CN102995118A - Method for preparing D type optical fiber colloidal crystal micro-nano structure - Google Patents
Method for preparing D type optical fiber colloidal crystal micro-nano structure Download PDFInfo
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- CN102995118A CN102995118A CN2012105129698A CN201210512969A CN102995118A CN 102995118 A CN102995118 A CN 102995118A CN 2012105129698 A CN2012105129698 A CN 2012105129698A CN 201210512969 A CN201210512969 A CN 201210512969A CN 102995118 A CN102995118 A CN 102995118A
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Abstract
A method for preparing D type optical fiber colloidal crystal micro-nano structure relates to the field of photoelectronic technique. The method comprises the following steps of firstly preparing micro-nano structure on a plane of D type optical fiber, then preparing colloidal crystal in the micro-nano structure by utilizing colloidal particles, wherein the specific processes comprise gluing, exposure, etching, degumming and assembling the colloidal particles into the micro-nano structure through the combination of the action of static electri field and lifting. According to the method, the colloidal crystal micro-nano structure is prepared on the D type optical fiber plane finally, therefore, a evanescent field of the D type optical fiber is regulated by both micro-nano structure and photonic band gap of the colloidal crystal, and in the D type optical fiber, the optical field is stronger, and the regulation is controllable, so that the D type optical fiber can be widely used in field such as optical information processing, optical sense, optical integration, and the like.
Description
Technical field
The present invention relates to the photoelectron technology field, be specifically related to a kind of preparation method of D shape optical fiber colloidal crystal micro-nano structure.
Background technology
The refractive index cycle modulated structure more and more is subject to the attention of optical communication and sensory field in recent years.They can form Prague forbidden band relevant with period of change, play reflex action in the transmission course of light wave.Be in the three-dimensional dielectric materials of periodic arrangement at dielectric coefficient, hertzian wave is after the dielectric function scattering, the electromagnetic intensity of some wave band can be exponential attenuation because of destruction interference, can't in system, transmit, be equivalent to form energy gap at frequency spectrum, so dispersion relation also has zonal structure, this is so-called photonic band structures (photonic band structures).Dielectric material with photonic band structures just is called photonic band-gap system (photonic band-gap system is called for short the PBG system), or is called for short photonic crystal (photonic crystals).Layered periodic structure just is being based on that the concept development of photonic crystal gets up, and the research that colloidal crystal also just is being based on photonic crystal has obtained widely research and development.
The micro-nano structure of fabrication cycle has multiple use on optical fiber, for example utilizes the variations in refractive index of evanescent field testing environment medium, thereby monitors the character such as its chemical concentrations and pH value.For evanescent field intensity is increased, the covering of ordinary optic fibre is corroded, reduce the thickness of covering, perhaps optical fiber is ground, wherein simultaneously polishing of covering become D shape plane, optical fiber will have more energy leakage in external environment like this, stronger evanescent field occur, make the change of surrounding medium can directly have influence on the variation of each parameter of light field.A kind of like this ordinary optic fibre is ground, just be called D shape optical fiber thereby change the special optical fiber that its shape of cross section and structure change the basic mode transport property.
Because colloidal crystal has good periodic structure, and be distributed in three dimensions and have a photon band gap, colloidal crystal can interact with D shape optical fiber plane evanescent field on the D shape optical fiber, makes at the light of inside of optical fibre transmission to be modulated, and then realizes the functions such as light sensing, light regulation and control.And can be directly and the ordinary optic fibre welding with the D shape optical fiber of colloidal crystal, realize full optical fibre device, and do not need corresponding body block part.But yet there are no report about glue body crystal micro-nano structure on D shape optical fiber at present, because of the optical fiber volume little, and the photon band gap of the colloidal crystal for preparing is positioned at communication band, the particle that needs is larger, therefore needs more accurate technique and method at optical fiber preparation colloidal crystal micro-nano structure.
Summary of the invention
Purpose of the present invention just provides a kind of preparation method of D shape optical fiber colloidal crystal micro-nano structure, namely first prepare micro-nano structure at D shape optical fiber, and then utilize colloidal particle in micro-nano structure, to prepare colloidal crystal, to realize modulation stronger to light field in the D shape optical fiber and that can control, widen the range of application of D shape optical fiber.
