CN110902647A - Method for manufacturing nano channel with gradually changed size - Google Patents
Method for manufacturing nano channel with gradually changed size Download PDFInfo
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- CN110902647A CN110902647A CN201911234646.5A CN201911234646A CN110902647A CN 110902647 A CN110902647 A CN 110902647A CN 201911234646 A CN201911234646 A CN 201911234646A CN 110902647 A CN110902647 A CN 110902647A
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- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
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- B81—MICROSTRUCTURAL TECHNOLOGY
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- B81C2201/00—Manufacture or treatment of microstructural devices or systems
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Abstract
The invention provides a method for manufacturing a nano channel with gradually changed size, which comprises the following steps: manufacturing a nano line structure template: coating a first photoresist on the surface of one side of a first quartz glass substrate; then, carrying out holographic exposure, and developing after the exposure is finished until a nano line structure appears on the photoresist; carrying out ion beam etching on the developed photoresist I under the protective gas, and removing the photoresist after etching to obtain a nano line structure template; nano-imprint transfer of nano-line structures on a template: coating a second photoresist on the second quartz glass substrate; coating a release agent on the nano line structure template, pressing the nano line structure template into a second photoresist, and carrying out ultraviolet exposure until the nano line structure on the template is transferred to the second photoresist; after the transfer is finished, modifying and curing the photoresist II, and removing the nano line structure template; dividing the nano line structure area on the nano line structure substrate into a plurality of parts, and sequentially carrying out silicon dioxide film deposition at gradually changed angles one by one.
Description
Technical Field
The invention relates to a manufacturing method of a nano channel, in particular to a manufacturing method of a nano channel with gradually changed size.
Background
The micro-nano flow control chip can shrink basic operations such as sample preparation, biochemical reaction, separation, detection and the like related in the fields of biology, chemistry and the like to a substrate with the size of dozens of square centimeters. By designing a proper micro-nano channel structure, fluid can flow in a channel according to a certain mode, so that the chip can obtain a specific function on the whole. However, as the size of the channel decreases, the influence of the size effect will increase, and the fluid in the micro-nano channel will have some special properties different from those of the macro fluid. For example, when the channel size reaches the nanometer scale, quantum effects, interfacial effects, and nanoscale effects will be non-negligible. Nanochannel based fluidic systems are therefore of increasing interest.
Nanofluidic systems were utilized and studied, provided that nanochannels were fabricated. The traditional method for manufacturing the nano-channel is to manufacture a polymer micro-nano groove structure by technologies such as nano-imprinting, mask plate photoetching or electron beam direct writing, and then realize top sealing of the channel by combining a thermal bonding technology. The thermal bonding technology is a technology for forming a channel by heating and adhering a bonding layer to a micro-nano groove to seal the top of the groove. Under the action of external pressure, the high polymer bonding layer with the temperature higher than the glass state temperature realizes entanglement of the sub-chains at the interface through infiltration and bonding, and realizes close interface contact. Fig. 1 is a simplified flow diagram of a conventional thermal bonding technique. However, the polymer in the molten state inevitably flows into the interior of the channel strand structure during bonding. As the size of the fabricated channel decreases, especially when the size reaches the nanometer level, the bonding method is very likely to cause channel blockage, which adversely affects the precise control of the channel size and the process reliability. Therefore, the existing thermal bonding method is mainly used for manufacturing channels with micron and above sizes.
In addition, when the size reaches the nanometer level, it is difficult to guide a substance or a particle to be studied into the nanochannel due to the small size of the channel when some biochemical experiments are performed using the nanochannel. For example, when DNA stretching experiments are required, it is difficult to guide DNA particles into nanochannels due to their snaking into clusters. If a graded nanochannel can be created with channel sizes that taper from large to small, the particles can enter the large channel first and then the small channel. This helps to guide the particles into the nanochannel, however, there is no similar process in the conventional processing methods.
