CN104609741B - A kind of method that micro structure is prepared in capillary glass tube - Google Patents
A kind of method that micro structure is prepared in capillary glass tube Download PDFInfo
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- CN104609741B CN104609741B CN201510083118.XA CN201510083118A CN104609741B CN 104609741 B CN104609741 B CN 104609741B CN 201510083118 A CN201510083118 A CN 201510083118A CN 104609741 B CN104609741 B CN 104609741B
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Abstract
A kind of method that micro structure is prepared in capillary glass tube, comprises the following steps：Capillary glass tube is cleaned up and photoresist is injected；Open femto-second laser and micro Process workbench, to import to after femto-second laser locked mode in micro Process workbench, the capillary glass tube that inside fills photoresist is fastened transversely in the three-dimensional mobile platform of micro Process workbench, focused, made the intersection of the diapire that the focus of femto-second laser falls in capillary glass tube and photoresist；The movement of micro Process workbench is controlled using control software and while the photoetching of micro structure is carried out with femto-second laser；Unexposed photoresist in capillary glass tube is suctioned out.The method that micro structure is prepared in the capillary glass tube utilizes Fs laser double photon micro-processing technology, and process velocity is fast, and high precision, motility are strong, can prepare various micro structures, and preparation process is simple to operation in capillary glass tube.
Description
Technical field
The present invention relates to a kind of micro-structure preparation method, more particularly to one kind prepares micro structure in hollow glass capillary tube
Method.
Background technology
Capillary glass tube has important application, such as gas chromatogram, biological point sample etc. in numerous areas.Common glass
The general inner hollow of capillary tube and inner wall smooth, thus limit its use in special dimension.Such as, need sometimes
The micro structures such as filter screen are set inside glass capillary, a kind of passage with screening function are prepared in order to screening sample.
But, capillary glass tube internal diameter arranges micro structure difficulty greatly inside which all only between 0.1mm～1mm, therefore needs badly and send out
It is bright go out a kind of simple and feasible, the maneuverable method that micro structure is prepared in capillary glass tube.
On the other hand, Fs laser double photon micro-processing technology has machining accuracy high, and heat effect is little, maskless, flexibly
Property it is high, and become one of micro-processing technology means most welcome at present the advantages of can really realize three-dimensional micro Process, in recent years
Come in biological engineering, Aero-Space, the field such as national defence has obtained quick development and has been widely applied.
The content of the invention
It is simple, workable, stable performance that the technical problem to be solved is to provide a kind of manufacture method
The method that micro structure is prepared in capillary glass tube.
The present invention solve the technical scheme that adopted of above-mentioned technical problem for：1st, micro structure is prepared in a kind of capillary glass tube
Method, it is characterised in that：Comprise the following steps：
1) capillary glass tube is cleaned up and injects photoresist；
2) femto-second laser and micro Process workbench are opened, micro Process workbench will be imported to after femto-second laser locked mode
In, the capillary glass tube that inside fills photoresist is fastened transversely in the three-dimensional mobile platform of micro Process workbench,
3) first step focusing is carried out, makes the focus of femto-second laser fall in the center position of capillary glass tube horizontal width
Put；
4) second step focusing is carried out, is made on the photoresist that the focus of femto-second laser falls in capillary glass tube；
5) carry out the 3rd step burnt, make the boundary of the diapire that the focus of femto-second laser falls in capillary glass tube and photoresist
Place；
6) movement of micro Process workbench is controlled using control software and while carry out micro structure with femto-second laser
Photoetching；
7) unexposed photoresist in capillary glass tube is suctioned out.
Preferably, the step 1) it is specially and a small amount of photoresist is taken in dark surrounds is placed in small beaker, treat photoresist
When be inserted vertically into wherein
Between, treat that suction is full of being drawn off after photoresist in capillary glass tube, with the lens paper wiped clean for being moistened with dehydrated alcohol.
Preferably, the first step focusing specifically includes following steps：
1) control three-dimensional mobile platform movement and then adjust height and the position of capillary glass tube, make the height of capillary glass tube
Degree is just in the near focal point of femtosecond laser；
2) three-dimensional mobile platform is made to move horizontally and by the ccd video camera observation of surface until finding light and shade mutation
Boundary position, adjusts the height of capillary glass tube, reaches border most clear；
3) capillary glass tube is moved horizontally toward deeper direction is extended, until finding the border of another light and shade mutation, is taken
The half of the distance for moving horizontally, makes capillary glass tube move from another light and shade boundary toward by-level, and now femtosecond swashs
The focus of light fall capillary glass tube horizontal width center position.