For reaching above-mentioned purpose, technical scheme of the present invention is: a kind of preparation method of D shape optical fiber colloidal crystal micro-nano structure comprises the steps:
(1), be fixed on the base plate with the circular face of silica gel with D shape optical fiber, coat photoresist material on D shape optical fiber plane, then oven dry;
(2), D shape optical fiber and the required mask plate that will scribble photoresist material be contained on the lithography machine, exposed in D shape optical fiber plane, then with D shape optical fiber 30-60 ℃ of lower heating 3-5 minute, develop with acetone afterwards and remove the photoresist material of exposed portion;
(3), under the agitation condition, with HF acid buffered soln etching D shape optical fiber plane, realize the preparation of micro-nano structure on the D shape optical fiber plane, etching temperature 30-50 ℃, time 3-10 minute;
(4), with KOH solution flush away D shape optical fiber plane remaining photoresist material, then with deionized water ultrasonic cleaning D shape optical fiber and dry;
(5), preparation colloidal particle suspension liquid, volumetric concentration is 2-5%, then ultrasonic concussion is evenly distributed colloidal particle;
(6), the end with the D shape optical fiber of micro-nano structure that step (4) is made is fixed on the stepper-motor, D shape optical fiber rest part is inserted in the colloidal particle suspension liquid, it is the electrostatic field of 600-1300V/m that whole device places strength of electric field, keeping the temperature of colloidal particle suspension liquid is 40-60 ℃, then stepper-motor lifts D shape optical fiber with the speed of 0.5-2mm/min, until D shape optical fiber breaks away from suspension liquid, can in the micro-nano structure on D shape optical fiber plane, make colloidal crystal.
Described HF acid buffered soln is HF, the NH of 1:1:8 by mass ratio
4F and H
2O forms.
Colloidal particle in the described colloidal particle suspension liquid are PS, PMMA or SiO
2In a kind of.
Beneficial effect: the present invention adopts first photoetching technique required micro-nano structure of etching on D shape optical fiber plane, then take micro-nano structure as template, utilize the colloidal crystal self-assembling technique that colloidal particle are assembled in the micro-nano structure, finally prepared the colloidal crystal micro-nano structure at D shape optical fiber, this D shape optical fiber with the colloidal crystal micro-nano structure can make the evanescent field of optical fiber accept simultaneously the modulation of micro-nano structure and colloidal crystal photon band gap, micro-nano structure has formed the period profile of specific refractory power, and colloidal crystal can form the three-dimensional refractive index distributed architecture, the wavelength of evanescent field and the dual modulation of intensity have been accomplished simultaneously, can be widely used in optical information processing, the field such as optical sensing and optics are integrated.
Adopt photoetching technique, by the mask plate that adopts in the control process and the temperature and time of etching, can realize the preparation of the micro-nano structure of multiple figure and size on the D shape optical fiber, make the micro-nano structure grating than existing with phase masks and point-to-point writing method, its cost will be low many, easy and simple to handle and efficient is high.
Colloidal crystal self assembling process of the present invention adopts electrostatic field to stretch the method that combines with lifting, utilize the settling velocity of electrostatic field control colloidal particle in the process by controlling suitable technical parameter, thickness and the number of plies of pull rate control colloidal crystal, the final colloidal crystal that in the micro-nano structure of D shape optical fiber, has prepared different thickness and the number of plies, so that the centre wavelength of the photon band gap of the colloidal crystal that forms is controlled, thereby can control the interaction with D shape fiber evanescent field, namely control percentage coupling and efficient between evanescent field and colloidal crystal, form the purpose control of D shape fiber evanescent field, the practicality of evanescent field in sensing and measurement strengthened greatly.
The present invention is at D shape optical fiber preparation colloidal crystal micro-nano structure, because D shape plane only is the 7-15 micron from the distance at sandwich layer center, 1/8th to 1/20th (standard single-mode fiber cladding diameter representative value is 125um) of standard single-mode fiber cladding diameter, the micro-nano structure on D shape plane from sandwich layer very close to, the interaction of the interior colloidal crystal of micro-nano structure and D shape optical fiber plane evanescent field is strengthened, make in the optical modulation effect of sandwich layer internal transmission and strengthen, and then strengthen the functions such as light sensing, light regulation and control.
