CN103553319A - Method for preparing rare earth doped optical fibers by using nano self-assembly technique - Google Patents
Method for preparing rare earth doped optical fibers by using nano self-assembly technique Download PDFInfo
- Publication number
- CN103553319A CN103553319A CN201310471362.4A CN201310471362A CN103553319A CN 103553319 A CN103553319 A CN 103553319A CN 201310471362 A CN201310471362 A CN 201310471362A CN 103553319 A CN103553319 A CN 103553319A
- Authority
- CN
- China
- Prior art keywords
- rare
- rare earth
- prefabricated rods
- assembling
- silica
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01861—Means for changing or stabilising the diameter or form of tubes or rods
- C03B37/01869—Collapsing
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
The invention belongs to the technical field of optical fibers, and particularly relates to a method for preparing rare earth doped optical fibers by using a nano self-assembly technique. Rare earth ions are uniformly distributed in the optical fibers by using the nano self-assembly technique, quenching brought by uneven distribution of ions and laser efficiency reduction caused by scattering can be decreased. The rare earth ions and SiO2 can form a uniform and ordered structure in coagulation by using the nano structure self-assembly technique, so that uniform distribution of the rare earth ions in high doping concentrations can be realized, thereby facilitating preparation of high concentration doped optical fibers.
Description
Technical field
The invention belongs to optical fiber technology field, particularly a kind of method of using nanoassemble fabrication techniques rare-earth doped optical fibre.
Background technology
At present, aspect doped fiber making, the wet method doping manufacture craft of using MCVD technique making tectorium then to soak rare earths salt is widely adopted, and is the main technique means of making at present doped fiber.
Utilize MCVD method to make doped fiber process as follows: first deposited barrier layer (covering) under high temperature as ordinary optic fibre making processes first, then when deposition sandwich layer, reduce the temperature (being controlled at 1200 ℃～1400 ℃) of heating unit, the particle that is attached to inner surface of tube wall at this temperature can not form glass coating but exist to have tectorium (soot) form of vesicular structure by sintering when heating.Utilize the method for soaking rare earths salt that rare earth ion is entered in tectorium.Drying then, the processes such as dehydration are removed moisture.Under high temperature, the tectorium that soaked rare earths salt is carried out to sintering, vitrifying.Rare-earth doped optical fibre is produced in retrude rod, wire drawing, for making amplifier and laser apparatus.
The situation of the tectorium depositing in doped optical fiber prefabricated rod making processes, as granular size, homogeneity, thickness, density, adhesion strength etc., all, by having influence on distribution and the content of hotchpotch in prefabricated rods, the performance of doped fiber is had to vital effect.
Under conventional MCVD method deposition conditions, reaction product particle forms longer hangover track under airflow function, in one section of long region, is attached to silica tube inwall, and partial reaction product particle is not attached to tube wall but runs off with air-flow in addition.The track that trails when improving reactant flow in order to improve sedimentation effect will be subject to the effect of air-flow velocity increasing and lengthen, and adhering zone also lengthens thereupon.Long hangover makes to experience very long process before some reaction product particle deposition, in this process, because the interaction between air-flow and reaction product particle can cause the granular layer homogeneity variation being finally attached on tube wall, and the difference between the particulate matter of experience different tracks also obviously increases.This is particularly evident when making doped fiber low temperature depositing tectorium.
First traditional technology is to make SiO as can be seen here
2porosity and looseness layer, then by soaking rare earths salt, rare earth composition is brought in tectorium, rear-earth-doped composition is concentrated and is distributed in the hole of tectorium, and its homogeneity depends on porosity and looseness layer pattern, and tectorium pattern is very responsive wayward to temperature, the different kinds of parameters that becomes to grade; In addition, in consolidation process, because rare earth oxide fusing point is high, easily cause rare earth ion agglomerating and form crystallite etc.Want thoroughly to change this difficult problem and just must pick up from the micro nano structure of rare-earth ion-doped quartz material, the develop rapidly of Material Field nanotechnology makes the microstructure of material control effectively and become possibility.The ordered structure that is various yardsticks by nanomaterial assembly can produce more excellent overall coordination character, so we propose to adopt nanostructure package technique when cohesion, to make rare earth ion and SiO in preform manufacture
2form uniform sequential structure, thereby the rare earth ion of realizing in high-dopant concentration situation is uniformly distributed.