Preferably, the second step focusing is comprised the following steps：By one area of Computer Design for 10um × 10um's
Plane micro structure, and the three-dimensional mobile platform motion of the fixed capillary glass tube of runs software control, and capillary glass tube is entered
Row photoetching, if the micro structure in capillary glass tube is can't see in the ccd video camera of surface, moving three dimension mobile platform is adjusted
The height of section capillary glass tube, is raised and lowered capillary glass tube, and 20um is often raised and lowered then running a software is carried out
Photoetching, until it can be seen that micro structure.
Preferably, the 3rd step Jiao includes：1) height of capillary glass tube is raised, and often raises 5um operations one
Secondary software carries out photoetching, until microstructure positional can not be processed；2) and then back capillary glass tube is gradually reduced every 1um
Highly, while runs software carries out photoetching, make just process micro structure；3) move axially capillary glass tube.
Preferably, wherein 7) the step of includes the end thereof contacts of capillary glass tube are absorbing water on napkin, will using napkin
In capillary glass tube, unexposed photoresist is sucked out completely, then again capillary glass tube is inserted vertically in dehydrated alcohol, is treated
Dehydrated alcohol takes out after being full of capillary glass tube and suctions out dehydrated alcohol with napkin again, repeatedly this step 3～4 time.
For the ease of sucking photoresist in capillary glass tube, the capillary glass tube at least 1/3rd length insertion
To in photoresist.
Compared with prior art, it is an advantage of the current invention that the method that micro structure is prepared in the capillary glass tube utilizes femtosecond
Laser Two-photon micro-processing technology, process velocity are fast, high precision, and motility is strong, and various micro- knots can be prepared in capillary glass tube
Structure, and preparation process is simple to operation.Realize simultaneously and micro structure is set in capillary glass tube, so as to increased glass capillary
The purposes of pipe, expands the application of capillary glass tube.And focusing step therein, reduces focusing to a certain extent
Difficulty, reduce focusing needed for time.
Description of the drawings
The schematic diagram of devices of the Fig. 1 used by the method for the capillary glass tube preparation micro structure of the embodiment of the present invention.
Specific embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
The method that micro structure is prepared in capillary glass tube of the embodiment of the present invention, as shown in figure 1, the device bag used by which
The light source femto-second laser 1 for Fs laser double photon micro-processing technology is included, for carrying capillary glass tube 4 to be processed
Micro Process workbench 2, connects the computer 3 of the control module 21 of micro Process workbench, and it is soft that the computer 3 is provided with control
Part, for designing micro structure and the running of micro Process workbench being controlled by control module 21, as the glass of processing object
Capillary tube 4, as the microscope slide 5 of the carrier of capillary glass tube, and for reflecting the position of the laser sent by femto-second laser
High reflectance eyeglass group 6 between femto-second laser 1 and micro Process workbench.Wherein micro Process workbench 2 includes being calculated
The control of machine 3 is used for the control module 21 for controlling micro Process process and the three-dimensional mobile platform 22 for carrying microscope slide 4,.The control
Molding block 21 controls moving three dimension mobile platform 22 to adjust the position of capillary glass tube 4 on the microscope slide 5, and control and regulation are expanded
Light path 24 and then the size for adjusting laser beam expanding, and for controlling the position of microcobjective 23.Wherein the three-dimensional is mobile flat
Fix the microscope slide 5 on platform 22, the light path 24 that expands after high reflectance eyeglass group 6, for will be through high reflection
Microcobjective 23 is injected in the laser aiming of rate lens set 6, and the microcobjective 23 is located at the surface of microscope slide 5, i.e., positioned at glass
The surface of glass capillary tube 4, femtosecond laser are incident upon the capillary glass tube 4 on microscope slide 5, ccd video camera by microcobjective 23
25 surfaces for being located at the microcobjective 23 are used to be observed in process, and the ccd video camera 25 is connected to calculating
Machine 3.