Description of drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the micro-nano structure on the D shape optical fiber plane after the etching among the embodiment 2.
Fig. 2 is the scanning electron microscope (SEM) photograph of the colloidal crystal in the D shape optical fiber plane micro-nano structure that makes among the embodiment 2.
Fig. 3 is the transmitted light spectrogram with the D shape optical fiber of colloidal crystal micro-nano structure that makes among the embodiment 2.
Fig. 4 is the scanning electron microscope (SEM) photograph of the micro-nano structure on the D shape optical fiber plane after the etching among the embodiment 3.
Fig. 5 is the reflected light spectrogram with the D shape optical fiber of three kinds of different size colloidal crystal micro-nano structures that makes among the embodiment 3.
Embodiment
A kind of preparation method of D shape optical fiber colloidal crystal micro-nano structure comprises the steps:
(1), be fixed on the base plate with the circular face of silica gel with D shape optical fiber, coat photoresist material on D shape optical fiber plane, then oven dry;
(2), D shape optical fiber and the required mask plate that will scribble photoresist material be contained on the lithography machine, exposed in D shape optical fiber plane, then with D shape optical fiber 30-60 ℃ of lower heating 3-5 minute, develop with acetone afterwards and remove the photoresist material of exposed portion;
(3), under the agitation condition, with HF acid buffered soln etching D shape optical fiber plane, realize the preparation of micro-nano structure on the D shape optical fiber plane, etching temperature 30-50 ℃, time 3-10 minute;
(4), with KOH solution flush away D shape optical fiber plane remaining photoresist material, then with deionized water ultrasonic cleaning D shape optical fiber and dry;
(5), preparation colloidal particle suspension liquid, volumetric concentration is 2-5%, then ultrasonic concussion is evenly distributed colloidal particle;
(6), the end with the D shape optical fiber of micro-nano structure that step (4) is made is fixed on the stepper-motor, D shape optical fiber rest part is inserted in the colloidal particle suspension liquid, it is the electrostatic field of 600-1300V/m that whole device places strength of electric field, keeping the temperature of colloidal particle suspension liquid is 40-60 ℃, then stepper-motor lifts D shape optical fiber with the speed of 0.5-2mm/min, until D shape optical fiber breaks away from suspension liquid, can in the micro-nano structure on D shape optical fiber plane, make colloidal crystal.
Described HF acid buffered soln is HF, the NH of 1:1:8 by mass ratio
4F and H
2O forms.
Colloidal particle in the described colloidal particle suspension liquid are PS, PMMA or SiO
2In a kind of.
Embodiment 1
Be fixed on the base plate with the circular face of silica gel with D shape optical fiber, coat photoresist material AZ-1350 on D shape optical fiber plane, then oven dry, D shape optical fiber and the mask plate that carries required pattern be contained in carry out exposure-processed on the lithography machine, exposure position is the central position on D shape optical fiber plane, the pattern that mask plate carries be one unimodal, wide 5 microns, long 30 microns, length direction is perpendicular to the fiber core direction, the exposure purpose is the photoresist material generation photochmeical reaction that makes photosensitive area, and molten change occurs when next step development; On drying machine optical fiber was heated 5 minutes after the exposure, 40 ℃ of temperature are immersed in D shape optical fiber afterwards in the acetone and develop to remove the photoresist material of exposed portion, have realized the design transfer on the mask plate to the photoresist material on D shape optical fiber plane; Then, D shape optical fiber is immersed in the HF acid buffered soln in the stirring, with the D shape optical fiber plane of etching exposed portion, etching temperature is 40 ℃, and 10 minutes time, HF acid buffered soln is HF, the NH of 1:1:8 by mass ratio
4F and H
2O forms, and has so just obtained the micro-nano structure identical with pattern on the mask plate on D shape optical fiber plane, then uses the remaining photoresist material in KOH solution flush away D shape optical fiber plane, again with deionized water ultrasonic cleaning D shape optical fiber and dry.
