw material melts fully, logical oxygen dewaters, reach capacity up to fluorescence lifetime, then its grog is poured in the platinum crucible, temperature still remains on 1200～1300 ℃, stir successively, the operating process of clarification, be cast at last on the swage, be moved in the muffle furnace that preheat temperature is material transition temperature (Tg) and anneal, insulation earlier 2 hours, then with after 50～100 ℃ of 2 ℃/hour the speed coolings, be cooled to room temperature with 5 ℃/hour speed again;
2. founding of inner cladding (2) glass: when inner cladding (2) material was the phosphate glass system, the process of founding of founding process and above-mentioned fibre core (1) phosphate glass system was identical; When inner cladding (2) material is the silicate glass system, after mixing by above-mentioned raw material, directly putting into platinum crucible melts, the operating process of stirring successively and clarifying, keep temperature of fusion is 1300～1450 ℃ always, is cast on the swage at last, be moved in the muffle furnace that preheat temperature is material transition temperature (Tg) and anneal, insulation earlier 2 hours is lowered the temperature 50～100 ℃ with 2 ℃/hour speed then, and then is cooled to room temperature with 5 ℃/hour speed;
＜3〉preparation prefabricated rods:
At first according to the size and the definite size that will prepare prefabricated rods of their length of the diameter and inner cladding (2) cross-sectional area of the fiber core (1) that will draw; Found fibre core (1) the glass cutting that obtains and be polished into round bar shape above-mentioned, pass through frosted, polishing then successively, be processed into fibre core (1) prefabricated rods of required size; Found inner cladding (2) the glass cutting that obtains and be polished into round bar shape above-mentioned, carry out frosted and polishing then successively; Hole to the center in the glass pole axon of inner cladding (2) again, the prefabricated rods of making inner cladding (2) is a cover rod, polish overlapping excellent bore area again, the sharp processing that to overlap excellent xsect again becomes desired square or rectangular or other polygon, with ultrasound wave or hydrofluorite to above-mentioned make fibre core (1) prefabricated rods and cover rod and clean after, the prefabricated rods of fibre core (1) is inserted in the cover rod, constituted core package zoarium;
＜4〉fibre-optical drawing:
Above-mentioned core package zoarium is fixed on the wire drawing machine, under 650～700 ℃ temperature, after core package zoarium is drawn into optical fiber, optical fiber is passed be equipped with device to form surrounding layer (3) as the melt liquid plastics of surrounding layer (3), its doubly clad optical fiber is passed after ultraviolet-curable materials applies, solidify with the xenon lamp irradiation.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02136859 CN1402028A (en) | 2002-09-06 | 2002-09-06 | Rare earth element doped glass double-clad optical fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02136859 CN1402028A (en) | 2002-09-06 | 2002-09-06 | Rare earth element doped glass double-clad optical fiber and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
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| CN1402028A true CN1402028A (en) | 2003-03-12 |
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|---|---|---|---|
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