CN113058665B - Preparation method of microfluidic channel based on two-dimensional material and microfluidic device - Google Patents
Preparation method of microfluidic channel based on two-dimensional material and microfluidic device Download PDFInfo
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Abstract
A preparation method of a microfluidic channel based on a two-dimensional material and a microfluidic controller device are provided. According to one embodiment, the preparation method comprises the following steps: growing a two-dimensional material film on a substrate, depositing a protective layer on the two-dimensional material film, and finally continuously depositing an inorganic film with a certain thickness by magnetron sputtering. When meeting an excitation source such as water, the stress in the film is partially released and deformed, so that a micro-flow channel with a hollow structure is generated at the interface of the two-dimensional material and the substrate. The method is simple and convenient to operate, and the inner wall of the prepared microfluidic channel is provided with an atomically flat surface, so that the method is favorable for the transmission of liquid in a microfluidic pipeline.
Description
Technical Field
The application belongs to the technical field of microfluidic devices and processes, and particularly relates to a preparation method of a microfluidic channel based on a two-dimensional material and a specific application of the microfluidic channel in a microfluidic device.
Background
The microfluidic system has a huge application prospect in the analysis field, has the advantages of high resolution and high sensitivity when analyzing and processing samples, and can greatly save the consumption of the samples and reagents, reduce the analysis cost and shorten the analysis time. Microfluidic systems with these advantages have now played a significant role in the fields of life sciences, chemical engineering, as well as environmental monitoring and defense science, among others.
The microfluidic channel is an important component of a microfluidic system, and at present, high polymers such as PDMS, silicon-based materials such as silicon oxide and silicon nitride are mostly used as the component materials of the microfluidic channel, but complicated processing methods such as photolithography and ion beam processing are often required when the microfluidic channel is constructed on the basis of the materials. In addition, the inner walls of the microfluidic channels processed by the conventional method are rough, and when the dimensions of the microfluidic channels are small, the rough walls of the microfluidic channels can adversely affect the transport of fluids in the microfluidic channels. In addition, at present, a method using a carbon tube and an etched graphene channel as a fluid transmission channel is also available, but the method faces the problems of poor controllability and complex processing process.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a microfluidic channel, which uses a two-dimensional material to prepare a microfluidic channel having an atomically flat inner wall. The method of the invention can conveniently and quickly construct a microfluidic device.
One aspect of the present invention provides a method for preparing a microfluidic channel based on a two-dimensional material, the method comprising the steps of:
obtaining a two-dimensional material on a substrate;
depositing an inorganic thin film on the two-dimensional material; and
releasing the stress in the inorganic thin film causes the two-dimensional material to deform, thereby forming a microfluidic channel between the interface of the two-dimensional material and the substrate.
In some examples, the substrate comprises sapphire, silicon nitride, or copper foil.
In some examples, the method may further include: and pre-treating the substrate before the growth of the two-dimensional material so as to enable the surface of the substrate to be flat.
In some examples, the two-dimensional material comprises a single layer or multiple layers of two-dimensional material.
In some examples, the obtaining a two-dimensional material on a substrate includes: growing a two-dimensional material on the substrate by a deposition method, an epitaxy method or a deposition method, or transferring a two-dimensional material onto the substrate.
In some examples, the inorganic thin film comprises silicon, a metal, or a metal oxide.
In some examples, the method may further include: depositing a protective layer on the two-dimensional material prior to depositing an inorganic thin film on the two-dimensional material.
In some examples, the method may further include: and patterning the inorganic thin film to control the area and the direction of the formed microfluidic channel.
In some examples, the relieving stress in the inorganic thin film such that the two-dimensional material deforms includes: and (3) putting the film in a humid environment or contacting the film with water so as to excite the two-dimensional material to generate deformation.
Another aspect of the present invention provides a microfluidic device comprising: a substrate; a two-dimensional material disposed on the substrate; an inorganic thin film disposed over the two-dimensional material; and a microfluidic channel formed between an interface of the two-dimensional material and the substrate.
The microfluidic channel is prepared on the basis of the two-dimensional material by utilizing the fact that the two-dimensional material has an atomically flat surface and excellent mechanical property and chemical stability. Compared with the traditional microfluidic channel processing technology, the method provided by the invention has the advantages that ion etching is not needed in the process of preparing the microfluidic channel, and the processing process is simpler, more convenient and faster. The inner wall of the processed micro-flow channel is provided with an atomically flat surface, which is beneficial to the transmission of liquid and other fluids with small size. Meanwhile, the method can effectively control the formation, the size and the direction of the microfluidic channel by controlling an external excitation source, and the prepared microfluidic channel has uniform size and good uniformity. The micro-fluidic device obtained by processing has application potential in the fields of chemical industry, medicine, environmental monitoring and the like.
Drawings
In order to more clearly illustrate the technical solutions and advantages of the embodiments of the present invention, the drawings used in the present invention will be briefly described below.
Fig. 1 is a schematic process diagram illustrating a method for manufacturing a microfluidic channel according to an exemplary embodiment of the present disclosure.
FIG. 2 shows an atomic force microscope topography of a sapphire substrate after annealing in an exemplary embodiment of the present application.
Fig. 3 shows a plurality of microfluidic channels with uniform directions prepared according to an exemplary embodiment of the present application.
Fig. 4 is a schematic process diagram of a method for manufacturing a microfluidic channel according to another exemplary embodiment of the present disclosure.
Fig. 5 is an SEM cross-sectional view of a microfluidic channel prepared according to an exemplary embodiment of the present disclosure.
Fig. 6 shows the fluid transport process in a microfluidic channel prepared according to an exemplary embodiment of the present application.
FIG. 7 is a schematic view of a microfluidic channel propagating along a specified area obtained by patterning according to another exemplary embodiment of the present application.
Detailed Description
Hereinafter, exemplary embodiments of the present application will be described in detail with reference to the accompanying drawings. It should be understood that the described embodiments are only some embodiments of the present application and not all embodiments of the present application, and that the present application is not limited by the example embodiments described herein. Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art.
It is an object of the present invention to obtain microfluidic channels based on two-dimensional material preparation on a substrate. Fig. 1 is a schematic process diagram illustrating a method for manufacturing a microfluidic channel according to an embodiment of the present disclosure.
As shown in fig. 1, the preparation method may begin with step S110, obtaining a two-dimensional material 20 on a substrate 10.
In one example, the substrate 10 may include, but is not limited to, a substrate material such as sapphire, silicon dioxide, silicon nitride, or copper foil, which may be selected as appropriate depending on the two-dimensional material to be grown or the microfluidic device to be processed, etc.
Generally, the substrate 10 may be pre-treated prior to preparation, such as by cleaning, for example, by an ultrasonic cleaning operation to remove surface particles and thereby obtain a clean surface. The two-dimensional material 20 may be grown in situ on the substrate 10 by a deposition method, an epitaxial method, a precipitation method, or the like, or the two-dimensional material obtained by the preparation may be transferred to a suitable substrate 10 by a transfer method or the like.
For example, a two-dimensional material, which may be a single layer or multiple layers of two-dimensional materials, may be grown on the substrate by chemical vapor deposition, physical deposition, molecular beam epitaxy, solution-precipitation, etc., and a single layer of two-dimensional material 20 is preferably grown on the substrate 10 for subsequent controlled deformation to form the microfluidic channel. Specifically, a single-layer two-dimensional transition metal chalcogenide (MoS) compound can be prepared by the above-described method2、MoSe2、MoTe2) And the graphene can be prepared on the metal substrate by a metal catalytic epitaxial growth method, a chemical vapor deposition method and the like. In addition, in order to control the preparation of the device and the performance regulation at the later stage, the two-dimensional material prepared by growth may need to be transferred to other substrates. Two-dimensional by transfer mediaThe material is detached from the growth substrate and then transferred to a target substrate.