Summary of the invention
The object of this invention is to provide a kind of method of using nanoassemble fabrication techniques rare-earth doped optical fibre, by using Assembling of Nanoparticles to improve the distributing homogeneity of rare earth ion in preform and optical fiber.For achieving the above object, thereby forming uniform sequential structure by nanomaterial assembly in making, the prefabricated rods that the present invention is applied to doped fiber by the silica nanometer package technique in Material Field realizes rare earth ion being uniformly distributed in silica fibre.
A kind of method of using nanoassemble fabrication techniques rare-earth doped optical fibre, it utilizes Assembling of Nanoparticles that rare earth ion is uniformly distributed in optical fiber, reduce the quencher bringing because of ion distribution inequality, the lasing efficiency reduction that scattering causes, its concrete scheme has two kinds of following a, b:
A. utilize the even porous layer of nanoassemble technique construction, the method for then utilizing earth solution doping is by rare earth ion Uniform Doped in porous layer, and concrete steps are as follows:
(1) the quartzy base tube of making prefabricated rods is placed in and on lathe, carries out polishing, barrier deposition pre-treatment;
(2) adopt Assembling of Nanoparticles to build even porous silica thin film layer at the inwall of quartzy base tube;
(3) building porous microstructure can adopt online doping or off-line adulterating method that rare-earth ion solution is joined in silica tube afterwards.
(4) contracting rod, sintering form the prefabricated rods of rare-earth doped optical fibre.
B. the silica membrane layer that directly solution that contains rare earth ion and self-assembly mother solution mixing direct construction is contained to rare earth ion, concrete steps are as follows:
(1) the quartzy base tube of making prefabricated rods is placed in and on lathe, carries out polishing, barrier deposition pre-treatment;
(2) adopt Assembling of Nanoparticles to build even porous silica thin film layer at the inwall of quartzy base tube, now sneak into rare earths salt simultaneously rare earth ion is evenly distributed on to vesicular structure the inside;
(3) contracting rod, sintering form the prefabricated rods of rare-earth doped optical fibre.
Described not being doped to online taken off silica tube directly and utilized tubule pressurization to inject rare earths salt from tail end from lathe.
Described off-line is doped to silica tube is taken off, and is directly dipped in rare earths salt.
Described Assembling of Nanoparticles is mould plate technique.
When prefabricated rods is made in described step (1), use the technology of being combined with MCVD first to deposit tectorium at silica tube inwall, with the film combination that enlarge active surface is convenient to and nanometer assembling afterwards builds.
When prefabricated rods is made in described step (1), use the technology of being combined with MCVD to carry out nanometer assembling at silica tube inwall, prevent outside contamination, guarantee the purity of preform.
Described rare earth element is Er.
Beneficial effect of the present invention is:
(1) uniform doping is good.The porous layer that nanometer assemble method builds or the doped layer uniform properties of direct construction are better than the space distribution character of the tectorium of traditional MCVD method making.
(2) be not only rare earth ion, can meet all special optical fibers that can adopt infusion method to prepare.
The inventive method is by adopting nanostructure package technique to make rare earth ion and SiO when condensing
2form uniform sequential structure, thereby the rare earth ion of realizing in high-dopant concentration situation is uniformly distributed.Be conducive to the making of high-concentration dopant optical fiber.
Accompanying drawing explanation
Fig. 1 is silica tube structural representation of the present invention;
Fig. 2 is silica tube inwall deposited barrier layer structural representation of the present invention;
Fig. 3 is that the present invention utilizes nanometer assemble method to make silica membrane porous layer or doped layer structural representation at inwall;
Fig. 4 is the present invention's prefabricated rods structural representation that contracting rod completes that dewaters;
Number in the figure:
Embodiment
Embodiment 1
Choose and be of a size of 18mm * 1.5mm(external diameter * wall thickness) optical fiber level high purity quartz pipe as deposited tube, adopt MCVD method deposited barrier layer.By the pre-high purity quartz pipe two ends preshrunk that has deposited blocking layer once.Then from tail pipe end, with feeding device, adding 20～100ml concentration is online the Er of 0.1～3.0mol/l
3+ion mother solution, described Er
3+ion mother solution is by Er