It is for the ease of being more clearly understood that, following with a capillary glass tube that internal diameter is as 0.3mm, length is as 10cm
Prepare a diameter of 100um, highly for 100um three-dimensional cylinder micro structure method as a example by.
First, first capillary glass tube 4 is crossed with washes of absolute alcohol and is dried, a small amount of photoetching is taken in dark surrounds
Glue is placed in small beaker, stands a period of time, and dried capillary glass tube 4 is inserted vertically into which during bubble-free in the photoresist
In, and continue to stand a period of time, allow photoresist be filled with capillary glass tube 4 automatically using capillarity.In order that glass fiber
The photoresist of enough height can be injected in tubule 4, the length of capillary glass tube 4 at least 1/3rd photoresist should be inserted into
In.Photoresist, such as syringe injection, high pressure can also be injected in capillary glass tube 4 from other methods according to actual needs
Pumping takes.It is drawn off after the photoresist for treating the suction certain altitude of capillary glass tube 4, with the lens paper for being moistened with dehydrated alcohol
Surface wipes are clean.
Then, femto-second laser 1 and mobile micro Process workbench 2 are opened, femto-second laser 1 is tuned into into mode-lock status, will
The wavelength of launching of femto-second laser 1 is adjusted to 780nm.Control module 21 and video camera 25 in micro Process workbench 2 is led to
Cross data wire to be connected on described computer 3.After 1 locked mode success of femto-second laser, using the speculum group 6 of high reflectance
Femtosecond laser is imported in micro Process workbench 2, and the microcobjective carried by micro Process workbench 2 expands light path light path
24 femtosecond laser is expanded after imported in microcobjective 23 again.
The capillary glass tube 4 of internal injection photoresist is secured transverse on microscope slide 5 with adhesive tape, then is positioned over micro Process
Focused on the three-D displacement platform 22 of workbench 2.Focusing mainly comprises the steps：1) using computer 3 by controlling mould
Capillary glass tube 4 is adjusted to micro- thing by height and the position of the control three-D displacement of block 21 platform 22 and then regulation capillary glass tube 4
At the underface of mirror 23, and make the height of capillary glass tube 4 just near the focal length of microcobjective 23, i.e., positioned at femtosecond laser
Near focal point.2) three-D displacement platform 22 is controlled, moves horizontally capillary glass tube 4, and carried by micro Process workbench 2
Ccd video camera 25 is observed, till finding the border of light and shade mutation.The height of glass capillary 4 is adjusted, border is reached most
Clearly.3) capillary glass tube 4 is moved horizontally toward the deeper direction of color, till finding the border of another light and shade mutation,
And read in control software three-D displacement platform 22 from a light and shade boundary be moved horizontally to another light and shade boundary when distance.
Then the half of its distance is taken, capillary glass tube 4 is moved horizontally toward another border from a light and shade boundary, position now is
For the centre of 4 horizontal width of capillary glass tube.4) design in first passing through the design software on computer 3 area for 10um ×
The plane micro structure of 10um, and runs software carries out photoetching to capillary glass tube 4, makes micro Process workbench 2 enter micro Process shape
State, i.e. micro Process workbench 2 are moved under the control of control module 21, and while carry out photoetching by femto-second laser 1, if
Now the focus of femto-second laser falls in the photoresist of capillary glass tube 4, then can carve micro structure, if femto-second laser
Focus fall on capillary glass tube 4, then cannot make micro structure by lithography, be processed out micro- if losing sight of in video camera 25
Structure, then adjust the height of capillary glass tube 4 by control module about 21.Capillary glass tube 4 is often raised and lowered 20um, fortune
Row software once, till it can see the micro structure inscribed out in video camera 25.Femtosecond laser has been represented now
Focused in the photoresist in capillary glass tube 4 by microcobjective 22.5) continue to raise the height of capillary glass tube 4, and per liter
High 5um runs softwares once, repeat this step, and till it can not process micro structure, now, the focus of femtosecond laser is close to
The inner bottom wall of capillary glass tube 4 and the intersection of photoresist, and focus on inner bottom wall and photoresist friendship positioned at capillary glass tube 4
In the diapire of the capillary glass tube of the lower section of the bottom margin of the lower section at boundary, i.e. capillary glass tube and photoresist.Then back
The height of capillary glass tube 4 is gradually reduced every 1um, while runs software, makes just carve micro structure.Now show femtosecond
The focus of laser just fall the bottom tube wall in photoresist Yu capillary glass tube 4 inner surface on, i.e. the diapire of capillary glass tube
On the border of photoresist, i.e., focus process is completed.6) capillary glass tube 4 is moved axially into certain distance, it is preferable that about
200um, recycles one a diameter of 100um of controlling software design, is highly the three-dimensional column structure of 100um, and runs software
Micro structure is carved in the photoresist of capillary glass tube 4, now i.e. capillary glass tube bottom tube wall inner surface glazing
Carve the micro structure.
