CN104609741A - Method for preparing microstructure in glass capillary tube - Google Patents
Method for preparing microstructure in glass capillary tube Download PDFInfo
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- CN104609741A CN104609741A CN201510083118.XA CN201510083118A CN104609741A CN 104609741 A CN104609741 A CN 104609741A CN 201510083118 A CN201510083118 A CN 201510083118A CN 104609741 A CN104609741 A CN 104609741A
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Abstract
The invention discloses a method for preparing a microstructure in a glass capillary tube. The method comprises the following steps: cleaning the glass capillary tube and injecting a photoresist; opening a femtosecond laser device and a micromachining work bench; locking a mold of the femtosecond laser device and then introducing into the micromachining work bench; transversely fixing the glass capillary tube which is fully filled with the photoresist on a three-dimensional mobile platform of the micromachining work bench, and focusing, so that a focus point of the femtosecond laser device falls on the juncture of the bottom wall of the glass capillary tube and the photoresist; controlling movement of the micromachining work bench by virtue of control software, and simultaneously carrying out microstructure photoetching by virtue of the femtosecond laser device; and absorbing unexposed photoresist in the glass capillary tube. The method for preparing the microstructure in the glass capillary tube is high in machining speed, high in accuracy and high in flexibility by using a femtosecond laser two-photon micromachining technology; kinds of microstructures can be prepared in the glass capillary tube; and the preparation process is simple and easy to operate.
Description
Technical field
The present invention relates to a kind of micro-structure preparation method, particularly relate to a kind of method preparing microstructure in hollow glass kapillary.
Background technology
Glass capillary has important application in numerous areas, as gas-chromatography, biological point sample etc.The general inner hollow of common glass capillary and inner wall smooth, thus limit its use at special dimension.Such as, need sometimes to arrange the microstructures such as filter screen in glass capillary inside, be prepared into and a kind ofly there is the passage of screening function so that screening sample.But glass capillary internal diameter, all only between 0.1mm ~ 1mm, arranges microstructure difficulty therein very big, therefore need badly invent a kind of simple and feasible, the maneuverable method preparing microstructure in glass capillary.
On the other hand, it is high that Fs laser double photon micro-processing technology has working accuracy, heat effect is little, non-mask, handiness is high, and can really realize the advantages such as three-dimensional micro Process and become one of micro-processing technology means of current most welcome, in recent years at biotechnology, aerospace, the fields such as national defence obtain development fast and apply widely.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of making method is simple, workable, the method preparing microstructure in glass capillary of stable performance.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of method 1, preparing microstructure in glass capillary, is characterized in that: comprise the following steps:
1) glass capillary cleaned up and inject photoresist material;
2) open femto-second laser and micro Process worktable, will import in micro Process worktable after femto-second laser locked mode, glass capillary inside being filled photoresist material be laterally fixed in the three-dimensional mobile platform of micro Process worktable,
3) carry out the first step focusing, make the focus of femto-second laser drop on the center position of glass capillary horizontal clearance;
4) second step focusing is carried out, on the photoresist material that the focus of femto-second laser is dropped in glass capillary;
5) carry out the 3rd step burnt, make the focus of femto-second laser drop on the diapire of glass capillary and the intersection of photoresist material;
6) control software design is utilized to control the movement of micro Process worktable and carry out the photoetching of microstructure simultaneously with femto-second laser;
7) by photoresist material sucking-off unexposed in glass capillary.
Preferably, described step 1) be specially the photoresist material that to take a morsel in dark surrounds and be placed in small beaker, in photoresist material, also dry described glass capillary during bubble-free, will be crossed vertically insert wherein with washes of absolute alcohol, and leave standstill for some time, treat that in glass capillary, suction is taken out, by the lens wiping paper wiped clean being moistened with dehydrated alcohol after being full of photoresist material.
Preferably, described the first step focusing specifically comprises the following steps:
1) control three-dimensional mobile platform move and then regulate height and the position of glass capillary, make the height of glass capillary just in time at the near focal point of femtosecond laser;
2) three-dimensional mobile platform is moved horizontally and ccd video camera directly over passing through is observed until find the boundary position of light and shade sudden change, regulate the height of glass capillary, make border reach the most clear;
3) glass capillary is moved horizontally toward extending darker direction, until find the border that another light and shade is suddenlyd change, get the half of the distance that this moves horizontally, glass capillary is moved from another light and shade boundary toward by-level, and now the focus of femtosecond laser drops on the center position of the horizontal clearance of glass capillary.