3+solion adds the template aqueous solution that ionic surface active agent and mixed in hydrochloric acid are configured to add silicic acid fat to be mixed with again, and is specially tensio-active agent is added to the water, then add Er
3+ion (Er
2cl
3) solution, and be 1～4 with the pH value of hydrochloric acid control solution, stir, obtain the template aqueous solution; Wherein the concentration of tensio-active agent is 0.5～3mmol/L, in the template aqueous solution obtaining, add non-polar organic solvent or polar organic solvent, make oil-water mixture, wherein the concentration of non-polar organic solvent is 0.3～10mmol/L, and the concentration of polar organic solvent is 0.1～2mmol/L; The oil-water mixture making is added to silicon ester, and the concentration of the mixed solution mesosilicic acid ester obtaining is 2.0～10mmol/L.Add Er
3+after ion mother solution, withdraw from feeding device, start to rotate prefabricated rods 20 minutes～200 minutes, prefabricated rods is unloaded from MCVD lathe, from tail pipe end, pour out residual mother solution, again gone up the speed of rotation with 10 revs/min～100 revs/min on MCVD lathe and rotated 30 minutes～300 minutes, complete self assembling process and (make silicon-dioxide be assembled into even vesicular structure, Er
3+ion salt solution is uniformly distributed in wherein), complete doping.Then pass into high purity oxygen gas and helium in silica tube, (the two volume ratio is (1～10): the in the situation that of 1), at 100～200 ℃ of temperature, heat 30 minutes～300 minutes, get rid of water vapour and tensio-active agent residue, at the temperature of 700～1000 ℃, pass into again high-purity chlorine and helium (the two volume ratio for (1:10)～(10:1)), further processed is 20～200 minutes, finally pass into high purity oxygen gas by the silica microstructural thin layer being assembled into, at 1500～1900 ℃ of temperature, vitrifying is processed 10～60 minutes.As needs further increase thickness, can repeat above step on this layer of basis Multiple depositions until reach the thickness of demand.
Claims (9)
1. a method of using nanoassemble fabrication techniques rare-earth doped optical fibre, it is characterized in that: utilize Assembling of Nanoparticles that rare earth ion is uniformly distributed in optical fiber, reduce the quencher bringing because of ion distribution inequality, the lasing efficiency reduction that scattering causes.
2. method according to claim 1, is characterized in that, utilizes the even porous layer of nanoassemble technique construction, and the method for then utilizing earth solution doping is by rare earth ion Uniform Doped in porous layer, and concrete steps are as follows:
(1) the quartzy base tube of making prefabricated rods is placed in and on lathe, carries out polishing, barrier deposition pre-treatment;
(2) adopt Assembling of Nanoparticles to build even porous silica thin film layer at the inwall of quartzy base tube;
(3) building porous microstructure can adopt online doping or off-line adulterating method that rare-earth ion solution is joined in silica tube afterwards.
(4) contracting rod, sintering form the prefabricated rods of rare-earth doped optical fibre.
3. method according to claim 1, is characterized in that, the silica membrane layer that directly solution that contains rare earth ion and self-assembly mother solution mixing direct construction is contained to rare earth ion, and concrete steps are as follows:
(1) the quartzy base tube of making prefabricated rods is placed in and on lathe, carries out polishing, barrier deposition pre-treatment;
(2) adopt Assembling of Nanoparticles to build even porous silica thin film layer at the inwall of quartzy base tube, now sneak into rare earths salt simultaneously rare earth ion is evenly distributed on to vesicular structure the inside;
(3) contracting rod, sintering form the prefabricated rods of rare-earth doped optical fibre.
4. method according to claim 2, is characterized in that: described not being doped to online taken off silica tube directly and utilized tubule pressurization to inject rare earths salt from tail end from lathe.
5. method according to claim 2, is characterized in that: described off-line is doped to silica tube is taken off, and is directly dipped in rare earths salt.
6. it is characterized in that according to the method in claim 2 or 3: described Assembling of Nanoparticles is mould plate technique.
7. according to the method in claim 2 or 3, it is characterized in that: when prefabricated rods is made in described step (1), use the technology of being combined with MCVD first to deposit tectorium at silica tube inwall, with the film combination that enlarge active surface is convenient to and nanometer assembling afterwards builds.
8. according to the method in claim 2 or 3, it is characterized in that: when prefabricated rods is made in described step (1), use the technology of being combined with MCVD to carry out nanometer assembling at silica tube inwall, prevent outside contamination, guarantee the purity of preform.
