CN100573733C - Field optical fibre probe and preparation method thereof - Google Patents
Field optical fibre probe and preparation method thereof Download PDFInfo
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- CN100573733C CN100573733C CNB2006100587143A CN200610058714A CN100573733C CN 100573733 C CN100573733 C CN 100573733C CN B2006100587143 A CNB2006100587143 A CN B2006100587143A CN 200610058714 A CN200610058714 A CN 200610058714A CN 100573733 C CN100573733 C CN 100573733C
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Abstract
A kind of elder generation carries out pre-service to optical fiber and corrodes the method for preparing field optical fibre probe with HF acid again.In preprocessing process, the method of at first utilizing HF acid corrosion or heating to draw is processed optical fiber, make it form certain cone angle and point diameter reduces, utilize the plastic solution of organic solvent dissolution plastics gained again or the molten plastic that plastics heat gained is wrapped in optical fiber to have on the part of cone angle, form plastic foil at optical fiber surface after waiting the solvent evaporates of plastic solution or molten plastic cooled and solidified at last; In the corrosion preparation process, will insert in the HF acid that has the oil guard layer through pretreated optical fiber and corrode, utilize corrosion of the organic solvent dissolution or the concentrated sulphuric acid or mechanical means to remove the optical fiber surface plastic foil after etching and can obtain probe.This method has realized the corrosion of (less than the ordinary optic fibre diameter) in the small scale scope for the first time, and the prepared probe tip diameter that goes out is little, and smooth surface, cone angle is big and shape is determined.
Description
Technical field
The invention belongs to the preparing technical field of optical precision instrument core component, relate to a kind of method for preparing field optical fibre probe, especially a kind ofly optical fiber is carried out pre-service earlier corrode the method for preparing the high-quality field optical fibre probe again.
Background technology
Optical microscope for scanning near field (SNOM or NOSM) is increasingly extensive in the application in fields such as physics, chemistry, material science, life science, geology and information industry as a kind of important optical instrument.It is mainly used in the exterior appearance and the optical property of observing and studying object on nanometer and the meso-scale as the newcomer in the scanning probe microscopy family, and wherein utilizing SNOM that low-dimensional Jie sight system under the nanoscale is carried out spectral investigation is one of important application of SNOM.The collection efficiency that how to improve the near field optic information on sample surface effectively is to improve the major issue of SNOM.Therefore, how improving the core component of SNOM---the preparation technology of near field probe, realization can repeat to prepare in a large number the probe that tip diameter is little, shape is determined, light collection efficiency is high becomes a key factor that influences the SNOM widespread use.
At present, utilize in the method that chemical corrosion method prepares field optical fibre probe numerous, Turner method the earliest is bare fibre directly to be inserted in the HF acid corrode, and its device is simple, but probe shape is subject to the influence of external disturbance, causes rough; Dynamically etch is utilizing the relatively moving corrosion between bare fibre and the HF acid solution face to prepare needle point on the basis of Turner method, this square law device complexity, and the prepared same rough surface of probe that goes out, rough, and tip diameter is inadequately little; The Tube etching method that last century Mo proposes; its key step is that optical fiber is inserted in the HF acid together with its plastic protective layer; utilize optical fiber side direction HF acid permeating corrosion and optical fiber bottom HF acid convection current corrosion preparation needle point, treat to utilize again after needle point forms concentrated sulphuric acid corrosion or machinery to remove plastic protective layer and obtain optical fiber probe.Though utilize the prepared probe smooth surface that goes out of Tube etching method, owing to be to corrode in the optic fibre plastics protective seam, the corrosion scope is bigger, therefore resulting probe tip diameter is big and shape is uncertain.
Summary of the invention
At the problems referred to above, the purpose of this invention is to provide a kind of brand-new preparation high-quality field optical fibre probe and preparation method thereof, described method is carried out pre-service to optical fiber earlier to be made its formation cone angle and the fibre diameter of cone angle fore-end is reduced, and then corrode, realized for the first time the corrosion of (less than the ordinary optic fibre diameter) in the small scale scope, the prepared probe tip diameter that goes out is little, and smooth surface, cone angle is big and shape is determined.
According to purpose of the present invention, the method for preparing field optical fibre probe comprises pre-service and two processes of corrosion preparation:
Described preprocessing process comprises step:
(1) method of utilizing hydrofluorite (HF) corrosion or heating to draw is processed an end of optical fiber, its fibre diameter that forms cone angle and cone angle end portion is reduced, as shown in Figure 1;
Wherein, used optical fiber can be the single mode or the multimode optical fiber of various models, and its external diameter can be the optical fiber of 80 microns, 125 microns, 140 microns, 200 microns and other all size.