Preferably, described second step focusing comprises the following steps: the plane microstructure by Computer Design one area being 10um × 10um, and operating software controls the three-dimensional mobile platform motion of fixing glass kapillary, and photoetching is carried out to glass capillary, if directly over ccd video camera in can't see microstructure in glass capillary, then moving three dimension mobile platform regulates the height of glass capillary, glass capillary is raised or reduces, often raise or reduce 20um and then run a software and carry out photoetching, until can microstructure be seen.
Preferably, described 3rd step Jiao comprises: 1) raise the height of glass capillary, and often raises 5um and run a software and carry out photoetching, until can not process microstructure positional; 2) then back progressively reduce the height of glass capillary every 1um, operating software carries out photoetching simultaneously, makes just in time can process microstructure; 3) glass capillary is moved axially.
Preferably, step 7 wherein) comprise the end thereof contacts of glass capillary on water suction paper handkerchief, paper handkerchief is utilized to be sucked out completely by photoresist material unexposed in glass capillary, and then glass capillary is vertically inserted in dehydrated alcohol, treat dehydrated alcohol be full of glass capillary after take out again with paper handkerchief by dehydrated alcohol sucking-off, repeatedly this step 3 ~ 4 time.
For the ease of sucking photoresist material in glass capillary, described glass capillary 1/3 length be inserted in photoresist material.
Compared with prior art, the invention has the advantages that the method preparing microstructure in this glass capillary utilizes Fs laser double photon micro-processing technology, process velocity is fast, precision is high, handiness is strong, can prepare various microstructure, and preparation process is simple to operation in glass capillary.Achieve simultaneously and microstructure is set in glass capillary, thus add the purposes of glass capillary, expand the Application Areas of glass capillary.And focusing step wherein, reduces the difficulty of focusing to a certain extent, reduces time needed for focusing.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that the method for microstructure device used prepared by the glass capillary of the embodiment of the present invention.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
The method preparing microstructure in glass capillary of the embodiment of the present invention, as shown in Figure 1, its device used comprises the light source femto-second laser 1 for Fs laser double photon micro-processing technology, for carrying the micro Process worktable 2 of glass capillary 4 to be processed, connect the computer 3 of the control module 21 of micro Process worktable, described computer 3 is provided with control software design, for designing microstructure and being controlled the running of micro Process worktable by control module 21, as the glass capillary 4 of processing object, as the slide glass 5 of the carrier of glass capillary, and be used for reflecting the high-reflectivity eyeglass group 6 between femto-second laser 1 and micro Process worktable of laser that femto-second laser sends.The control that wherein micro Process worktable 2 comprises by computer 3 is used for controlling the control module 21 of micro Process process and the three-dimensional mobile platform 22 of carrying slide glass 4.This control module 21 controls moving three dimension mobile platform 22 to regulate the position of glass capillary 4 on this slide glass 5, and regulating and controlling expands light path 24 and then for regulating the size of laser beam expanding, and is used for controlling the position of microcobjective 23.Wherein this three-dimensional mobile platform 22 fixes described slide glass 5, describedly expand after light path 24 is positioned at high-reflectivity eyeglass group 6, for microcobjective 23 is injected in the laser aiming through high-reflectivity eyeglass group 6, described microcobjective 23 is positioned at directly over slide glass 5, namely be positioned at directly over glass capillary 4, femtosecond laser is incident upon the glass capillary 4 on slide glass 5 by microcobjective 23, ccd video camera 25 is arranged in for observing in the course of processing directly over this microcobjective 23, and described ccd video camera 25 is connected to computer 3.
For the ease of more clearly understanding, following to be 0.3mm at an internal diameter, to prepare that diameter is 100um, height is the method for the three-dimensional cylinder microstructure of 100um in the length glass capillary that is 10cm.
First, first glass capillary 4 is crossed with washes of absolute alcohol and drying, the described photoresist material that takes a morsel in dark surrounds is placed in small beaker, leave standstill for some time, during bubble-free, dried glass capillary 4 is vertically inserted wherein in photoresist material, and continue to leave standstill for some time, utilize capillarity to allow photoresist material automatically be filled with in glass capillary 4.In order to make the photoresist material that can inject enough height in glass capillary 4, the length of glass capillary 4 1/3 should be inserted in photoresist material.Also other method can be selected according to actual needs in glass capillary 4 to inject photoresist material, as injector to inject, high-pressure pump extraction etc.Treat that glass capillary 4 is taken out after sucking the photoresist material of certain altitude, with the lens wiping paper being moistened with dehydrated alcohol, surface wipes is clean.