9. it is characterized in that according to the method in claim 2 or 3: described rare earth element is Er.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310471362.4A CN103553319B (en) | 2013-10-10 | 2013-10-10 | A kind of method that uses nanoassemble fabrication techniques rare-earth doped optical fibre |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310471362.4A CN103553319B (en) | 2013-10-10 | 2013-10-10 | A kind of method that uses nanoassemble fabrication techniques rare-earth doped optical fibre |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103553319A true CN103553319A (en) | 2014-02-05 |
| CN103553319B CN103553319B (en) | 2016-05-11 |
Family
ID=50007740
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310471362.4A Expired - Fee Related CN103553319B (en) | 2013-10-10 | 2013-10-10 | A kind of method that uses nanoassemble fabrication techniques rare-earth doped optical fibre |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103553319B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0520402A2 (en) * | 1991-06-24 | 1992-12-30 | Sumitomo Electric Industries, Ltd | Method for producing glass preform for optical fiber |
| US20040031290A1 (en) * | 2002-08-16 | 2004-02-19 | Fitel Usa Corp. | High-temperature sintering of soot bodies doped using molecular stuffing |
| CN1511785A (en) * | 2002-12-30 | 2004-07-14 | 新加坡纳米材料科技有限公司 | Silicon dioxide mesoporous material and its preparing method |
| CN101033113A (en) * | 2007-04-05 | 2007-09-12 | 复旦大学 | Process of preparing rare earth ion doped optical fiber prefabricated rod |
| CN102515500A (en) * | 2011-12-06 | 2012-06-27 | 长飞光纤光缆有限公司 | Preparation method for rare earth doped optical fiber preform |
-
2013
- 2013-10-10 CN CN201310471362.4A patent/CN103553319B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0520402A2 (en) * | 1991-06-24 | 1992-12-30 | Sumitomo Electric Industries, Ltd | Method for producing glass preform for optical fiber |
| US20040031290A1 (en) * | 2002-08-16 | 2004-02-19 | Fitel Usa Corp. | High-temperature sintering of soot bodies doped using molecular stuffing |
| CN1511785A (en) * | 2002-12-30 | 2004-07-14 | 新加坡纳米材料科技有限公司 | Silicon dioxide mesoporous material and its preparing method |
| CN101033113A (en) * | 2007-04-05 | 2007-09-12 | 复旦大学 | Process of preparing rare earth ion doped optical fiber prefabricated rod |
| CN102515500A (en) * | 2011-12-06 | 2012-06-27 | 长飞光纤光缆有限公司 | Preparation method for rare earth doped optical fiber preform |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103553319B (en) | 2016-05-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103360019B (en) | The preparation method of the silicon dioxide silica aerogel composite material that silicon carbide fiber felt strengthens | |
| Liu et al. | Robust and antireflective superhydrophobic surfaces prepared by CVD of cured polydimethylsiloxane with candle soot as a template | |
| Larbot et al. | Silica membranes by the sol-gel process | |
| CN105541104B (en) | High power mixes the preparation method of Yb silica fibres and preform | |
| JP3527707B2 (en) | Optical fiber preform having OH blocking layer and method for manufacturing the same | |
| CN102515500B (en) | Preparation method for rare earth doped optical fiber preform | |
| JPH0753232A (en) | Method for doping of optical fiber | |
| CN100503494C (en) | Process of making rare earth doped optical fibre | |
| US5151117A (en) | Solution doping of porous preforms | |
| EP2470472B1 (en) | Composite materials containing aligned nanotubes and the production thereof | |
| CN103992030A (en) | Preparation method for rare earth doped optical fiber prefabricated bar | |
| JPS61155225A (en) | Manufacture of optical wave guide tube | |
| CN105837025A (en) | Method for efficiently preparing optical fiber doped preform rod and optical fiber doped preform rod | |
| CN104932054B (en) | A kind of triple clad thulium doped fiber and preparation method thereof | |
| CN104876434B (en) | A kind of preparation method of Uniform Doped quartz glass bar | |
| CN113800774A (en) | Erbium-doped glass optical fiber used as gain medium and application thereof in optical fiber laser | |
| CN106986552B (en) | Method for manufacturing high-temperature-resistant quartz glass | |
| CN111574046A (en) | Gas-liquid phase composite doping method for preparing rare earth doped optical fiber | |
| CN103553319A (en) | Method for preparing rare earth doped optical fibers by using nano self-assembly technique | |
| CN117209134A (en) | Quartz deposition tube, rare earth doped optical fiber preform and preparation method of optical fiber | |
| CN109293249A (en) | The preparation method of preform and optical fiber | |
| JP2000191336A (en) | Production of optical fiber preform and production of optical fiber | |
| CN109856720B (en) | Preparation method of magneto-optical fiber with high Verdet constant | |
| JP2009078928A (en) | Optical fiber preform, method for producing the same and rare earth-added optical fiber | |
| CN105884201A (en) | Yb-doped quartz optical fiber capable of bearing high power and preparation method of quartz optical fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160511 Termination date: 20201010 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |