CN102218595B - Method for preparing micro-fluidic chip - Google Patents

Method for preparing micro-fluidic chip Download PDF

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Publication number
CN102218595B
CN102218595B CN 201110007738 CN201110007738A CN102218595B CN 102218595 B CN102218595 B CN 102218595B CN 201110007738 CN201110007738 CN 201110007738 CN 201110007738 A CN201110007738 A CN 201110007738A CN 102218595 B CN102218595 B CN 102218595B
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thin slice
chip
femtosecond laser
micro
microchannel
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CN102218595A (en
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曲士良
李岩
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Harbin Institute of Technology
Harbin Institute of Technology Weihai
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Harbin Institute of Technology Weihai
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Abstract

The invention relates to a method for preparing a micro-fluidic chip. A glass substrate sheet is ablated by a femto-second laser; during the machining process, a cleaning solution always carries out effective cleaning on a machining part inside the sheet; heat treatment is carried out on the glass substrate sheet that is machined by the femto-second laser; after the heat treatment, the diameter of a micro-fluidic passage and the dimension of a liquid bath in the sheet are reduced; the internal surfaces of the micro-fluidic passage and the liquid bath are smooth; a PDMS (Polydimethylsiloxane) sheet is selected as a connecting body; the position on the PDMS sheet corresponding to the longitudinal passage opening position of a micro-fluidic glass chip is bored; and subsequently the PDMS sheet is bonded with the micro-fluidic glass chip, thereby obtaining the micro-fluidic chip. The method has simple machining process and ensures that the laser can carry out continuously stable ablation on substration material; and the integrated micro-fluidic chip with complex and multi-layer structures can be prepared in the glass substrate. The prepared micro-fluidic chip has the characteristics of miniaturization and integration, has the functions of separation, reaction and detection, and can be widely applied to the analysis fields.