Take water as solvent, the preparation diameter is the SiO of 710nm
2Colloidal particle suspension liquid, volumetric concentration are 5%, and then ultrasonic concussion is 5 minutes.End with the D shape optical fiber of micro-nano structure that then will make is fixed on the stepper-motor, and D shape optical fiber rest part is inserted in SiO
2In the colloidal particle suspension liquid, it is the electrostatic field of 1000V/m that whole device places strength of electric field, keeps SiO
2The temperature of colloidal particle suspension liquid is 50 ℃, and then stepper-motor outwards lifts D shape optical fiber with the speed of 1mm/min, breaks away from suspension liquid through about 30 minutes D shape optical fiber, can make SiO in the micro-nano structure on D shape optical fiber plane
2Colloidal crystal.
In the process, with the micro-nano structure on the D shape optical fiber plane after the S-4800 scanning electron microscopic observation etching, it is a strip groove, and its degree of depth is about 2-5 micron, wide 5 microns, long 30 microns.Fixing at the micro-nano structure pattern that D shape optical fiber prepares, what pattern of needs preparation is just used the mask with corresponding pattern, and mask can customize.
With the colloidal crystal in the scanning electron microscopic observation micro-nano structure, the structure of colloidal crystal according to the degree of depth of micro-nano structure, can estimate that colloidal crystal thickness is about the 2-5 micron take face-centred cubic structure as main, and the number of plies is about the 3-8 layer.
With the AQ6378 spectrum analyzer the prepared D shape optical fiber with the colloidal crystal micro-nano structure is carried out spectrum test, from the transmitted light spectrogram that obtains, can obviously find out the photon band gap of colloidal crystal, and can see through the wavelength of evanescent field and produce effectively selective action, according to 710nm SiO
2The Theoretical Calculation of the photon band gap of colloidal crystal is 1551nm, conforms to our test result.
Embodiment 2
Be fixed on the base plate with the circular face of silica gel with D shape optical fiber, coat photoresist material UV-258 on D shape optical fiber plane, then oven dry, D shape optical fiber and the mask plate that carries required pattern be contained in carry out exposure-processed on the lithography machine, exposure position is the central position on D shape optical fiber plane, the pattern that mask plate carries is unimodal, wide 5 microns, long 100 microns, length direction is parallel to the fiber core direction, the exposure purpose is the photoresist material generation photochmeical reaction that makes photosensitive area, and molten change occurs when next step development; On drying machine, optical fiber was heated 3 minutes after the exposure, 30 ℃ of temperature, D shape optical fiber is immersed in develops in the acetone afterwards removes the photoresist material of exposed portion, has realized the design transfer on the mask plate to the photoresist material on D shape optical fiber plane; Then, D shape optical fiber is immersed in the HF acid buffered soln in the stirring, with the D shape optical fiber plane of etching exposed portion, etching temperature is 50 ℃, and 5 minutes time, HF acid buffered soln is HF, the NH of 1:1:8 by mass ratio
4F and H
2O forms, and has so just obtained the micro-nano structure identical with pattern on the mask plate on D shape optical fiber plane, then uses the remaining photoresist material in KOH solution flush away D shape optical fiber plane, again with deionized water ultrasonic cleaning D shape optical fiber and dry.
Take water as solvent, the preparation diameter is the PMMA colloidal particle suspension liquid of 690nm, and volumetric concentration is 3%, and then ultrasonic concussion is 3 minutes.End with the D shape optical fiber of micro-nano structure that then will make is fixed on the stepper-motor, D shape optical fiber rest part is inserted in the colloidal particle suspension liquid, it is the electrostatic field of 1300V/m that whole device places strength of electric field, keeping the temperature of PMMA colloidal particle suspension liquid is 60 ℃, then stepper-motor outwards lifts D shape optical fiber with the speed of 2mm/min, break away from suspension liquid through about 30 minutes D shape optical fiber, can in the micro-nano structure on D shape optical fiber plane, make the PMMA colloidal crystal.
