CN110902647B - Manufacturing method of nano channel with gradually changed size - Google Patents
Manufacturing method of nano channel with gradually changed size Download PDFInfo
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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 template with a nanowire structure: coating photoresist I on one side surface of the quartz glass substrate I; then carrying out holographic exposure, and developing after the exposure is finished until a nanowire structure appears on the photoresist; carrying out ion beam etching on the developed photoresist I under the protection gas, and removing the photoresist after etching to obtain a nanowire structure template; nanowire structures on nanoimprint transfer templates: coating a second photoresist on the second quartz glass substrate; coating a template of the nanowire structure with a release agent, pressing the template into the photoresist II, and performing ultraviolet exposure until the nanowire structure on the template is transferred to the photoresist II; after the transfer is completed, modifying and curing the photoresist II to remove the template of the nanowire structure; dividing the nanowire structure area on the nanowire structure substrate into a plurality of parts, and carrying out silicon dioxide film deposition one by one according to the sequence and at gradual change angles.
Description
Technical Field
The invention relates to a method for manufacturing a nano channel, in particular to a method for manufacturing a nano channel with gradually changed size.
Background
The micro-nano flow control chip can miniaturize basic operations of 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 tens of square centimeters. By designing the appropriate micro-nano channel structure, fluid can flow in the channel in a certain way, so that the chip as a whole obtains a specific function. However, as the channel size decreases, the effect of the size effect will increase and the fluid in the micro-nano channel will exhibit specific properties that are different from those of the macroscopic fluid. For example, quantum effects, interface effects, and nanoscale effects will not be negligible when the channel dimensions reach the nanoscale. Nanochannel-based fluidic systems are therefore of increasing interest.
Nanofluidic systems were utilized and studied, provided nanochannels were fabricated. The traditional nano channel manufacturing method is to manufacture a polymer micro-nano groove structure through nano imprinting, mask plate photoetching or electron beam direct writing and other technologies, and then to combine a thermal bonding technology to realize top sealing of the channel. The thermal bonding technology is a technology of adhering the bonding layer to the micro-nano groove by heating so as to seal the top of the groove to form a channel. Under the action of external pressure, the high polymer bonding layer with the temperature higher than the glass state temperature realizes entanglement of molecular chains at the interface through infiltration and adhesion, and realizes tight interface contact. FIG. 1 is a flow diagram of a conventional thermal bonding technique. However, the polymer in the molten state inevitably flows into the inside of the channel line structure during bonding. As the size of the fabricated channels decreases, particularly when the size reaches the nanometer level, the bonding manner 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 the channels with the dimensions of micrometers and above.
In addition, when some biochemical experiments are performed using nanochannels when the dimensions reach the nanoscale, it is difficult to guide substances or particles to be studied into the nanochannels due to the channel dimensions being too small. For example, when DNA stretching experiments are required, it is difficult to guide DNA particles into nanochannels as they are packed into clusters. If a graded nanochannel can be created, the channel size is graded from large to small, then particles can first enter the large channel and then the small channel. This helps to guide the particles into the nanochannel, however, there is no similar process in conventional processing methods.
Disclosure of Invention
In view of the above, it is necessary to provide a method for fabricating nano-channels with graded dimensions, which is problematic in the existing nano-channel fabrication process. The technical scheme of the invention is as follows:
in a first aspect, the present invention provides a method for fabricating a nano-channel of graded dimensions, comprising the steps of:
step 1, manufacturing a template with a nanowire structure;
step 1.1, coating photoresist I on one side surface of quartz glass substrate I;
step 1.2, carrying out holographic exposure on the first photoresist, and developing after the exposure is finished until a nanowire structure appears on the first photoresist;
step 1.3, carrying out ion beam etching on the developed photoresist I under a protective gas, and removing the photoresist after etching to obtain a nanowire structure template;
step 2, nanoimprint transferring the nanowire structures on the template;
step 2.1, coating a photoresist II on a quartz glass substrate II;
step 2.2, coating the template of the nanowire structure obtained in the step 1 with a release agent, pressing the template into the photoresist II, and then carrying out ultraviolet exposure until the nanowire structure on the template is transferred to the photoresist II;
step 2.3, after the transfer is completed, modifying and curing the photoresist II, and removing the template of the nanowire structure to obtain a nanowire structure substrate;
and 3, dividing the nanowire structure area on the nanowire structure substrate into a plurality of parts, and sequentially depositing silicon dioxide films on the nanowire structure surface of each part one by one at a gradual change angle to form a gradual change size nano channel.
Preferably, in the step 1.1, the first photoresist coating condition is: the spin 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 for 30min at 90 ℃.
Optionally, the first photoresist is AZ701 photoresist.
Preferably, in the step 1.2, the conditions of holographic exposure are: the exposure time is 4-5 minutes; wavelength 442m, light intensity 130mw. The holographic photoetching adopts a laser with a certain wavelength as a light source, expands and filters beams through a spatial filter, and finally forms interference fringes by adopting a Laue mirror light path. After exposing the photoresist, the photoresist records interference fringe information. For two-beam light wave interference, 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 or laser wavelength of the two interference beams on the surface of the sample, photoresist line patterns with different periods can be manufactured.
Further, the aspect ratio of the etched channel in the step 1.3 is 1 (2-2.5).
Further, in the step 2.1, the conditions for coating the photoresist two are as follows: the spin speed of the spin coater is 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-8 2002 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 the step 2.2, the conditions of the ultraviolet exposure are as follows: exposure time was 2 minutes, exposure dose was 200mJ/cm 2 。
Preferably, in the step 2.3, the modifying and curing conditions are as follows: the temperature was 90℃and the time was 10min.
Further, the gradual change angle range in the step 3 is 25-80 ℃.
In a second aspect, the present invention provides a nano-channel with gradually changed dimensions, which is manufactured by the manufacturing method.
The beneficial effects of the invention are as follows: the invention firstly utilizes a holographic photoetching method to prepare a template with a nano line structure which accords with expectations, then transfers the nano line structure on the template to photoresist of another substrate, and then releases the template, and then realizes the sealing of the nano channel by a mode of depositing a film. The method has the advantages that the nano channels with gradually changed sizes can be obtained, and meanwhile, the problem that the traditional sealing channel method is easy to cause channel blockage is avoided. In addition, the problem of connection between the large nano channel and the small nano channel can be solved, so that the nano particles to be detected can be smoothly introduced into the nano channel, further, other biochemical analysis can be more conveniently carried out, and the application range of the nano-particle detector is widened.
Drawings
FIG. 1 is a schematic process flow diagram of a conventional thermal bonding process, wherein a) represents spin coating a polymer on a substrate, b) represents a prepared micro-nano pattern, and c) represents thermal bonding.
Fig. 2 is a schematic diagram of a process for fabricating a template of a nanowire structure according to embodiment 1 of the present invention.
Fig. 3 is a schematic diagram of a process for fabricating a nanowire structure on a nanoimprint transfer template according to embodiment 1 of the present invention.
Fig. 4 is a schematic structural diagram of a first partial shielding and a thin film deposition sealing channel at an angle θ1=25° in embodiment 1 of the present invention, wherein 4-1 is a schematic structural diagram for shielding the remaining portion, and 4-2 is a schematic structural diagram for performing silicon dioxide deposition at a coating angle θ1.
Fig. 5 is a schematic structural diagram of a second partial shielding and a thin film deposition sealing channel at an angle θ2=35° in embodiment 1 of the present invention, wherein 5-1 is a schematic structural diagram for shielding the remaining portion, and 5-2 is a schematic structural diagram for performing silicon dioxide deposition at a coating angle θ1.
Fig. 6 is a schematic structural diagram of a third partial shielding and a thin film deposition sealing channel at an angle θ3=45° in embodiment 1 of the present invention, wherein 6-1 is a schematic structural diagram for shielding the remaining portion, and 6-2 is a schematic structural diagram for performing silicon dioxide deposition at a coating angle θ1.
Fig. 7 is a schematic structural diagram of a fourth partial shielding and a thin film deposition sealing channel at an angle θ4=60° in embodiment 1 of the present invention, wherein 7-1 is a schematic structural diagram for shielding the remaining portion, and 7-2 is a schematic structural diagram for performing silicon dioxide deposition at a coating angle θ1.
Fig. 8 is a schematic diagram of the structure of the final-obtained graded-size seal passage in example 1 of the present invention.
Fig. 9 is a schematic view showing the structure of a first partial shielding and thin film deposition sealing channel at an angle θ1=20° in comparative example 2 of the present invention.
Fig. 10 is a schematic view showing the structure of a fourth partial shielding and thin film deposition sealing channel at an angle θ4=85° in comparative example 3 of the present invention.
Detailed Description
In the description of the present invention, it is to be noted that the specific conditions are not specified in the examples, and the description is performed under the conventional conditions or the conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The invention will now be described in further detail with reference to specific examples, which are intended to illustrate, but not to limit, 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 template with a nanowire structure; the manufacturing process is shown in fig. 2.
Step 1.1, taking a piece of quartz glass with high light transmittance and flat 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 was placed in an asher and ashed for one hour to enhance its surface adhesion. And then coating a layer of tackifier (AZ AD PROMOTER tackifier) on the quartz surface by a spin coater to increase the substrate viscosity and prevent photoresist from degumming during development. The spin speed of the spin coater is 1500r/min for 30s, and the spin coater is placed in an oven at 90 ℃ for 10 minutes;
step 1.2, coating AZ701 photoresist on the pretreated quartz substrate, wherein the photoresist is prepared by a special diluent (AZ 1500 thin diluent) according to the volume ratio of 1:5, the spin-coated post-adhesive layer is thinner, which is beneficial to the subsequent exposure and development. The rotating speed of the spin coater is 1000r/min, the time is 30s, and the thickness of the photoresist is about 200nm; then it was placed in an oven at 90 ℃ for 30 minutes to completely remove the excess solvent;
step 1.3, carrying out holographic exposure on the substrate for 4 minutes; wavelength 442, intensity 130mw. The holographic photoetching adopts a laser with a certain wavelength as a light source, expands and filters beams through a spatial filter, and finally forms interference fringes by adopting a Laue mirror light path. After exposing the photoresist, the photoresist records interference fringe information. For two-beam light wave interference, 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 or laser wavelength of the two interference beams on the surface of the sample, photoresist line patterns with different periods can be manufactured. The nanowire manufactured in the embodiment is 1500 wires, namely the period of the nanowire structure is 667nm;
step 1.4, after exposure, the substrate is placed in NaOH solution with the mass percent of 5 per mill for development, and the development time is 1 minute and 10 seconds; at this time, a nanowire structure will appear on the substrate;
step 1.5, flushing through deionized water after development is completed, and drying by nitrogen;
step 1.6, placing the substrate in an ion beam etching machine, and performing ion beam etching in a trifluoromethyl alkane (CF 3) and argon environment, wherein the etching depth is 160nm and the width is 333nm, so that the aspect ratio of the channel manufactured by the embodiment is about 1:2.
And 1.7, removing the protected photoresist by using acetone to finally obtain the template of the nanowire structure meeting the expectations.
Step 2, nanoimprint transferring the nanowire structures on the template; the manufacturing process is shown in fig. 3.
And 2, pressing the nanowire structure template manufactured in the step 1 into the SU-8 by using glass as a substrate and SU-8 as a transferred photoresist material, and performing ultraviolet exposure, wherein the whole SU-8 is exposed and cured because the quartz template is transparent, so that the nanowire structure is transferred onto the SU-8 photoresist. The purpose and the function of transferring the nanowire structures to the photoresist are two, firstly, the cost can be saved, and the original template can be reused. Second, in the present embodiment, the channel is sealed by thin film deposition, and the deposited thin film material and the photoresist have strong bonding force, so that the structure strength of the fabricated channel is better. The specific process steps are as follows:
step 2.1, taking another piece of flat glass as a substrate, cleaning with clear water and acetone, placing in an oven, baking at 130 ℃ for 10 minutes to remove water vapor and residual acetone, naturally cooling, and placing in an ashing machine for ashing for 1 hour to enhance the surface adhesion;
step 2.2, after the quartz substrate is pretreated, SU-8 2002 photoresist is coated on the quartz substrate. The rotating speed of the spin coater is 600r/min for 9 seconds, then 2000r/min for 60 seconds, and the thickness of the adhesive layer is about 2.5 mu m. Placing the silicon wafer on a hot table, 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 rear template is conveniently separated from SU-8. The release agent is a mixed solution of a Dow Corning organosilicon release agent DC-20 and isopropanol, and the volume ratio DC 20 is as follows: isopropanol=1: 200. Spin coating a release agent at 2000rpm after the template cleaning and drying, wherein the release agent forms a monolayer on the surface of the substrate;
and 2.4, exposing the substrate coated with the release agent under an ultraviolet exposure machine for 2 minutes, wherein the exposure dose is 200mJ/cm < 2 >, and performing post-baking on the exposed SU-8 photoresist to enable the SU-8 photoresist to be modified and cured, wherein the post-baking temperature is 90 ℃ and the time is 10 minutes. After SU-8 is exposed and solidified, the surface energy becomes low, which is beneficial to the subsequent demoulding.
And 2.5, separating the imprinting templates after the SU-8 is solidified. Finally, the nanowire structures were transferred onto SU-8 gel. The demolding process should be carried out below the glass transition temperature of the polymer.
Step 3, manufacturing a size-graded nano channel; the step is to realize the manufacture of the size gradual change nano channel by shielding and changing the coating angle. On the one hand, the problem that the traditional channel sealing process is easy to cause 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 coating, treating the SU-8 nanowire structure by oxygen plasma to remove the release agent remained on the substrate and brought by the template, and simultaneously, improving the surface energy of SU-8, enhancing the surface energy of SU-8 and silicon dioxide (SiO) deposited later 2 ) The bonding force between the films;
step 3.2, dividing the nanowire structure area on the manufactured nanowire structure substrate into 4 parts, sequentially depositing silicon dioxide films, and shielding the rest parts by a shielding plate when one part is deposited, as shown in figures 4-7Placing the substrate in a magnetron sputtering coating machine, adjusting the angle between the substrate and the target, and adding silicon dioxide (SiO 2 ) The film is deposited on the substrate in the first portion, the portion of the channel near the entrance of the channel, the angle of the coating is greater, so that the size of the channel formed by the coating seal is relatively greater. Here SiO is used 2 As the coating material is a transparent material, the internal condition of the channel can be conveniently observed, and the coating material is convenient to apply to other chemical biological experiments. Then, the second portion is masked, and the coating angle (θ2=35°) is adjusted again, as shown in fig. 5, so that the coating angle is smaller, and thus the size of the channel formed by the seal is relatively smaller. The steps are repeated, as shown in fig. 6 and 7, the third part and the fourth part are shielded, the film deposition angle (θ3=45°, θ4=60°) is changed, and finally the nano-channel with gradual width is manufactured. The width of the fabricated channel (schematically one of them) gradually changes from a to b, then to c, and finally to d from the inlet to the outlet, as shown in fig. 8, wherein a, b, c, d is about 330nm, 220nm, 160nm, and 90nm.
Comparative example 1
The difference between the method for manufacturing nano channels with gradually changed sizes and the method for manufacturing nano channels with gradually changed sizes in embodiment 1 is that: and step 3, adopting bonding sealing, namely covering a layer of cover plate on the substrate obtained in the step 2 for sealing, and finally only obtaining a channel with one size.
Comparative example 2
The difference between the method for manufacturing nano channels with gradually changed sizes and the method for manufacturing nano channels with gradually changed sizes in embodiment 1 is that: θ1=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 at the time of channel sealing by deposition cannot be lower than 25 °.