Disclosure of Invention
In view of the above, there is a need to provide a method for fabricating a nanochannel with gradually changed dimensions, which is directed to the problems of the conventional nanochannel fabrication process. The technical scheme of the invention is as follows:
in a first aspect, the present invention provides a method for fabricating a size-graded nanochannel, comprising the steps of:
step 1, manufacturing a nano line structure template;
step 1.1, coating a first photoresist on the surface of one side of a first quartz glass substrate;
step 1.2, performing holographic exposure on the first photoresist, and developing after the exposure is finished until a nano line structure appears on the first photoresist;
step 1.3, performing ion beam etching on the developed photoresist I under protective gas, and removing the photoresist after etching to obtain a nano line structure template;
step 2, nanoimprinting the nanowire strip structure on the transfer template;
step 2.1, coating a second photoresist on a second quartz glass substrate;
step 2.2, coating a release agent on the nano line structure template obtained in the step 1, pressing the nano line structure template into a second photoresist, and carrying out ultraviolet exposure on the second photoresist until the nano line structure on the template is transferred onto the second photoresist;
step 2.3, after the transfer is finished, modifying and curing the photoresist II, and removing the nano line structure template to obtain a nano line structure substrate;
and 3, dividing the nano line structure area on the nano line structure substrate into a plurality of parts, and sequentially depositing the silicon dioxide films on the surface of each part of the nano line structure one by one at a gradual change angle to form a nano channel with a gradual change size.
Preferably, in step 1.1, the conditions for coating the first photoresist are as follows: the rotating speed of the spin coater is 1000-2000 r/min, the time is 30s, the coating thickness is 180-220 nm, and the temperature is kept at 90 ℃ for 30 min.
Optionally, the first photoresist is AZ701 photoresist.
Preferably, in step 1.2, the holographic exposure conditions are as follows: the exposure time is 4-5 minutes; wavelength 442m, intensity 130 mw. Holographic lithography adopts a laser with a certain wavelength as a light source, expands the beam through a spatial filter, filters and finally forms interference fringes by adopting a Laue lens light path. After exposure of the photoresist, the photoresist records the interference fringe information. For the interference of two light waves, the fringe spacing or period is determined by (λ/2)/sin (θ/2), where λ is the wavelength and θ is the angle between the two coherent light waves. By changing the included angle of the two interference beams on the surface of the sample or the laser wavelength, photoresist line patterns with different periods can be manufactured.
Furthermore, the width-depth ratio of the channel etched in the step 1.3 is 1 (2-2.5).
Further, in the step 2.1, the conditions for coating the second photoresist are as follows: the rotating speed of the spin coater is firstly 600r/min for 9 seconds, then 2000r/min for 60 seconds, the coating thickness is 2-2.5 mu m, and the temperature is kept at 90 ℃ for 10 minutes.
Optionally, the second photoresist is SU-82002 photoresist.
Optionally, in the step 2.2, the release agent is formed by mixing an organosilicon release agent and isopropanol according to a volume ratio of 1: 200.
Preferably, in step 2.2, the conditions of the ultraviolet exposure are as follows: the exposure time is 2 minutes, and the exposure dose is 200mJ/cm2。
Preferably, in the step 2.3, the conditions for modifying and curing are as follows: the temperature is 90 deg.C and the time is 10 min.
Further, the gradient angle range in the step 3 is 25-80 ℃.
In a second aspect, the present invention provides a nanochannel with gradually changed dimensions, which is fabricated by the above-mentioned fabrication method.
The invention has the beneficial effects that: the invention firstly utilizes the holographic photoetching method to make a template with a nano line structure which is in line with expectation, then transfers the nano line structure on the template to the photoresist of another substrate, then releases the mold, and then realizes the sealing of a nano channel by a mode of depositing a film. The method has the advantages that the nano channel with gradually changed size can be obtained, and the problem that the channel is easy to block in the traditional channel sealing method is solved. In addition, the method can also solve the problem of connection between the large nanochannel and the small nanochannel, and is beneficial to smoothly introducing the nano particles to be detected into the nanochannel, thereby facilitating other biochemical analysis and expanding the application range of the method.