In the process, with the micro-nano structure on the D shape optical fiber plane after the S-4800 scanning electron microscopic observation etching, see accompanying drawing 1, it is a strip groove, and the degree of depth is about the 2-5 micron, and is wide 5 microns, long 100 microns.
With the colloidal crystal in the scanning electron microscopic observation micro-nano structure, see accompanying drawing 2, the structure of colloidal crystal according to the degree of depth of micro-nano structure, can estimate that colloidal crystal thickness is about 3 microns take face-centred cubic structure as main, the number of plies is about the 4-5 layer.
With the AQ6378 spectrum analyzer the prepared D shape optical fiber with the colloidal crystal micro-nano structure is carried out spectrum test, the transmitted spectrum that obtains, see accompanying drawing 3, can obviously find out the photon band gap of colloidal crystal among the figure, and can see through the wavelength of evanescent field and produce effectively selective action, Theoretical Calculation according to the photon band gap of 690nmPMMA colloidal crystal is 1544nm, conform to our test result, because colloidal crystal has long crystallographic direction in the fibre core direction, therefore larger to the modulation amplitude of D shape fiber evanescent field, reached-10dB.
Embodiment 3
Be fixed on the base plate with the circular face of silica gel with D shape optical fiber, coat photoresist material AZ-1350 on D shape optical fiber plane, then oven dry, D shape optical fiber and the mask plate that carries required pattern be contained in carry out exposure-processed on the lithography machine, exposure position is the central position on D shape optical fiber plane, the pattern that mask plate carries be three unimodal, 5 microns of peak width, long 50 microns, length direction is perpendicular to the fiber core direction, the exposure purpose is the photoresist material generation photochmeical reaction that makes photosensitive area, and molten change occurs when next step development; On drying machine, optical fiber was heated 3 minutes after the exposure, temperature 60 C, D shape optical fiber is immersed in develops in the acetone afterwards removes the photoresist material of exposed portion, has realized the design transfer on the mask plate to the photoresist material on D shape optical fiber plane; Then, D shape optical fiber is immersed in the HF acid buffered soln in the stirring, with the D shape optical fiber plane of etching exposed portion, etching temperature is 30 ℃, and 3 minutes time, HF acid buffered soln is HF, the NH of 1:1:8 by mass ratio
4F and H
2O forms, and has so just obtained the micro-nano structure identical with pattern on the mask plate on D shape optical fiber plane, is three parallel grooves, then uses the remaining photoresist material in KOH solution flush away D shape optical fiber plane, again with deionized water ultrasonic cleaning D shape optical fiber and dry.
Take water as solvent, preparing respectively diameter is the PS colloidal particle suspension liquid of 380nm, 510nm, 600nm, and volumetric concentration is 2%, and then each ultrasonic concussion is 3 minutes, and is for subsequent use.Close on the D shape optical fiber wherein two grooves with the AB rubber seal, then the end with D shape optical fiber is fixed on the stepper-motor, D shape optical fiber rest part is inserted in the 380nm PS colloidal particle suspension liquid, it is the electrostatic field of 600V/m that whole device places strength of electric field, keeping the temperature of PS colloidal particle suspension liquid is 40 ℃, then stepper-motor outwards lifts D shape optical fiber with the speed of 0.5mm/min, break away from suspension liquid through about 30 minutes D shape optical fiber, can in a groove on D shape optical fiber plane, make 380nm PS colloidal crystal.
Then wash AB glue in second groove on the D shape optical fiber with acetone, use again aforesaid method, the PS colloidal crystal of preparation 510nm in second groove, by that analogy, the PS colloidal crystal of preparation 600nm finally makes the colloidal crystal micro-nano structure that carries three kinds of different sizes on D shape optical fiber plane in the 3rd groove.
In the process, with the micro-nano structure on the D shape optical fiber plane after the S-4800 scanning electron microscopic observation etching, see accompanying drawing 4, it is three parallel grooves, and depth of groove is about 3 microns, wide 5 microns, long 50 microns.
With the colloidal crystal in the scanning electron microscopic observation micro-nano structure, the thickness of colloidal crystal is about 3 microns, and the number of plies is about the 3-5 layer.