Comparative example 3
This comparative example provides a method for fabricating a nano-channel of graded dimensions, which differs from example 1 in that: θ4=85°. As a result, channel clogging occurs at the time of the fourth partial deposition, and as shown in fig. 10, it is presumed that the channel clogging is caused due to a series of reasons such as inter-particle collision, scattering, and the like, and in any case, the end result is that if the deposition maximum angle is more than 80 °, the channel clogging is failed.
In summary, the invention firstly utilizes the holographic lithography method to prepare the template with the expected nanowire structure, then transfers the nanowire structure on the template to the photoresist of another substrate, and then releases the mold, and then realizes the sealing of the nanochannel by a mode of depositing a film. The method has the advantages that the nano channels with gradually changed sizes can be obtained, and meanwhile, the problem that the traditional sealing channel method is easy to cause channel blockage is avoided. In addition, the problem of connection between the large nano channel and the small nano channel can be solved, so that the nano particles to be detected can be smoothly introduced into the nano channel, further, other biochemical analysis can be more conveniently carried out, and the application range of the nano-particle detector is widened.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. A manufacturing method of a nano channel with gradually changed size is characterized in that: the method comprises the following steps:
step 1, manufacturing a template with a nanowire structure;
step 1.1, coating photoresist I on one side surface of a quartz glass substrate I with high light transmittance, wherein the thickness of the photoresist I is 180-220 nm;
step 1.2, carrying out holographic exposure on the first photoresist, and developing after the exposure is finished until a nanowire structure appears on the first photoresist;
step 1.3, carrying out ion beam etching on the developed photoresist I under a protective gas, and removing the photoresist after etching to obtain a nanowire structure template;
step 2, nanoimprint transferring the nanowire structures on the template;
step 2.1, coating a photoresist II on a quartz glass substrate II;
step 2.2, coating the template of the nanowire structure obtained in the step 1 with a release agent, pressing the template into the photoresist II, and then carrying out ultraviolet exposure until the nanowire structure on the template is transferred to the photoresist II;
step 2.3, after the transfer is completed, modifying and curing the photoresist II, and removing the template of the nanowire structure to obtain a nanowire structure substrate;
and 3, dividing the nanowire structure area on the nanowire structure substrate into a plurality of parts, and sequentially depositing silicon dioxide films on the nanowire structure surface of each part one by one at a gradual change angle to form a gradual change size nano channel.
2. The method for fabricating a nano-channel with gradually changed size according to claim 1, wherein: in the step 1.1, the condition for coating the photoresist one is as follows: the spin speed of the spin coater is 1000-2000 r/min, the time is 30s, and the temperature is kept at 90 ℃ for 30min.
3. The method for fabricating a nano-channel with gradually changed size according to claim 1, wherein: in the step 1.2, the conditions of holographic exposure are as follows: the exposure time is 4-5 minutes; wavelength 442m, light intensity 130mw.
4. The method for fabricating a nano-channel with gradually changed size according to claim 1, wherein: and the width-depth ratio of the etched channel in the step 1.3 is 1 (2-2.5).
5. The method for fabricating a nano-channel with gradually changed size according to claim 1, wherein: in the step 2.1, the condition for coating the photoresist II is as follows: the spin speed of the spin coater is 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 for fabricating a nano-channel with gradually changed size according to claim 1, wherein: 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.
7. The method for fabricating a nano-channel with gradually changed size according to claim 1, wherein: in the step 2.2, the conditions of ultraviolet exposure are as follows: exposure time was 2 minutes, exposure dose was 200mJ/cm 2 。
8. The method for fabricating a nano-channel with gradually changed size according to claim 1, wherein: in the step 2.3, the conditions for modifying and curing are as follows: the temperature was 90℃and the time was 10min.
9. The method for fabricating a nano-channel with gradually changed size according to claim 1, wherein: and in the step 3, the gradual change angle range is 25-80 degrees.
10. A tapered nanochannel, characterized in that: is manufactured by the manufacturing method according to any one of claims 1 to 9.
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