Then, open femto-second laser 1 and mobile micro Process worktable 2, by femto-second laser 1 furnishing mode-lock status, the wavelength of launching of femto-second laser 1 is adjusted to 780nm.Control module 21 in micro Process worktable 2 and pick up camera 25 are connected on described computer 3 by data line.After the success of femto-second laser 1 locked mode, utilize the speculum group 6 of high-reflectivity to be imported in micro Process worktable 2 by femtosecond laser, and expanded after femtosecond laser expands by light path light path 24 by the microcobjective that micro Process worktable 2 carries and import to again in microcobjective 23.
Glass capillary 4 adhesive tape inside being injected photoresist material is laterally fixed on slide glass 5, then the three-D displacement platform 22 being positioned over micro Process worktable 2 is focused.Focusing mainly comprises the steps: 1) utilize computer 3 control three-D displacement platform 22 by control module 21 and then regulate height and the position of glass capillary 4, glass capillary 4 is adjusted to immediately below microcobjective 23 and locates, and make the height of glass capillary 4 just in time near the focal length of microcobjective 23, be namely positioned at the near focal point of femtosecond laser.2) control three-D displacement platform 22, glass capillary 4 is moved horizontally, and is observed by the ccd video camera 25 that micro Process worktable 2 carries, until find the border of light and shade sudden change.Regulate the height of glass capillary 4, make border reach the most clear.3) glass capillary 4 is moved horizontally toward the direction that color is darker, until find the border that another light and shade is suddenlyd change, and on control software design, read distance when three-D displacement platform 22 is moved horizontally to another light and shade boundary from a light and shade boundary.Then get the half of its distance, glass capillary 4 is moved horizontally from a light and shade boundary toward another border, and position is now the centre of glass capillary 4 horizontal clearance.4) first by designing the plane microstructure that an area is 10um × 10um in the design software on computer 3, and operating software carries out photoetching to glass capillary 4, micro Process worktable 2 is made to enter micro Process state, namely micro Process worktable 2 moves under the control of control module 21, and carry out photoetching by femto-second laser 1 simultaneously, if now the focus of femto-second laser drops in the photoresist material of glass capillary 4, then microstructure can be carved, if the focus of femto-second laser drops on glass capillary 4, then by lithography microstructure cannot be made, if lose sight of processed microstructure out in pick up camera 25, then by the height of control module 21 up-down adjustment glass capillary 4.Glass capillary 4 often raises or reduces 20um, operating software once, until the microstructure inscribed out can be seen in pick up camera 25.Now namely represent femtosecond laser to be focused in the photoresist material in glass capillary 4 by microcobjective 22.5) height raising glass capillary 4 is continued, and often raise 5um operating software once, repeat this step, until can not microstructure be processed, now, the focus of femtosecond laser close to the intersection of diapire and photoresist material in glass capillary 4, and focuses on and is positioned at the diapire of glass capillary 4 and the below of photoresist material intersection, i.e. in the diapire of the glass capillary of the below of the bottom margin of glass capillary and photoresist material.Then back progressively reduce the height of glass capillary 4 every 1um, operating software, makes just in time can carve microstructure simultaneously.Now show that the focus of femtosecond laser just in time drops on the internal surface of bottom tube wall of photoresist material and glass capillary 4, namely on the diapire of glass capillary and the border of photoresist material, namely focus process completes.6) glass capillary 4 is moved axially certain distance, preferably, about 200um, recycling controlling software design diameter is 100um, it is highly the three-dimensional column structure of 100um, and microstructure is carved in the photoresist material of glass capillary 4 by operating software, now namely on the internal surface of the bottom tube wall of glass capillary, make this microstructure by lithography.
Finally, take off glass capillary 4, by its end thereof contacts on water suction paper handkerchief, utilize paper handkerchief to be sucked out completely by photoresist material unexposed in glass capillary 4.And then glass capillary 4 is vertically inserted in dehydrated alcohol, treat dehydrated alcohol be full of glass capillary 4 after take out again with paper handkerchief by dehydrated alcohol sucking-off.Repeatedly about this step 3 ~ 4 time, treat that namely preparation process completes by complete for photoresist material cleaning unexposed in glass capillary 4, obtain required diameter and be 100um, highly be the three-dimensional column structure of 100um.
This photoresist material is commercially available negative photoresist material, has had resolving power higher, is insoluble to the feature of the organic reagents such as ethanol when having unexposed after dissolving in the organic reagents such as ethanol, exposure.Therefore, namely the photoresist material after femto-second laser exposure forms microstructure and is arranged in glass capillary.
Described glass capillary can be commercially available biological point sample kapillary, and internal diameter is 0.3mm, and length is 10cm.Also can according to practical use and needs, the internal diameter of selected glass capillary and length parameter.
Described femto-second laser can select the U.S. to be concerned with the femto-second laser of companies market, and model is Mari-f900, and outgoing wavelength is set as 780nm.Also can adopt the commercially available femto-second laser of other model, only require that the infrared laser of energy outgoing 780nm wavelength also can locked mode.
Femtosecond laser parallel micromachining worktable can select the uFAB type micro Process platform into U.S. Newport companies market, and its operation wavelength is 780nm, and supportingly has described control module.
Described control software design is used to the related software of the control module manipulated on described micro Process worktable, and with design function.Control software design described in utilization, overallly can manipulate the movement of all accessories on micro Process worktable, and can design the microstructure of different shape, size.
The foregoing is only specific embodiment of the present invention, the meticulous plane of various complex structure or three-dimensional structure can also be prepared in glass capillary.
The method preparing microstructure in this glass capillary utilizes Fs laser double photon micro-processing technology, and process velocity is fast, and precision is high, and handiness is strong, can prepare various microstructure, and preparation process is simple to operation in glass capillary.Achieve simultaneously and microstructure is set in glass capillary, thus add the purposes of glass capillary, expand the Application Areas of glass capillary.And focusing step wherein, reduces the difficulty of focusing to a certain extent, reduces time needed for focusing.
Claims (7)
1. prepare a method for microstructure in glass capillary, it is characterized in that: comprise the following steps:
1) glass capillary (4) is cleaned up and injects photoresist material;
2) open femto-second laser and micro Process worktable, will import in micro Process worktable after femto-second laser locked mode, glass capillary inside being filled photoresist material be laterally fixed in the three-dimensional mobile platform of micro Process worktable;
3) carry out the first step focusing, make the focus of femto-second laser (1) drop on the center position of glass capillary (4) horizontal clearance;
4) second step focusing is carried out, on the photoresist material that the focus of femto-second laser (1) is dropped in glass capillary (4);
5) carry out the 3rd step burnt, make the focus of femto-second laser (1) drop on the diapire of glass capillary (4) and the intersection of photoresist material;
6) control software design is utilized to control the movement of micro Process worktable and carry out the photoetching of microstructure simultaneously with femto-second laser;
7) by photoresist material sucking-off unexposed in glass capillary (4).
2. in glass capillary as claimed in claim 1, prepare the method for microstructure, it is characterized in that: described step 1) be specially the photoresist material that to take a morsel in dark surrounds and be placed in small beaker, in photoresist material, also dry described glass capillary (4) during bubble-free, will be crossed vertically insert wherein with washes of absolute alcohol, and leave standstill for some time, treat that in glass capillary (4), suction is taken out, by the lens wiping paper wiped clean being moistened with dehydrated alcohol after being full of photoresist material.
3. prepare the method for microstructure as claimed in claim 1 or 2 in glass capillary, it is characterized in that: described the first step focusing specifically comprises the following steps:
1) control three-dimensional mobile platform move and then regulate height and the position of glass capillary (4), make the height of glass capillary (4) just in time at the near focal point of femtosecond laser;
2) three-dimensional mobile platform is moved horizontally and ccd video camera (25) directly over passing through is observed until find the boundary position of light and shade sudden change, regulate the height of glass capillary (4), make border reach the most clear;
3) glass capillary (4) is moved horizontally toward extending darker direction, until find the border that another light and shade is suddenlyd change, get the half of the distance that this moves horizontally, glass capillary (4) is moved from another light and shade boundary toward by-level, and now the focus of femtosecond laser drops on the center position of the horizontal clearance of glass capillary (4).
4. in glass capillary as claimed in claim 3, prepare the method for microstructure, it is characterized in that: described second step focusing comprises the following steps: the plane microstructure by Computer Design one area being 10um × 10um, and operating software controls the three-dimensional mobile platform motion of fixing glass kapillary (4), and photoetching is carried out to glass capillary (4), if directly over ccd video camera (25) in can't see microstructure in glass capillary (4), then moving three dimension mobile platform regulates the height of glass capillary, glass capillary is raised or reduces, often raise or reduce 20um and run a software and carry out photoetching, until can microstructure be seen.
5. in glass capillary as claimed in claim 4, prepare the method for microstructure, it is characterized in that: described 3rd step Jiao comprises: the height 1) raising glass capillary (4), and often raise 5um to run a software and carry out photoetching, until can not microstructure positional be processed; 2) then back progressively reduce the height of glass capillary (4) every 1um, operating software carries out photoetching simultaneously, makes just in time can process microstructure; 3) glass capillary (4) is moved axially.
6. in glass capillary as claimed in claim 1, prepare the method for microstructure, it is characterized in that: step 7 wherein) comprise the end thereof contacts of glass capillary (4) on water suction paper handkerchief, paper handkerchief is utilized to be sucked out completely by unexposed photoresist material in glass capillary (4), and then glass capillary (4) is vertically inserted in dehydrated alcohol, treat dehydrated alcohol be full of to take out after glass capillary (4) again with paper handkerchief by dehydrated alcohol sucking-off, repeatedly this step 3 ~ 4 time.
7. prepare the method for microstructure in glass capillary as claimed in claim 2, it is characterized in that: described glass capillary (4) 1/3 length be inserted in photoresist material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967532A (en) * | 2016-06-06 | 2016-09-28 | 宁波大学 | Device and method for rotatably machining microstructure in glass capillary |
| CN108319113A (en) * | 2018-01-31 | 2018-07-24 | 宁波大学 | The distortion correcting method of processing micro structure in a kind of capillary glass tube |
| CN108838546A (en) * | 2018-07-24 | 2018-11-20 | 长春理工大学 | Thin micro tube inner surface micro-structure laser processing |
| CN109188869A (en) * | 2018-09-29 | 2019-01-11 | 宁波市效实中学 | A method of preparing micro-structure in opaque substrate |
| CN109336049A (en) * | 2018-10-11 | 2019-02-15 | 宁波大学 | A kind of micro-structure operating method and operating device |
| CN111496395A (en) * | 2020-04-17 | 2020-08-07 | 中国电子科技集团公司第十一研究所 | Machining tool and machining method for throttle hole of J-T refrigerator |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105967532A (en) * | 2016-06-06 | 2016-09-28 | 宁波大学 | Device and method for rotatably machining microstructure in glass capillary |
| CN105967532B (en) * | 2016-06-06 | 2018-12-18 | 宁波大学 | The devices and methods therefor of processing micro structure is rotated in a kind of capillary glass tube |
| CN108319113A (en) * | 2018-01-31 | 2018-07-24 | 宁波大学 | The distortion correcting method of processing micro structure in a kind of capillary glass tube |
| CN108319113B (en) * | 2018-01-31 | 2021-01-08 | 宁波大学 | Deformation correction method for processing microstructure in glass capillary |
| CN108838546A (en) * | 2018-07-24 | 2018-11-20 | 长春理工大学 | Thin micro tube inner surface micro-structure laser processing |
| CN109188869A (en) * | 2018-09-29 | 2019-01-11 | 宁波市效实中学 | A method of preparing micro-structure in opaque substrate |
| CN109188869B (en) * | 2018-09-29 | 2020-08-28 | 宁波市效实中学 | Method for preparing microstructure on opaque substrate |
| CN109336049A (en) * | 2018-10-11 | 2019-02-15 | 宁波大学 | A kind of micro-structure operating method and operating device |
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| CN111496395A (en) * | 2020-04-17 | 2020-08-07 | 中国电子科技集团公司第十一研究所 | Machining tool and machining method for throttle hole of J-T refrigerator |
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Effective date of registration: 20200624 Address after: 313219 Zhejiang city of Huzhou province Deqing County LEIDIAN Town Industrial Park Patentee after: ZHEJIANG JINCHEN GLASS Co.,Ltd. Address before: 315211 Zhejiang Province, Ningbo Jiangbei District Fenghua Road No. 818 Patentee before: Ningbo University |