The above-mentioned D shape optical fiber that carries three kinds of different size colloidal crystal micro-nano structures that makes is carried out spectral measurement, reflection spectrum is seen accompanying drawing 5, can find out among the figure and have 3 photon band gaps, centre wavelength and the calculated results coincide, and equally evanescent field have been produced obvious modulation and wavelength selective action.
Claims (3)
1. the preparation method of a D shape optical fiber colloidal crystal micro-nano structure is characterized in that: comprise the steps:
(1), be fixed on the base plate with the circular face of silica gel with D shape optical fiber, coat photoresist material on D shape optical fiber plane, then oven dry;
(2), D shape optical fiber and the required mask plate that will scribble photoresist material be contained on the lithography machine, exposed in D shape optical fiber plane, then with D shape optical fiber 30-60 ℃ of lower heating 3-5 minute, develop with acetone afterwards and remove the photoresist material of exposed portion;
(3), under the agitation condition, with HF acid buffered soln etching D shape optical fiber plane, realize the preparation of micro-nano structure on the D shape optical fiber plane, etching temperature 30-50 ℃, time 3-10 minute;
(4), with KOH solution flush away D shape optical fiber plane remaining photoresist material, then with deionized water ultrasonic cleaning D shape optical fiber and dry;
(5), preparation colloidal particle suspension liquid, volumetric concentration is 2-5%, then ultrasonic concussion is evenly distributed colloidal particle;
(6), the end with the D shape optical fiber of micro-nano structure that step (4) is made is fixed on the stepper-motor, D shape optical fiber rest part is inserted in the colloidal particle suspension liquid, it is the electrostatic field of 600-1300V/m that whole device places strength of electric field, keeping the temperature of colloidal particle suspension liquid is 40-60 ℃, then stepper-motor lifts D shape optical fiber with the speed of 0.5-2mm/min, until D shape optical fiber breaks away from suspension liquid, can in the micro-nano structure on D shape optical fiber plane, make colloidal crystal.
2. the preparation method of a kind of D shape optical fiber colloidal crystal micro-nano structure as claimed in claim 1 is characterized in that: described HF acid buffered soln is HF, the NH of 1:1:8 by mass ratio
4F and H
2O forms.
3. the preparation method of a kind of D shape optical fiber colloidal crystal micro-nano structure as claimed in claim 1, it is characterized in that: the colloidal particle in the described colloidal particle suspension liquid are PS, PMMA or SiO
2In a kind of.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105759363A (en) * | 2016-05-17 | 2016-07-13 | 河南科技大学 | Method for embedding micro-ring resonator into D-shaped optical fiber |
| CN111693464A (en) * | 2020-06-12 | 2020-09-22 | 山东大学 | Preparation method and preparation device of optical fiber sensor and sensor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101788697A (en) * | 2010-02-23 | 2010-07-28 | 南京师范大学 | Cladding type colloid crystalloid micro-structured fiber and preparation method thereof |
| CN101942700A (en) * | 2010-10-20 | 2011-01-12 | 南京师范大学 | Method for preparing circular cylindrical colloidal crystals based on optical fibers and crystals thereof |
| CN102053302A (en) * | 2010-12-14 | 2011-05-11 | 南京师范大学 | Colloidal crystal-modified optical fiber microstructural device and manufacturing method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101788697A (en) * | 2010-02-23 | 2010-07-28 | 南京师范大学 | Cladding type colloid crystalloid micro-structured fiber and preparation method thereof |
| CN101942700A (en) * | 2010-10-20 | 2011-01-12 | 南京师范大学 | Method for preparing circular cylindrical colloidal crystals based on optical fibers and crystals thereof |
| CN102053302A (en) * | 2010-12-14 | 2011-05-11 | 南京师范大学 | Colloidal crystal-modified optical fiber microstructural device and manufacturing method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105759363A (en) * | 2016-05-17 | 2016-07-13 | 河南科技大学 | Method for embedding micro-ring resonator into D-shaped optical fiber |
| CN111693464A (en) * | 2020-06-12 | 2020-09-22 | 山东大学 | Preparation method and preparation device of optical fiber sensor and sensor |
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