CN109701673A - The preparation method of three-dimensional large scale high-precision microfluidic channel - Google Patents
The preparation method of three-dimensional large scale high-precision microfluidic channel Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of three-dimensional large scale high-precision microfluidic channel, inside ultra-short pulse laser direct write irradiation transparent material, generate high-precision three-dimensional microchannel pattern and several accessory channel patterns for connecting sample surfaces and internal microchannel, then the above-mentioned pattern acquisition three-dimensional dimension of selective removal is handled by wet-chemical etching and shape is unrestricted, the compound communicating structure of hollow and connection three-dimensional micro-channel and accessory channel composition, successively all accessory channel surface openings are melted finally by carbon dioxide laser, closing is to realize the controllable preparation of three-dimensional large scale high-precision three-dimensional microfluidic channel.Efficiency, quality and the overall dimensions of three-dimensional micro-channel preparation can be improved by the way that the approach of accessory channel is melted, closed using carbon dioxide laser in the present invention, manufacture suitable for the high-performance of business level and technical grade three-dimensional microflow control system and integrated.
Description
Technical field
The present invention relates to the manufacturing methods of three-dimensional micro-channel and micro-fluidic device, especially a kind of to utilize ultra-short pulse laser
The method for preparing three-dimensional large scale high-precision microfluidic channel.The present invention is suitable for business level and technical grade micro-fluidic device and answers
With equal fields.
Background technique
Microflow control technique can realize to the quick, accurate of minute yardstick fluid, controllable operating and processing have high-throughput, high
The significant advantages such as efficiency, high sensitivity and low energy consumption are currently led in chemical, bio-pharmaceuticals, medical diagnosis, photonics etc.
Domain shows important application prospect.Core cell of the microchannel as micro-fluidic chip, high-performance and multi-functional technology of preparing
Development for promoting microflow control technique is of great significance.And relative to two dimension microchannels being used widely at present, three
Dimension microchannel can provide more flexible and efficient microscale spatial fluid for the further innovation of microflow control technique and manipulate ability.
Transparent material especially silica glass material is due to its high heat resistance and chemical stability, low thermal expansion system
Number, wide spectral transmission ranges and good biocompatibility, be the substrate that is widely used at present of micro-fluidic chip and device it
One.It is ultra-short pulse laser micro Process that the most representative technology of three-dimensional micro-channel is currently prepared inside transparent material.It is logical
The pulse energy for crossing regulation focusing ultra-short pulse laser can induce the modification such as nanometer of nonlinearity inside transparent material
Grating, Microfocus X-ray tube etc., and then the flexible controllable microchannel structure of three-dimensional space configuration can be prepared by different approaches.It grinds at present
Study carefully most extensively, there are mainly two types of the technological approaches of most application prospect.A kind of approach is that liquid auxiliary ultra-short pulse laser is direct
Three-dimensional ablation transparent material.Femtosecond laser ablation porous glass material for example is assisted using water and carries out high temperature closure nano-pore
Method can realize three-dimensional dimension and the unrestricted microchannel of diameter prepare (Y. Liao, et al. Opt. Lett. 2010,
35,3225-3227), but the large scale of above-mentioned cellular glass prepares and mass production, and there are still many technological levels at present
Limitation, limit its practicalization.Another approach is rotten using the radiation-induced selective chemical of ultra-short pulse laser
Lose transparent material.This method can realize the high-performance preparation of three-dimensional homogeneity microchannel, but due to by chemical corrosion process and change
The intrinsic limitation for learning corrosive agent hardly results in length unrestricted (for example more than Centimeter Level) with the increase of etching time
Homogeneity three-dimensional micro-channel structure.To break through above-mentioned limitation, while prepare three-dimensional micro-channel preparation connection sample surfaces with
Several accessory channels of microchannel are, it can be achieved that the unrestricted homogeneity three-dimensional micro-channel of length prepares (S. Ho, et al.
Appl. Phys. A 2012, 106, 5–13;S. He, et al. Opt. Lett. 2012,37,3825-3827).
It should be noted however that the three-dimensional micro-channel of above-mentioned preparation at present mainly passes through the bonding of dimethyl silicone polymer (PDMS) film
Come realize accessory channel surface closure, the material of enclosed region is mainly PDMS film.Therefore, the stability of micro-fluidic operation
And safety is limited by PDMS film thickness and its sealing intensity between transparent material to a certain degree.This method can be fine
The micro-fluidic research applied to common laboratory level, but for be commercialized and industrialize microfluidic applications occasion especially into
Row it is some time-consuming, the continuous flow minute yardstick organic chemical reactions of condition harshness when, accessory channel enclosed region PDMS material
Chemical stability and mechanical performance will be subjected to very test, choose greatly very much so that the leakproofness of the above method and safety be caused to exist
War.Therefore, it is micro-fluidic logical for preparing three-dimensional large scale high-precision to seek a kind of accessory channel closure techniques based on new principle
Road is of great significance and practical value.
Summary of the invention
It is an object of the invention to prepare technological challenge existing for three-dimensional microflow control channel for current ultra-short pulse laser,
A kind of preparation method of three-dimensional large scale high-precision microfluidic channel is provided.
Realize that the specific technical solution of the object of the invention is as follows:
A kind of preparation method of three-dimensional large scale high-precision microfluidic channel, this method include the following steps:
Step 1: ultra-short pulse laser irradiation
Transparent material sample is fixed on a programmable high-precision three-dimensional displacement platform, by microcobjective by ultrashort pulse
Laser focuses on transparent material, and drive displacement platform moves while starting ultra-short pulse laser irradiation, inside transparent material
Middle direct write goes out the high-precision three-dimensional microchannel pattern being pre-designed and several auxiliary for connecting sample and internal microchannel
Channel pattern；
Step 2: selective chemical corrosion
Transparent material sample after ultra-short pulse laser is irradiated is put into chemical attack solution, to the three-dimensional micro-channel of direct write and
Accessory channel pattern carries out spatial selectivity erosion removal, and then obtains in transparent material sample interior with three-dimensional geometry structure
The compound communicating structure of type, length unrestricted, hollow and connection three-dimensional micro-channel and accessory channel composition.
Step 3: carbon dioxide laser irradiation
Successively single accessory channel surface opening is irradiated by focusing carbon dioxide laser, all accessory channels are in dioxy
Change melting under carbon laser irradiation, closing, to realize the controllable preparation of three-dimensional large scale high-precision microfluidic channel.
The pulse width of the ultra-short pulse laser is 10 fs-20 ps, and repetition rate is 1 kHz-60 MHz, is focused
The numerical aperture of object lens is 0.1-1.4.
The transparent material is various transparent glass, transparent crystal, transparent polymer material.
The 5-20 mol/L potassium hydroxide solution or 1-20% hydrofluoric acid that the chemical attack solution is 80-95 DEG C are molten
Liquid.
The large scale is the unidirectional or three-dimensional length of microchannel in 1-100 cm.
The high-precision is the unidirectional or three-dimensional feature width of microchannel at 10-500 μm.
Compared with prior art compared with, the present invention has the advantages that
1), the Three-dimension process ability that large scale and high-precision have both.The introducing of accessory channel can be obviously improved selective chemical erosion
The efficiency in laser modified region is carved, ultrashort pulse can be greatly improved in the shortening of etching time and the process intensification of selective etch
Laser prepares processing dimension, processing quality and the machining accuracy of three-dimensional homogeneity microfluidic channel.In principle, accessory channel is utilized
Possess high machining accuracy simultaneously in the microchannel that can get almost random length.It should be noted that original use PDMS film
The technology of accessory channel is closed, influences micro-fluidic operating effect to avoid the accessory channel of sealing from generating biggish dead volume,
The accessory channel of processing, generally at tens microns, has for processing three-dimensional large scale microfluidic channel to a certain degree apart from surface
Considerable restraint.And the present invention can be achieved to be up to mm by the technical conditions such as depth of focus etc. of regulation carbon dioxide laser melting
The accessory channel closure of grade depth, has the accessory channel technical capability for realizing closing different depth, 3-dimensional multi-layered for preparing
The preparation of large scale complexity microfluidic channel has more application advantage.
2), stably and controllable accessory channel making capacity.It can using the single accessory channel of carbon dioxide laser irradiation is focused
So that the transparent material on accessory channel periphery generates space local controllable high-temperature melting zone, transparent material generates under high temperature action
Melting migration generates closure so that accessory channel inner wall collapses.The dynamic process of accessory channel closure can be swashed by carbon dioxide
Radiation parameter of light such as irradiation power, irradiation time, focal beam spot size, the depth of focus etc. controls, the processing of channel closure
Window is stablized, and flawless is reproducible.
3), good mechanical resistance to pressure and safe and reliable microfluidic applications ability.It is molten by control carbon dioxide laser
The parameter for melting processing can realize the enclosed region of hundreds of microns thickness, and being closed at region can go deep into miniflow inside transparent material
Passage proximate is controlled, this closed area being bonded with PDMS film only has apparent area in the characteristics of transparent sample face seal
Not, the resistance to pressure in commercialization and industrialized long-time continuous flow workplace will be more excellent.Moreover, because carbon dioxide swashs
The light melting closed region material of accessory channel is from transparent material melting migration (identical as baseplate material), for miniflow
The load fluid for controlling operation has intrinsic chemical inertness, this method that closure accessory channel is bonded with PDMS film is compared,
Chemical stability, safety and reliability are more preferable, wider in the applicability of various microfluidic applications technical fields.
Detailed description of the invention
Fig. 1 is the preparation flow schematic diagram of three-dimensional large scale high-precision microfluidic channel；
Fig. 2 is the light that selective chemical corrodes the single microchannel and accessory channel that obtain after laser modified quartz glass samples
Learn microscopic cross-section figure；
Fig. 3 is the optical microphotograph sectional view of the single accessory channel closure near carbon dioxide laser melting induction microchannel；
Fig. 4 is that selective chemical corrodes the three-dimensional spiral microchannel obtained after laser modified quartz glass samples and accessory channel
Optical microphotograph sectional view；
Fig. 5 is the optical microphotograph sectional view of the accessory channel closure of carbon dioxide laser melting inducing cycloidic passage proximate.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described, but protection model of the invention should not be limited with this
It encloses.
Embodiment 1
Step 1: ultra-short pulse laser irradiation
As shown in Figure 1, taking the clean quartz glass samples having a size of the mm of mm × 2 of 100 mm × 5 and the polishing of six faces, it is fixed on
On three-D displacement platform；The central wavelength of laser is 1026 nm, and repetition rate is 250 kHz, and pulse width is 270 fs；Using
The microcobjective that numerical aperture is 0.25 focuses the modified pattern of laser direct-writing.Processed using linearly polarized light, polarization direction perpendicular to
Direct write direction.Three-dimensional U-shape microchannel pattern length ~ 80 mm of direct write are located at 300 μm of Quartz glass surfaces or less, connect sample
Multiple accessory channel pattern lengths of product surface and microchannel are 300 μm, and the spacing between accessory channel is 1 mm.Swash
The mean power of light irradiation is 800 mW, and scanning speed is 5 mm/s.
Step 2: selective chemical corrosion
It is auxiliary that quartz glass samples after laser irradiation are placed in progress ultrasonic wave in 10 mol/L potassium hydroxide solutions (85 DEG C)
Corrosion is helped until the modified region of laser spatial selectivity is all removed, to obtain the three-dimensional micro-channel of ~ 80 mm long and auxiliary
The compound communicating structure for helping channel to form.Fig. 2 is the allusion quotation that selective chemical corrosion obtains the single accessory channel near microchannel
Type sectional view, it can be seen that the introducing of accessory channel is so that the homogeneity that the diameter of preparation microchannel has been kept.
Step 3: carbon dioxide laser irradiation
Carbon dioxide laser is focused using zinc selenide (ZnSe) lens that focal length is ~ 20 cm, is successively directed at each auxiliary
The surface opening in channel is irradiated, and the mean power of irradiation is ~ 9 W, and single irradiation time is 25 s, and accessory channel is in dioxy
Change melting under carbon laser irradiation, closing, to prepare the three-dimensional U-shape microchannel of ~ 80 mm long.Fig. 3 is that carbon dioxide laser is molten
Melt induction accessory channel closure sectional view, can be observed enclosed region glassy layer thickness it is reachable ~ 156 μm.