Description

A kind of preparation method of micro flow chip
Technical field
The present invention relates to a kind of ultrafast laser micro-processing technology, specifically a kind of preparation method of micro flow chip.It utilizes femtosecond laser ablation preparation micro flow chip.
Technical background
Micro flow chip is the core of micro-analysis system, the invention of micro flow chip impels the analytical instrument that is applied to chemistry, food, environment, medical science and life science to develop to microminiaturization, robotization, integrated and portability direction, its advantage is to detect various chemical reactions by micro flow chip, significantly reduce reagent consumption, and improved analysis efficiency greatly, the reduction expense.Design and produce the micro flow chip of forming with the microchannel network and can be applied to different analysis fields, comprise multiple fields such as chemical analysis, food hygiene, environmental monitoring, medical science chemical examination, life science, criminal science and national defence.
The main material of making micro flow chip has quartz, glass and superpolymer etc.Use superpolymer to make micro flow chip and have advantage easy to prepare, but the structural stability of superpolymer is poor, can not satisfy the requirement of long-term detection.It is good to have structural stability at glass and quartz glass internal production micro flow chip, advantages such as long service life, but its traditional preparation process complex process, and the chip microchannel network is single.Utilize superpolymer to make micro flow chip and mainly adopt methods such as photoetching, ion beam etching and multi-photon absorption, these method for makings are complex process but also costly not only, and this kind micro flow chip rests on the laboratory applications stage mostly.Adopt laser and femtosecond laser directly to write out the laser ablation zone in medium inside mostly at the glass of silicon base medium and the traditional preparation process method of quartz glass internal production micro flow chip, through forming passage in the laser ablation zone behind the hf etching, the openend diameter that there is passage mostly in the method for this making micro flow chip is obviously greater than the diameter of passage zone line, and this method for making has very big restriction to structure, passage length and the base material of channel network.
The method for preparing at present micro flow chip mainly adopts photoetching and chemical etching, as patent ZL 200610019354.6 and patent ZL 200510019720.3.The main material that uses has quartz, glass and superpolymer etc., use superpolymer to make the method that micro flow chip adopts the photoetching preparation mostly, this preparation method has the advantage of preparation high-quality micro flow chip, but the structural stability of superpolymer is poor, can not satisfy requirement and the complicated cost height of photoetching process of long-term use.Mainly adopt the chemical etching method preparation at glass and quartz glass internal production micro flow chip, it is good that matrix material has structural stability, advantages such as long service life.Many scientific workers use femtosecond laser to prepare three-dimensional micro flow chip in silica-based transparent medium inside such as quartz by the mode of directly writing continuous the exploration in recent years, but limited by technological means, the micro flow chip that can't prepare large-size, because the method that traditional technology of preparing is mainly used femtosecond laser directly to write and used hf etching then prepares, preparation large scale micro flow chip the time hf etching time also can increase, major defect is micro flow chip openend and hydrofluorite duration of contact longly to cause the open ended passage diameter obviously greater than inner passage diameter, causes chip quality to descend.
Summary of the invention
Technical matters to be solved by this invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of processing simple, the efficient height, has the good optical processing characteristics, chemical stability is good, good reproducibility, and the ablation effect is continual and steady, and can clean microchannel effectively, the preparation method of the micro flow chip of the powder that the discharge laser ablation produces.This method can prepare the micro flow chip that two and three dimensions has specific function at the glass basis material internal.
The technical scheme that the present invention solves the problems of the technologies described above employing is: a kind of preparation method of micro flow chip is characterized in that concrete steps are as follows:
(1) choose the glass basis material, cut into the thick thin slice of 1 ~ 5mm, polishing is fixed on the thin slice after the polishing on the three-dimensional platform;
(2) below thin slice on the three-dimensional platform, install one and be used for auxiliary femtosecond laser ablation glass basis material and the liquid wash device that cleans microchannel, described liquid wash device mainly comprises a rubber hose and a pump, rubber hose one end port closely contacts with the lower surface of thin slice, and the other end connects pump;
(3) utilize femtosecond laser ablation glass basis thin slice, at first promote pump, make cleaning fluid outflow and contact thin slice lower surface in the rubber hose, simultaneously femtosecond laser is focused on the thin slice lower surface of rubber hose port center correspondence, by femtosecond laser processing vertical passage opening, the moving three dimension platform is processed microchannel and liquid pool by femtosecond laser in thin slice inside then; In whole process, cleaning fluid enters microchannel and the liquid pool of thin slice inside by the vertical passage opening, by the taking out, annotate of pump control cleaning fluid, is used for auxiliary femtosecond laser ablation glass basis material and clean microchannel and liquid pool;
(4) the glass basis thin slice after the above-mentioned femtosecond laser processing is heat-treated, the microchannel diameter of thin slice inside and liquid pool size are dwindled, the inside surface of microchannel and liquid pool is smooth, prepares the miniflow glass-chip;
(5) choose the PDMS thin slice as connector, on the PDMS thin slice, with respect to the punching of miniflow glass-chip vertical passage aperture position place, then with PDMS thin slice and miniflow glass-chip bonding, obtain micro flow chip.
Cleaning fluid of the present invention is deionized water or distilled water or pure class I liquid I or hydrofluorite.
Femtosecond laser of the present invention is pulse width 50fs ~ 500fs (10 -15Second) ultra-short pulse laser between.
Heat treatment process of the present invention is the softening temperature that the glass basis thin slice after the femtosecond laser processing is heated to the glass basis material, is incubated 0 ~ 10 minute, naturally cools to room temperature then.Make the yardstick that dwindles of the inner microchannel diameter of thin slice and liquid pool, the inside surface of microchannel and liquid pool polishes.
The present invention utilizes femtosecond laser ablation glass basis thin slice, cleaning fluid effectively cleans the working position of thin slice inside all the time in the process, against existing technologies, processing technology of the present invention is simple, can effectively clean microchannel, the powder that laser ablation produces is discharged, guaranteed that laser can be to the continual and steady ablation effect of matrix material.Can be at the integrated micro flow chip of glass basis inner preparation labyrinth and sandwich construction.Selected glass basis material has the good optical processing characteristics, and chemical stability is good, and liquid pool and microchannel have good reproducibility, characteristics such as easy processing.The micro flow chip of preparation has microminiaturization, integrated characteristics, has separation, reaction and measuring ability, can be widely used in analysis field.Micro flow chip is one-piece construction, after the external linkage sterile device, can realize the gnotobasis of totally-enclosed, and light transmission is good, can use optical instrument to carry out life science research.
Embodiment
The present invention is further described below in conjunction with embodiment.
A kind of preparation method of micro flow chip, its concrete steps are:
(1) chooses the quartz substrate material, matrix material is cut into the thick thin slice of 3mm, polishing, quartzy thin slice after the polishing is fixed on the anchor clamps, anchor clamps are fixed on circular glass plate bottom, guarantee quartzy thin slice upper and lower surface level, then circular glass plate and quartzy thin slice etc. are fixed on the three-dimensional platform together.
(2) below thin slice on the three-dimensional platform, install one and be used for auxiliary femtosecond laser ablation glass basis material and the liquid wash device that cleans microchannel, described liquid wash device mainly comprises a rubber hose and a pump, rubber hose one end port closely contacts with the lower surface of thin slice, closely push quartzy thin slice lower surface, the other end connects pump; Pump can be an injector for medical purpose, and syringe inside is full of the cleaning fluid for auxiliary laser ablation and cleaning microchannel.Described cleaning fluid is deionized water or distilled water or pure class I liquid I or hydrofluorite.
(3) utilize femtosecond laser ablation glass basis thin slice, pushing syringe at first, make cleaning fluid outflow and contact thin slice lower surface in the rubber hose, simultaneously femtosecond laser is focused on the thin slice lower surface of rubber hose port center correspondence, laser frequency and energy are set to 1kHz and 6mW respectively, use 20 *, the NA=0.45(numerical aperture) condenser lens is with femtosecond laser incident and focus on the quartzy thin slice lower surface in rubber hose center directly over the quartzy thin slice, shutter is opened, by femtosecond laser processing vertical passage opening, the degree of depth is 800 μ m.The moving three dimension platform is processed microchannel and liquid pool by femtosecond laser in thin slice inside then; Carry out program setting according to the micro flow chip design pattern, can realize automatic control behind the program start.Start-up routine control platform moves, shutter is opened, femtosecond laser begin to ablate quartz substrate and produce powdered, preparation is parallel to the microchannel of quartzy thin slice lower surface, the microchannel diameter is 60 μ m, according to the micro flow chip design pattern, can prepare the shaped form microchannel by the mode that changes the laser scanning route.
In whole process, cleaning fluid enters microchannel and the liquid pool of thin slice inside by the vertical passage opening, by the taking out, annotate of pump control cleaning fluid, is used for auxiliary femtosecond laser ablation glass basis material and clean microchannel and liquid pool.In the microchannel preparation process, growth along with passage length, thereby fresh deionized water admission passage is inner to make femtosecond laser can't continue the quartz substrate of ablating because a large amount of accumulation of powder can stop in channel interior, therefore change the pressure of rubber hose inside by the syringe of the continuous push-and-pull connection of machinery control rubber hose, thereby make the rubber hose air entrapment under the situation that pressure changes, bubble volume recurs the powder passing away outside that variation is ablated femtosecond laser to produce, reach the purpose of cleaning microchannel, and fresh deionized water is injected into microchannel inside, make the femtosecond laser quartz substrate materials increases microchannel that can continue to ablate.Must keep the upper surface drying of quartzy thin slice in whole process, because under the situation that has water to exist, the position that the water evaporation can make refractive index change and make laser focus on quartzy inside changes, thereby the micro flow chip quality of preparation is descended.
(4) the glass basis thin slice after the above-mentioned femtosecond laser processing is heat-treated, concrete thermal treatment is that quartzy thin slice is placed in the electric furnace, temperature is raised to 755 ℃, stop heating then immediately, temperature in the electric furnace is cooled to room temperature naturally, also can the interior temperature of electric furnace be raised to 740 ℃ of insulations after 10 minutes, cool to room temperature naturally and take out.Microchannel diameter and the liquid pool size of thin slice inside are dwindled, and diameter is that to become xsect be the microchannel of 10 μ m for circular diameter to the microchannel of 60 μ m.The inside surface of microchannel and liquid pool is smooth, prepares the miniflow glass-chip.
(5) choose the PDMS thin slice as connector, with respect to the punching of miniflow glass-chip vertical passage aperture position place, then the bonding under 80 ℃ of conditions with PDMS thin slice and miniflow glass-chip obtains micro flow chip on the PDMS thin slice.
A plurality of rubber hose also can be fixed in the quartzy thin slice of the present invention below, prepare the quartz chip with a plurality of openings by the above preparation method.
Femtosecond laser of the present invention is pulse width 50fs ~ 500fs (10 -15Second) ultra-short pulse laser between.
Thermal treatment of the present invention is the softening temperature that the glass basis thin slice after the femtosecond laser processing is heated to the glass basis material, is incubated 0 ~ 10 minute, naturally cools to room temperature then.Make the yardstick that dwindles of the inner microchannel diameter of thin slice and liquid pool, the inside surface of microchannel and liquid pool polishes.
Processing technology of the present invention is simple, can effectively clean microchannel, and the powder that laser ablation produces is discharged, and has guaranteed that laser can be to the continual and steady ablation effect of matrix material.Can be at the integrated micro flow chip of glass basis inner preparation labyrinth and sandwich construction.Selected glass basis material has the good optical processing characteristics, and chemical stability is good, and liquid pool and microchannel have good reproducibility, characteristics such as easy processing.The micro flow chip of preparation has microminiaturization, integrated characteristics, has separation, reaction and measuring ability, can be widely used in analysis field.Micro flow chip is one-piece construction, after the external linkage sterile device, can realize the gnotobasis of totally-enclosed, and light transmission is good, can use optical instrument to carry out life science research.

Claims (4)

1. the preparation method of a micro flow chip is characterized in that concrete steps are as follows:
(1) choose the glass basis material, cut into the thick thin slice of 1 ~ 5mm, polishing is fixed on the thin slice after the polishing on the three-dimensional platform;
(2) below thin slice on the three-dimensional platform, install one and be used for auxiliary femtosecond laser ablation glass basis material and the liquid wash device that cleans microchannel, described liquid wash device mainly comprises a rubber hose and a pump, rubber hose one end port closely contacts with the lower surface of thin slice, and the other end connects pump;
(3) utilize femtosecond laser ablation glass basis thin slice, at first promote pump, make cleaning fluid outflow and contact thin slice lower surface in the rubber hose, simultaneously femtosecond laser is focused on the thin slice lower surface of rubber hose port center correspondence, by femtosecond laser processing vertical passage opening, the moving three dimension platform is processed microchannel and liquid pool by femtosecond laser in thin slice inside then; In whole process, cleaning fluid enters microchannel and the liquid pool of thin slice inside by the vertical passage opening, by the taking out, annotate of pump control cleaning fluid, is used for auxiliary femtosecond laser ablation glass basis material and clean microchannel and liquid pool;
(4) the glass basis thin slice after the above-mentioned femtosecond laser processing is heat-treated, the microchannel diameter of thin slice inside and liquid pool size are dwindled, the inside surface of microchannel and liquid pool is smooth, prepares the miniflow glass-chip;
(5) choose the PDMS thin slice as connector, on the PDMS thin slice, with respect to the punching of miniflow glass-chip vertical passage aperture position place, then with PDMS thin slice and miniflow glass-chip bonding, obtain micro flow chip.
2. according to the preparation method of the described micro flow chip of claim 1, it is characterized in that: described cleaning fluid is deionized water or distilled water or pure class I liquid I or hydrofluorite.
3. according to the preparation method of the described micro flow chip of claim 1, it is characterized in that: described femtosecond laser is pulse width 50fs ~ 500fs (10 -15Second) ultra-short pulse laser between.
4. according to the preparation method of the described micro flow chip of claim 1, it is characterized in that: described thermal treatment is the softening temperature that the glass basis thin slice after the femtosecond laser processing is heated to the glass basis material, is incubated 0 ~ 10 minute, then cool to room temperature.
CN 201110007738 2011-01-14 2011-01-14 Method for preparing micro-fluidic chip Expired - Fee Related CN102218595B (en)

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CN102789884B (en) * 2012-06-21 2014-07-02 西安交通大学 Preparation method of solenoid micro-inductor inside quartz material
CN105396631B (en) * 2015-12-11 2017-08-25 武汉纺织大学 A kind of three-dimensional micro-fluidic chip and preparation method thereof
CN108527744B (en) * 2017-03-03 2021-03-30 南开大学 Controllable nano material synthesis reactor based on microfluidic chip

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