Wherein, employed HF acid concentration can be regulated between 20% to 55%.The height of HF acid concentration influences corrosion speed, and the HF acid concentration is big more, corrodes fast more.Under the room temperature, 20% HF acid corrosion speed is 1.3 microns/minute, and 40% HF acid corrosion speed is 1.9 microns/minute.Under certain corrosion speed,, can make the scope of the fibre diameter of cone angle front end be reduced to 5 to 70 micrometer ranges by the control etching time.For example 24 ℃ the time, 40%HF acid corrosion speed is 1.7 microns/minute, corrodes after 32 minutes, and the fibre diameter of cone angle front end is reduced to 70 microns; Corrode after 70.5 minutes, the fibre diameter of cone angle front end is reduced to 5 microns.
Wherein, described heating draws can adopt various type of heating well known in the prior art, includes but not limited to burning heating and LASER HEATING.Heat time heating time is long more, heating intensity is big more, and then the fibre diameter of cone angle front end is more little.
Wherein, the fibre diameter of cone angle front end reduce the cone angle size that degree influences last gained probe, the fibre diameter of cone angle front end reduces more for a short time, last gained probe cone angle is more little.For example, when the fibre diameter of cone angle front end was reduced to 5 microns, last gained probe cone angle was about 30 °; When the fibre diameter of cone angle front end was reduced to 25 microns, last gained probe cone angle was about 90 °.
(2) utilize the plastic solution of organic solvent dissolution plastics gained or the molten plastic that plastics heat gained is wrapped in the treated end of optical fiber, include but not limited to have the part of cone angle.Cone angle partly need be wrapped fully, and whether the part beyond the cone angle is wrapped Corrosion results is had no significant effect.Form plastic foil Deng after the solvent evaporates of plastic solution or the molten plastic cooled and solidified at optical fiber surface, its effect is the convection current corrosion cavity that forms among a small circle.
Wherein, the organic solvent that is used to dissolve plastics is the organism that can dissolve plastics, preferably can be chloroform or methylene chloride or tetrahydrofuran.The described mode that plastics are heated can adopt various type of heating well known in the prior art, includes but not limited to burning heating and LASER HEATING.
Wherein, described plastics can be any organic plastics that dissolve in, as long as its fusing point is lower than optical fiber and can forms overlay film at optical fiber surface.The plastic foil that is covered on the optical fiber is preferably more than 0.5 millimeter for good so that uniform and smooth and thickness is enough thick, permeates with effective preventions HF acid.
The corrosion preparation process comprises step:
(3) will insert in the 20%～55%HF acid that has the oil guard layer through pretreated optical fiber and corrode;
The variation of used HF acid concentration and when corrosion environment temperature variation only influence the required time that etches, the last prepared optical fiber probe shape that goes out is had no significant effect.Under the room temperature, concentration is that the required etching time of 20% HF acid is about 150 minutes, and concentration is that 50% the required etching time of HF acid is about 60 minutes.Corrosion temperature is also influential to corroding the required time: utilize concentration 40%HF acid, required etching time is about 2 hours in the time of 20 ℃; Required etching time is about 50 minutes in the time of 40 ℃.Be covered with one deck oil guard layer on the used HF acid solution face, the used oil material can be a density less than HF acid and water-fast organism, this oil substances must be not with the material of optical fiber and top institute coating plastic film generation chemical reaction thereof.The purpose of using this oil guard layer is to avoid the sour volatilization of HF and influence corrosion process.
Should be noted that, in this step, the degree of depth that optical fiber inserts HF acid can not surpass the scope that plastic foil covers, promptly, the part that optical fiber contacts with HF acid solution face must have plastic foil to cover, and can guarantee so only to corroding through pretreated optical fiber by the plastic film wrapped part.If it is shallow or dark excessively that optical fiber insertion HF acid solution face is crossed, the part that causes contacting with HF acid solution face is a bare fibre, and is then similar with Turner method of the prior art.
(4) after needle point formed in the corrosion process, corrosion can finish, and removed the optical fiber surface plastic foil and can obtain probe.
The concrete means of removing plastic foil can be to utilize organic solvent dissolution or concentrated sulphuric acid corrosion or mechanical curettage method.
In sum, utilize method provided by the invention, as long as regulate degree and parameters such as the optical fiber insertion depth in the corrosion process, etching time that the fibre diameter of cone angle front end in the preprocessing process reduces, can realize the preparation of industrialization of high-quality field optical fibre probe.Compared with prior art, method of the present invention has following advantage:
(1) preparation method is simple, implements easily, need not complicated precision apparatus, as long as before utilizing HF acid corrosion optical fiber optical fiber is carried out pre-service.
(2) probe mass of utilizing method of the present invention to prepare is stable, and the repeatability height can prepare in a large number, realizes suitability for industrialized production.
(3) reduce degree by optical fiber cone angle point diameter after regulating pre-service, can prepare the probe of different cone angle, to satisfy needs of different applications.
Advantages such as (4) probe that utilizes method of the present invention to prepare has simultaneously that shape is determined, tip diameter is little, smooth surface and cone angle are big and controlled, pattern behind its plated film and optical resolution height, logical optical efficiency height meets the technical requirement of high-quality field optical fibre probe fully.
Description of drawings
Fig. 1 is preparation technology's schematic flow sheet of a preferred embodiment of the present invention;
Fig. 2 is the scanning electron microscope image (enlargement factor is 90000 times) of the field optical fibre probe among the embodiment 1;
Fig. 3 is the scanning electron microscope image (enlargement factor is 100000 times) of the field optical fibre probe among the embodiment 2;
Fig. 4 is the scanning electron microscope image (enlargement factor is 120000 times) of the field optical fibre probe among the embodiment 3;
Among the figure, identical label is represented identical parts:
Optical fiber 7-optical fiber probe after bare fibre 3-plastic foil 4-isooctane protective seam 5-40%HF acid 6-preparation after the 1-bare fibre 2-pre-service corrosion etches
Embodiment
Embodiment 1:
As shown in Figure 1, the probe preparation technology flow process of present embodiment mainly was divided into for four steps:
The first step: with the bare fibre 1 usefulness concentration of having removed plastic protective layer in several cm range of end is 40% the HF acid corrosion 58 minutes that at room temperature (is 24 ℃ herein), obtains having certain cone angle, end diameter is the bare fibre 2 after 7 microns the pre-service corrosion;
Second step: will utilize the plastic solution of organic solvent chloroform dissolving plastics gained to be wrapped in the cone angle and the exposed part that links to each other with cone angle of optical fiber, and treat that the chloroform volatilization will then form uniform plastic foil 3 at optical fiber surface;
More than two the step belong to the preprocessing process before the fiber optical corrosive.
The 3rd step: will insert in the liquid level that the concentration that have isooctane protective seam 4 is 40% HF acid 5 through pretreated optical fiber and corrode, and corrode and at room temperature (be 24 ℃ herein) and carry out that etching time is 80 minutes;
The 4th step: the optical fiber 7 after will etching takes out, and with chloroform the plastic foil dissolving on surface is removed.
Through after above four steps, just prepared required field optical fibre probe 8, its scanning electron microscope image is as shown in Figure 2.As can be seen from the figure, the tip diameter of this probe is little, about 30nm; Smooth surface; Cone angle is bigger, about 37 °.
Embodiment 2:
In present embodiment and the following examples 3, probe preparation technology flow process is identical with embodiment 1, and different is has changed corrosion parameter and fibre diameter reduces degree, thereby changes the last prepared probe shape that goes out.
The first step: with the bare fibre 1 usefulness concentration of having removed plastic protective layer in several cm range of end is 30% the HF acid corrosion 73 minutes that at room temperature (is 24 ℃ herein), obtains having certain cone angle, end diameter is the bare fibre 2 after 16 microns the pre-service corrosion;
Second step: will utilize organic solvent dichloromethane dissolving plastics (to be polymethylmethacrylate herein, abbreviating PMMA as) the PMMA solution of gained is wrapped in the cone angle and the exposed part that links to each other with cone angle of optical fiber, treats that methylene chloride volatilization back forms uniform PMMA film 3 at optical fiber surface;
The 3rd step: will insert in the liquid level that the concentration that have isooctane protective seam 4 is 30% HF acid 5 through pretreated optical fiber and corrode, and corrode and at room temperature (be 24 ℃ herein) and carry out that etching time is 110 minutes;
The 4th step: the optical fiber 7 after will etching takes out, and with methylene chloride the PMMA film dissolving on surface is removed.Through after above four steps, just prepared required field optical fibre probe 8, its scanning electron microscope image is as shown in Figure 3.As can be seen from the figure, the tip diameter of this probe is little, about 20nm; Smooth surface; Cone angle is bigger, about 54 °.The prepared probe cone angle that goes out is bigger than the probe cone angle among the embodiment one in the present embodiment, is because optical fiber is reduced to 16 microns through diameter after the pre-service in the present embodiment, and is bigger than 7 microns among the embodiment one.
Embodiment 3:
The first step: with the bare fibre 1 usefulness concentration of having removed plastic protective layer in several cm range of end is 20% the HF acid corrosion 77 minutes that at room temperature (is 24 ℃ herein), obtains having certain cone angle, end diameter is the bare fibre 2 after 25 microns the pre-service corrosion;
Second step: will utilize the plastic solution of organic solvent tetrahydrofuran dissolving plastics (being poly-methyl carbonate herein) gained to be wrapped in the cone angle and the exposed part that links to each other with cone angle of optical fiber, and treat that tetrahydrofuran volatilization back will form uniform plastic foil 3 at optical fiber surface;
The 3rd step: will insert in the liquid level that the concentration that have isooctane protective seam 4 is 20% HF acid 5 through pretreated optical fiber and corrode, and corrode and at room temperature (be 24 ℃ herein) and carry out that etching time is 150 minutes;
The 4th step: the optical fiber 7 after will etching takes out, and with tetrahydrofuran the plastic foil dissolving on surface is removed.
Through after above four steps, just prepared required field optical fibre probe 8, its scanning electron microscope image is as shown in Figure 4.As can be seen from the figure, the tip diameter of this probe is little, about 25nm; Smooth surface; Cone angle is bigger, about 90 °.Fibre diameter reduces lessly (being 25 microns after reducing) herein in the present embodiment preprocessing process, so gained probe cone angle is also correspondingly bigger.This probe has possessed simultaneously that cone angle is big, tip diameter is little and show advantages such as smooth, is a kind of high-quality probe.
Claims (6)
1, a kind of method for preparing optical fiber probe comprises step:
(1) optical fiber is an exposed end corrodes with hydrofluorite, makes its fibre diameter that forms cone angle and cone angle front end be reduced to predetermined value;
(2) utilize the plastic solution of organic solvent dissolution plastics gained or the molten plastic that plastics heat gained is wrapped in described cone angle part, form plastic foil at optical fiber surface after waiting the solvent evaporates of plastic solution or molten plastic cooled and solidified;
(3) part that optical fiber is covered with plastic foil is inserted in the hydrofluorite have the oil guard layer and is corroded, and wherein the optical fiber degree of depth of inserting hydrofluorite is no more than the scope that plastic foil covers;
(4) treat that needle point forms after, corrosion finishes, the plastic foil of removing optical fiber surface obtains probe.
2, the method for claim 1 is characterized in that, the concentration of described hydrofluorite is 20%～55%.
3, the method for claim 1 is characterized in that, described organic solvent is chloroform or methylene chloride or tetrahydrofuran.
4, the method for claim 1 is characterized in that, the thickness of described plastic foil is at least 0.5 millimeter.
5, the method for claim 1 is characterized in that, described oil guard layer be density less than hydrofluorite and water-fast organism, its not with optical fiber and the top plastic foil generation chemical reaction that covers thereof.
6, method as claimed in claim 5 is characterized in that, described oil guard layer is an isooctane.
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| CNB2006100587143A CN100573733C (en) | 2006-03-03 | 2006-03-03 | Field optical fibre probe and preparation method thereof |
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| CNB2006100587143A CN100573733C (en) | 2006-03-03 | 2006-03-03 | Field optical fibre probe and preparation method thereof |
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| CN101602183B (en) * | 2009-06-26 | 2011-02-16 | 北京航空航天大学 | Grinding device for preparing near-field optical probes and method therefor |
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| CN104101737A (en) * | 2014-07-11 | 2014-10-15 | 华中科技大学 | Manufacture method of optical fiber probe |
| CN105806284A (en) * | 2016-05-12 | 2016-07-27 | 四川大学 | Microprobe machining and forming system and method |
| CN106290989B (en) * | 2016-07-25 | 2019-04-12 | 四川理工学院 | A kind of atomic force microscope probe tip modification method |
| CN106291813A (en) * | 2016-09-07 | 2017-01-04 | 中国科学院半导体研究所 | Many measuring points transparent optical electrode based on optical fiber |
| CN109212667A (en) * | 2018-08-29 | 2019-01-15 | 武汉理工大学 | The optical fiber optical tweezers probe with secondary cone angle prepared with two step method |
| CN109702660B (en) * | 2019-01-09 | 2020-11-06 | 南京航空航天大学 | Superhard abrasive material flexible tool for precisely machining micro-holes and manufacturing method thereof |
| CN111141221B (en) * | 2019-12-16 | 2021-03-23 | 西安交通大学 | Preparation method of optical fiber probe for micro-displacement sensor, micro-displacement sensor and application |
| CN111879251B (en) * | 2020-06-22 | 2021-07-13 | 西安交通大学 | Building component bending deformation detection sensor and preparation method thereof |
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| CN113311110A (en) * | 2021-05-18 | 2021-08-27 | 北极光电(深圳)有限公司 | Optical fiber chemical corrosion method |
| CN113390790A (en) * | 2021-05-24 | 2021-09-14 | 西安交通大学 | Optical fiber nano probe with large length-diameter ratio and preparation method and application thereof |
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|---|---|---|---|---|
| US4469554A (en) * | 1983-04-05 | 1984-09-04 | At&T Bell Laboratories | Etch procedure for optical fibers |
Non-Patent Citations (4)
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