Embodiment 2
Step 1: ultra-short pulse laser irradiation
The clean quartz glass samples having a size of the mm of mm × 2 of 20 mm × 10 and the polishing of six faces are taken, three-D displacement platform is fixed on
On；The central wavelength of laser is 1026 nm, and repetition rate is 250 kHz, and pulse width is 270 fs；Use numerical aperture for
0.25 microcobjective focuses laser, and quarter-wave plate is placed before focusing objective len and generates circularly polarized light, and then direct write is three-dimensional
Modified pattern.Helical duct pattern lateral length ~ 10 mm of direct write, pattern edge are located at 200 μ below Quartz glass surfaces
M, 300 μm of screw diameter, 500 μm of screw pitch.The single length of accessory channel of the connection sample surfaces and spiral microchannel of direct write
It is 200 μm, the spacing in adjacent two channel is 500 μm.The mean power of laser irradiation is 800 mW, scanning speed 5
mm/s。
Step 2: selective chemical corrosion
It is auxiliary that quartz glass samples after laser irradiation are placed in progress ultrasonic wave in 10 mol/L potassium hydroxide solutions (85 DEG C)
Corrosion is helped until the region that laser spatial selectivity is modified all is removed, to obtain three-dimensional spiral microchannel and accessory channel
The compound communicating structure of composition.Fig. 4 is that the typical case of three-dimensional spiral microchannel and accessory channel that selective chemical corrosion obtains cuts
Face figure, the introducing of same accessory channel is so that the homogeneity that the diameter for preparing three-dimensional spiral microchannel has had.
Step 3: carbon dioxide laser irradiation
Carbon dioxide laser is focused using zinc selenide (ZnSe) lens that focal length is ~ 20 cm, it is successively logical to each auxiliary
Road surface opening is irradiated, and the mean power of irradiation is ~ 7 W, and single irradiation time is 25 s, and accessory channel is in carbon dioxide
It melts, close under laser irradiation, to obtain the three-dimensional spiral microchannel that lateral length is ~ 10 mm.Fig. 5 is that carbon dioxide swashs
The sectional view of the multiple accessory channel closures of light melting induction three-dimensional spiral passage proximate, after carbon dioxide laser irradiation can be observed
All accessory channels are completed to be closed, and the glassy layer of enclosed region is with a thickness of ~ 85 μm.
Claims (6)
1. a kind of preparation method of three-dimensional large scale high-precision microfluidic channel, which is characterized in that this method includes the following steps:
Step 1: ultra-short pulse laser irradiation
Transparent material sample is fixed on a programmable high-precision three-dimensional displacement platform, by microcobjective by ultrashort pulse
Laser focuses on transparent material, and drive displacement platform moves while starting ultra-short pulse laser irradiation, inside transparent material
Middle direct write goes out the high-precision three-dimensional microchannel pattern being pre-designed and several auxiliary for connecting sample and internal microchannel
Channel pattern；
Step 2: selective chemical corrosion
Transparent material sample after ultra-short pulse laser is irradiated is put into chemical attack solution, to the three-dimensional micro-channel of direct write and
Accessory channel pattern carries out spatial selectivity erosion removal, and then obtains in transparent material sample interior with three-dimensional geometry structure
The compound communicating structure of type, length unrestricted, hollow and connection three-dimensional micro-channel and accessory channel composition；
Step 3: carbon dioxide laser irradiation
Successively single accessory channel surface opening is irradiated by focusing carbon dioxide laser, all accessory channels are in dioxy
Change melting under carbon laser irradiation, closing, to realize the controllable preparation of three-dimensional large scale high-precision microfluidic channel.
2. the method according to claim 1, wherein the pulse width of the ultra-short pulse laser is 10 fs-
20 ps, repetition rate are 1 kHz-60 MHz, and the numerical aperture of focusing objective len is 0.1-1.4.
3. the method according to claim 1, wherein the transparent material is various transparent glass, transparent crystalline substance
Body or transparent polymer material.
4. the method according to claim 1, wherein the 5-20 that the chemical attack solution is 80-95 DEG C
Mol/L potassium hydroxide solution or 1-20% hydrofluoric acid solution.
5. the method according to claim 1, wherein the large scale is the unidirectional or three-dimensional length of microchannel
In 1-100 cm.
6. the method according to claim 1, wherein the high-precision is the unidirectional or three-dimensional feature of microchannel
Width is at 10-500 μm.
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