Finally, capillary glass tube 4 is removed, by one end in contact on water suction napkin, using napkin by capillary glass tube 4
Unexposed photoresist is sucked out completely.Then again capillary glass tube 4 is inserted vertically in dehydrated alcohol, treats that dehydrated alcohol is full of
Take out after capillary glass tube 4 and dehydrated alcohol is suctioned out with napkin again.This step 3～4 time or so, treat capillary glass tube repeatedly
Unexposed photoresist cleaning in 4 is finished, i.e., preparation process is completed, and is obtained required a diameter of 100um, is highly 100um's
Three-dimensional column structure.
The photoresist is commercially available negative photoresist, has had resolution higher, with it is unexposed when to dissolve in ethanol etc. organic
The characteristics of after reagent, exposure insoluble in organic reagents such as ethanol.Therefore, the photoresist after femto-second laser exposure forms micro-
Structure is located in capillary glass tube.
Described capillary glass tube can be commercially available biological point sample capillary tube, and internal diameter is 0.3mm, and length is 10cm.Also may be used
According to practical use and needs, to select the internal diameter and length parameter of capillary glass tube.
Described femto-second laser can select the femto-second laser of the relevant companies market in the U.S., and model Mari-f900 goes out
Ejected wave length is set as 780nm.The commercially available femto-second laser of other models can also be adopted, energy outgoing 780nm wavelength is only required
Iraser simultaneously can locked mode.
Femtosecond laser parallel micromachining workbench can select the uFAB type micro Process platforms for U.S.'s Newport companies markets, its work
It is 780nm to make wavelength, and is configured with described control module.
The control software is the related software for manipulating the control module on the micro Process workbench, and with figure
Case design function.Using described control software, the movement of all accessories on micro Process workbench can be manipulated with the overall situation, and can
Design the micro structure of variously-shaped, size.
Only certain embodiments of the present invention is the foregoing is only, can be so that various complex structures be prepared in capillary glass tube
Fine plane or three dimensional structure.
The method that micro structure is prepared in the capillary glass tube utilizes Fs laser double photon micro-processing technology, process velocity
Hurry up, high precision, motility are strong, can prepare various micro structures, and preparation process is simple to operation in capillary glass tube.It is simultaneously real
Showing and micro structure has been set in capillary glass tube, so as to increased the purposes of capillary glass tube, having expanded answering for capillary glass tube
Use field.And focusing step therein, reduces the difficulty of focusing to a certain extent, reduces the focusing required time.
Claims (4)
1. a kind of method that micro structure is prepared in capillary glass tube, it is characterised in that：Comprise the following steps：
1) capillary glass tube (4) is cleaned up and injects photoresist；
2) femto-second laser and micro Process workbench are opened, will be imported to after femto-second laser locked mode in micro Process workbench,
The capillary glass tube that inside fills photoresist is fastened transversely in the three-dimensional mobile platform of micro Process workbench；
3) first step focusing is carried out, makes the focus of femto-second laser (1) fall in the center position of capillary glass tube (4) horizontal width
Put；
4) second step focusing is carried out, is made on the photoresist that the focus of femto-second laser (1) falls in capillary glass tube (4)；
5) carry out the 3rd step burnt, make the friendship of the diapire that the focus of femto-second laser (1) falls in capillary glass tube (4) and photoresist
At boundary；
6) movement of micro Process workbench is controlled using control software and while the photoetching of micro structure is carried out with femto-second laser；
7) unexposed photoresist in capillary glass tube (4) is suctioned out；
The first step focusing specifically includes following steps：
1) control three-dimensional mobile platform movement and then adjust height and the position of capillary glass tube (4), make capillary glass tube (4)
Height is just in the near focal point of femtosecond laser；
2) three-dimensional mobile platform is made to move horizontally and by ccd video camera (25) observation of surface until finding light and shade mutation
Boundary position, adjusts the height of capillary glass tube (4), reaches border most clear；
3) capillary glass tube (4) is moved horizontally toward deeper direction is extended, until finding the border of another light and shade mutation, takes this
The half of the distance for moving horizontally, makes capillary glass tube (4) move from another light and shade boundary toward by-level, and now femtosecond swashs
The focus of light fall capillary glass tube (4) horizontal width center position；
The second step focusing is comprised the following steps：By the plane micro structure that one area of Computer Design is 10um × 10um,
And the three-dimensional mobile platform motion of the fixed capillary glass tube (4) of runs software control, and photoetching is carried out to capillary glass tube (4),
If the micro structure in capillary glass tube (4) is can't see in the ccd video camera of surface (25), moving three dimension mobile platform is adjusted
The height of section capillary glass tube, is raised and lowered capillary glass tube, and a 20um softwares of operation are often raised and lowered carries out light
Carve, until it can be seen that micro structure；
3rd step Jiao includes：1) raise the height of capillary glass tube (4), and often raise a 5um softwares of operation
Row photoetching, until microstructure positional can not be processed；2) height of capillary glass tube (4) and then is back gradually reduced every 1um,
Runs software carries out photoetching simultaneously, makes just process micro structure；3) move axially capillary glass tube (4).
2. the method that micro structure is prepared in capillary glass tube as claimed in claim 1, it is characterised in that：The step 1) it is concrete
It is that a small amount of photoresist is taken in dark surrounds to be placed in small beaker, will be crossed simultaneously with washes of absolute alcohol during bubble-free in the photoresist
The dry capillary glass tube (4) is inserted vertically into wherein, and stands a period of time, treats that suction is full of in capillary glass tube (4)
It is drawn off after photoresist, with the lens paper wiped clean for being moistened with dehydrated alcohol.
3. the method that micro structure is prepared in capillary glass tube as claimed in claim 1, it is characterised in that：7) wherein the step of wraps
Include by the end thereof contacts of capillary glass tube (4) on water suction napkin, using napkin by unexposed photoetching in capillary glass tube (4)
Glue is sucked out completely, and then again capillary glass tube (4) is inserted vertically in dehydrated alcohol, treats that dehydrated alcohol is full of capillary glass tube
(4) take out after and dehydrated alcohol is suctioned out with napkin again, repeatedly this step 3～4 time.
4. the method that micro structure is prepared in capillary glass tube as claimed in claim 2, it is characterised in that：The capillary glass tube
(4) length of at least 1/3rd is inserted in photoresist.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN108319113B (en) * | 2018-01-31 | 2021-01-08 | 宁波大学 | Deformation correction method for processing microstructure in glass capillary |
| CN108838546B (en) * | 2018-07-24 | 2021-01-15 | 长春理工大学 | Laser processing method for inner surface microstructure of thin-wall microtube |
| CN109188869B (en) * | 2018-09-29 | 2020-08-28 | 宁波市效实中学 | Method for preparing microstructure on opaque substrate |
| CN109336049B (en) * | 2018-10-11 | 2023-10-24 | 宁波大学 | Microstructure operation method and operation 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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|---|---|---|---|---|
| GB1567281A (en) * | 1976-08-06 | 1980-05-14 | Perkin Elmer Corp | Gaseous discharge lamp |
| EP1990638A1 (en) * | 2007-05-11 | 2008-11-12 | Koninklijke Philips Electronics N.V. | Flow-through biosensor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6782746B1 (en) * | 2000-10-24 | 2004-08-31 | Sandia National Laboratories | Mobile monolithic polymer elements for flow control in microfluidic devices |
| US8449746B2 (en) * | 2010-07-16 | 2013-05-28 | Waters Technologies Corporation | Systems and methods for coupling molecule separation devices to analytical instruments |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1567281A (en) * | 1976-08-06 | 1980-05-14 | Perkin Elmer Corp | Gaseous discharge lamp |
| EP1990638A1 (en) * | 2007-05-11 | 2008-11-12 | Koninklijke Philips Electronics N.V. | Flow-through biosensor |
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