Drawings
Fig. 1 is a simplified process flow diagram of a conventional thermal bonding process, in which a) indicates spin-coating a polymer on a substrate, b) indicates a prepared micro-nano pattern, and c) indicates thermal bonding.
Fig. 2 is a schematic view of a process for manufacturing a template with a nanowire structure in embodiment 1 of the present invention.
Fig. 3 is a schematic view of a process for fabricating a nano-line structure on a nano-imprint transfer template in embodiment 1 of the present invention.
Fig. 4 is a schematic structural diagram of a first partial shielding and channel sealing by performing thin film deposition at an angle θ 1 of 25 ° in embodiment 1 of the present invention, where 4-1 is a schematic structural diagram of shielding the remaining portion, and 4-2 is a schematic structural diagram of performing silicon dioxide deposition at a plating angle θ 1.
Fig. 5 is a schematic structural view of a second partial shielding and channel sealing by a film deposition performed at an angle θ 2 of 35 ° in embodiment 1 of the present invention, where 5-1 is a schematic structural view of shielding the remaining portion, and 5-2 is a schematic structural view of performing a silicon dioxide deposition at a film deposition angle θ 1.
Fig. 6 is a schematic structural view of a third partial shielding and a channel sealing by a thin film deposition at an angle θ 3 of 45 ° in embodiment 1 of the present invention, where 6-1 is a schematic structural view of shielding the remaining portion, and 6-2 is a schematic structural view of a silicon dioxide deposition at a plating angle θ 1.
Fig. 7 is a schematic structural diagram of a fourth shielding part and a channel sealed by performing thin film deposition at an angle θ 4 of 60 ° in embodiment 1 of the present invention, where 7-1 is a schematic structural diagram of shielding the remaining part, and 7-2 is a schematic structural diagram of performing silicon dioxide deposition at a plating angle θ 1.
Fig. 8 is a schematic structural view of a sealing channel of gradually changing size finally obtained in example 1 of the present invention.
Fig. 9 is a schematic structural view of a first partial shadow and a channel sealed by a thin film deposition performed at an angle θ 1 of 20 ° in comparative example 2 of the present invention.
Fig. 10 is a schematic structural view of the fourth partial shadow of comparative example 3 of the present invention and the channel is sealed by the thin film deposition performed at an angle θ 4 of 85 °.
Detailed Description
In the description of the present invention, it is to be noted that those whose specific conditions are not specified in the examples are carried out according to the conventional conditions or the conditions recommended by the manufacturers. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
The embodiment provides a method for manufacturing a nano channel with gradually changed size, which comprises the following steps:
step 1, manufacturing a nano line structure template; the manufacturing process is shown in fig. 2.
Step 1.1, taking a piece of quartz glass with high light transmittance and smooth surface as a substrate, cleaning the quartz glass with clear water and acetone, placing the quartz glass in an oven, and baking the quartz glass at 130 ℃ for 10 minutes to remove water vapor and residual acetone. After natural cooling, the mixture is placed into an ashing machine for ashing for one hour to enhance the surface adhesion. And then coating a layer of tackifier (AZAD PROMOTER tackifier) on the quartz surface through a spin coater to increase the substrate viscosity and prevent the photoresist from degumming during development. The rotating speed of the spin coater is 1500r/min, the time is 30s, the mixture is placed in an oven, and the temperature is kept at 90 ℃ for 10 minutes;
step 1.2, after the quartz substrate is pretreated, coating AZ701 photoresist on the quartz substrate, wherein the photoresist is prepared by using a special diluent (AZ 1500 Thinner diluent) according to the volume ratio of 1: 5, the spin-coating method is adopted, so that the spin-coated back glue layer is thinner, and the subsequent exposure and the development are facilitated. The rotating speed of the spin coater is 1000r/min, the time is 30s, and the photoresist thickness is about 200 nm; it was then placed in an oven at 90 ℃ for 30 minutes to completely remove excess solvent;
step 1.3, carrying out holographic exposure on the substrate for 4 minutes; wavelength 442, light intensity 130 mw. Holographic lithography adopts a laser with a certain wavelength as a light source, expands the beam through a spatial filter, filters and finally forms interference fringes by adopting a Laue lens light path. After exposure of the photoresist, the photoresist records the interference fringe information. For the interference of two light waves, the fringe spacing or period is determined by (λ/2)/sin (θ/2), where λ is the wavelength and θ is the angle between the two coherent light waves. By changing the included angle of the two interference beams on the surface of the sample or the laser wavelength, photoresist line patterns with different periods can be manufactured. The nanowire manufactured in this example is 1500 wires, that is, the nanowire structure period is 667 nm;
step 1.4, after exposure, placing the substrate into NaOH solution with the mass percent of 5 per mill for development, wherein the development time is 1 minute and 10 seconds; the nanowire structure will appear on the substrate;
step 1.5, flushing with deionized water after the development is finished, and drying with nitrogen;
step 1.6, the substrate is placed in an ion beam etching machine, ion beam etching is carried out under the environment of trifluoromethyl alkane (CF3) and argon, the etching depth of the embodiment is 160nm, the width of the embodiment is 333nm, and therefore the aspect ratio of the channel manufactured by the embodiment is about 1: 2.
And step 1.7, removing the protected photoresist by using acetone to finally obtain the template with the expected nano line structure.
Step 2, nanoimprinting the nanowire strip structure on the transfer template; the manufacturing process is shown in fig. 3.
And 2, pressing the nano-line structure template manufactured in the step 1 into SU-8 by using glass as a substrate and SU-8 as a transfer-printed photoresist material, and carrying out ultraviolet exposure, wherein the whole SU-8 is exposed and cured because the quartz template is transparent, so that the nano-line structure is transferred onto the SU-8 photoresist. The purpose and the function of transferring the nano line structure to the photoresist are two, so that the cost can be saved, and the original template can be recycled. Secondly, the channel is sealed by a thin film deposition mode at the later stage of the embodiment, the adhesion force of the deposited thin film material and the photoresist is stronger, and the structural strength of the manufactured channel is better. The specific process steps are as follows:
step 2.1, taking another piece of flat glass as a substrate, cleaning the substrate with clear water and acetone, placing the substrate in a baking oven, baking the substrate at 130 ℃ for 10 minutes to remove water vapor and residual acetone, naturally cooling the substrate, and then placing the substrate in an ashing machine for ashing for 1 hour to enhance the surface adhesion of the substrate;
and 2.2, pre-treating the quartz substrate, and coating SU-82002 photoresist on the quartz substrate. The rotating speed of the spin coater is firstly 600r/min for 9 seconds, then 2000r/min for 60 seconds, and the thickness of the glue layer is about 2.5 μm. Placing the silicon wafer on a hot bench, baking for 10min at 90 ℃, and removing the organic solvent of SU-8;
and 2.3, spin-coating a release agent on the substrate, so that the later template can be conveniently separated from SU-8. The release agent is a mixed solution of Dow Corning organosilicon release agent DC-20 and isopropanol, and the volume ratio of DC 20: 1-isopropyl alcohol: 200 and mixing. After the template is cleaned and dried, spin-coating a release agent at the rotating speed of 2000rpm, wherein the release agent can form a monomolecular layer on the surface of the substrate;
and 2.4, placing the substrate coated with the release agent in an ultraviolet exposure machine for exposure for 2 minutes, wherein the exposure dose is 200mJ/cm2, and postbaking the exposed SU-8 photoresist to enable the SU-8 photoresist to be modified and cured, wherein the postbaking temperature is 90 ℃ and the postbaking time is 10 minutes. After SU-8 is exposed and cured, the surface energy is lowered, and the later demolding is facilitated.
And 2.5, separating the imprinting template after SU-8 is cured. Finally, the nanowire structures were transferred to SU-8 gel. The demolding process should be carried out below the glass transition temperature of the polymer.
Step 3, manufacturing a size-gradient nano channel; the step is to realize the manufacture of the size-gradually-changed nano channel by shielding and changing the angle of the coating. Therefore, on one hand, the problem that the traditional channel sealing process easily causes channel blockage can be solved, and meanwhile, the size of the channel can be controlled by changing the coating angle. The process method comprises the following steps:
step 3.1, before film coating, the SU-8 nanowire structure is treated by oxygen plasma to remove the release agent remained on the substrate brought by the template, and simultaneously, the surface energy of SU-8 can be improved, and SU-8 and silicon dioxide (SiO) deposited subsequently are enhanced2) The bonding force between the films;
step 3.2, dividing the nano-line structure area on the manufactured nano-line structure substrate into 4 parts, sequentially depositing silicon dioxide films, blocking the rest part by a baffle plate when depositing one part of the silicon dioxide films, as shown in fig. 4 to 7, placing the substrate in a magnetron sputtering coating machine, adjusting the angle between the substrate and a target material, and using the angle (theta 1-25 degrees) to enable silicon dioxide (SiO)2) The thin film is deposited on the first portion of the substrate at a greater angle in the portion of the channel near the entrance of the channel, so that the channel formed by the coated seal is relatively larger in size. Here, SiO is used2As the coating material is a transparent material, the condition inside the channel can be observed conveniently, and the coating material is convenient to be applied to other chemical and biological experiments. Then, the second portion is blocked, and as shown in fig. 5, the plating angle (θ 2 ═ 35 °) is adjusted again to be smaller, so that the size of the channel formed by sealing is relatively smaller. Repeating the above steps, as shown in fig. 6 and 7, blocking the third portion and the fourth portion, and changing the film deposition angle (θ 3 ═ 45 °, θ 4 ═ 60 °), so as to finally fabricate the nanochannel with gradually changed width. The width of the fabricated channel (one of which is shown in fig. 8) gradually changes from a to b, then to c, and finally to d from the inlet to the outlet, wherein a, b, c, and d are about 330nm, 220nm, 160nm, and 90 nm.
Comparative example 1
The present embodiment provides a method for manufacturing a size-graded nanochannel, which is different from embodiment 1 in that: and 3, bonding sealing is adopted, namely a layer of cover plate is covered on the substrate obtained in the step 2 for sealing, and finally, only a channel with one size can be obtained.
Comparative example 2
The present embodiment provides a method for manufacturing a size-graded nanochannel, which is different from embodiment 1 in that: θ 1 is 20 °. As a result, an irregular pattern is formed due to reflection of deposited particles, etc., and the channel size becomes uncontrollable, as shown in fig. 9. Therefore, the minimum plating angle when the channel sealing is performed by the deposition method cannot be less than 25 °.
Comparative example 3
This comparative example provides a method for fabricating a nanochannel with gradually varying dimensions, the difference from example 1 being: θ 4 is 85 °. As a result, channel clogging occurs at the time of the fourth partial deposition, as shown in fig. 10, presumably due to a series of causes such as collision, scattering, and the like between particles, and in any case, the final result is that if the deposition maximum angle is larger than 80 °, channel closure failure is caused.
In summary, the invention firstly uses the holographic lithography method to make the template with the expected nano-line structure, then transfers the nano-line structure on the template to the photoresist of another substrate, then releases the mold, and then realizes the sealing of the nano-channel by depositing the film. The method has the advantages that the nano channel with gradually changed size can be obtained, and the problem that the channel is easy to block in the traditional channel sealing method is solved. In addition, the method can also solve the problem of connection between the large nanochannel and the small nanochannel, and is beneficial to smoothly introducing the nano particles to be detected into the nanochannel, thereby facilitating other biochemical analysis and expanding the application range of the method.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for manufacturing a nanochannel with gradually changed size is characterized in that: the method comprises the following steps:
step 1, manufacturing a nano line structure template;
step 1.1, coating a first photoresist on the surface of one side of a first quartz glass substrate;
step 1.2, performing holographic exposure on the first photoresist, and developing after the exposure is finished until a nano line structure appears on the first photoresist;
step 1.3, performing ion beam etching on the developed photoresist I under protective gas, and removing the photoresist after etching to obtain a nano line structure template;
step 2, nanoimprinting the nanowire strip structure on the transfer template;
step 2.1, coating a second photoresist on a second quartz glass substrate;
step 2.2, coating a release agent on the nano line structure template obtained in the step 1, pressing the nano line structure template into a second photoresist, and carrying out ultraviolet exposure on the second photoresist until the nano line structure on the template is transferred onto the second photoresist;
step 2.3, after the transfer is finished, modifying and curing the photoresist II, and removing the nano line structure template to obtain a nano line structure substrate;
and 3, dividing the nano line structure area on the nano line structure substrate into a plurality of parts, and sequentially depositing the silicon dioxide films on the surface of each part of the nano line structure one by one at a gradual change angle to form a nano channel with a gradual change size.
2. The method of claim 1, wherein the step of fabricating the nanochannel with gradually changed dimensions comprises: in the step 1.1, the conditions for coating the first photoresist are as follows: the rotating speed of the spin coater is 1000-2000 r/min, the time is 30s, the coating thickness is 180-220 nm, and the temperature is kept at 90 ℃ for 30 min.
3. The method of claim 1, wherein the step of fabricating the nanochannel with gradually changed dimensions comprises: in the step 1.2, the holographic exposure conditions are as follows: the exposure time is 4-5 minutes; wavelength 442m, intensity 130 mw.
4. The method of claim 1, wherein the step of fabricating the nanochannel with gradually changed dimensions comprises: the width-depth ratio of the channel etched in the step 1.3 is 1 (2-2.5).
5. The method of claim 1, wherein the step of fabricating the nanochannel with gradually changed dimensions comprises: in the step 2.1, the conditions for coating the second photoresist are as follows: the rotating speed of the spin coater is firstly 600r/min for 9 seconds, then 2000r/min for 60 seconds, the coating thickness is 2-2.5 mu m, and the temperature is kept at 90 ℃ for 10 minutes.
6. The method of claim 1, wherein the step of fabricating the nanochannel with gradually changed dimensions comprises: in the step 2.2, the release agent is formed by mixing an organic silicon release agent and isopropanol according to the volume ratio of 1: 200.
7. The method of claim 1, wherein the step of fabricating the nanochannel with gradually changed dimensions comprises: in the step 2.2, the ultraviolet exposure conditions are as follows: the exposure time is 2 minutes, and the exposure dose is 200mJ/cm2。
8. The method of claim 1, wherein the step of fabricating the nanochannel with gradually changed dimensions comprises: in the step 2.3, the conditions of modification and curing are as follows: the temperature is 90 deg.C and the time is 10 min.
9. The method of claim 1, wherein the step of fabricating the nanochannel with gradually changed dimensions comprises: and in the step 3, the gradient angle range is 25-80 ℃.
10. A graded-size nanochannel, comprising: is manufactured by the manufacturing method of any one of claims 1 to 9.
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| CN111569963A (en) * | 2020-05-21 | 2020-08-25 | 中国科学院微电子研究所 | Horizontal nano-channel array, micro-nano fluidic chip and manufacturing method thereof |
| CN113203769A (en) * | 2021-04-15 | 2021-08-03 | 电子科技大学 | High-air-tightness micro thermal conductivity detector and manufacturing method thereof |
| CN113788452A (en) * | 2021-08-31 | 2021-12-14 | 上海交通大学 | Processing method of fine micro-nano glass structure |
| CN114545725A (en) * | 2022-01-25 | 2022-05-27 | 常州大学 | Method for preparing mask plate by using carbon nano tube film |
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