In one embodiment, in order to obtain a two-dimensional material with high flatness and high uniformity on a substrate, thereby preparing the inner wall of the microfluidic channel with an atomically flat surface, a substrate such as sapphire, silicon nitride, copper foil, etc. may be pretreated before growing/transferring the two-dimensional material, so as to flatten the surface of the substrate. For example, the substrate may be heated to 1000-1400 ℃ under vacuum to perform an annealing process, so that the substrate surface with atomically flat steps may be obtained. Fig. 2 shows an afm profile of a sapphire substrate (0001) annealed at 1000 c for 2h, which can be seen to have an atomically flat surface that provides a flat lower channel wall for the microfluidic channel.
Returning to fig. 1, after the two-dimensional material is obtained on the substrate, the step S120 may be continued to deposit the inorganic thin film 30 on the two-dimensional material 20.
For example, an inorganic thin film may be deposited on the two-dimensional material by magnetron sputtering deposition or the like, and the additionally deposited thin film may provide an external stress required for deformation of the two-dimensional material, thereby preparing the microfluidic channel composed of the two-dimensional material in a controlled manner. The inventors have found that if the inorganic thin film is not deposited on a two-dimensional material, the two-dimensional material is merely epitaxially grown on a substrate, wherein the stress present therein hardly reaches a critical value at which the two-dimensional material can be strained, and the magnitude and distribution of the stress are hardly controlled. The inorganic thin film 30 can provide stress required for deformation of the two-dimensional material, the released stress can deform the two-dimensional material when reaching a critical value, and a hollow structure generated at the separation part of the deformation part and the substrate can be used as a microfluidic channel for fluid transmission.
In one embodiment, the inorganic thin film 30 is configured to provide the stress required for deformation of the two-dimensional material, and may be selected from one or more of silicon, metal oxide, and other inorganic materials, preferably a transparent ITO thin film, which can accumulate stress in the inorganic thin film 30 under physical bombardment during magnetron sputter deposition. The stress can be controlled and adjusted by controlling the sputtering conditions and the film thickness of the film 30, for example, by adjusting the substrate heating temperature, the deposition rate, the deposition thickness, and the like, wherein the substrate heating temperature is preferably 150-; the thickness of the deposited film is 50-100nm, preferably 60-75nm, and the appropriate microfluidic channel size can be obtained in the thickness range, and the specific thickness can be selected according to the required microfluidic channel size.
The deposition of the film is preferably carried out under a vacuum condition, so that a clean film-two-dimensional material bonding interface can be obtained, the bonding force between the two is improved, namely a heterojunction of the two-dimensional material film/the inorganic material film is formed, the bonding force is larger than the bonding force between the two-dimensional material and the substrate when the two-dimensional material film/the inorganic material film is deformed, and the subsequent formation of a microfluidic channel with a smooth inner wall is facilitated.
In another embodiment, the inorganic film 30 may be obtained by vapor deposition or the like, wherein stress may be introduced into the film by subsequent processing of the deposited film, for example, by heating the inorganic film to form stress within the film.
After obtaining the inorganic thin film on the two-dimensional material, the preparation method may proceed to step S130, and release the stress in the inorganic thin film 30 to deform the two-dimensional material 20, so as to form a microfluidic channel between the interface of the two-dimensional material 20 and the substrate 10.
As previously mentioned, inorganic thin films have internal stresses during deposition or subsequent processing that provide the stresses necessary for deformation of the two-dimensional material. By changing the external environment, the stress in the inorganic thin film can be partially released and transferred to the two-dimensional material to deform the two-dimensional material.
In one example, water may be used as the excitation source, and the two-dimensional material may be excited to deform by placing a thin film on a substrate in a humid environment or by contacting the thin film with water. In this example, by utilizing the property that water can be inserted into the substrate due to different surface energies between the two-dimensional material and the substrate, when water starts to enter the interface between the substrate and the two-dimensional material, the stress balance between the two-dimensional material and the inorganic thin film is broken, so that the stress in the thin film is released and a certain period of deformation is generated to separate from the substrate, thereby causing the generation of a microfluidic channel.
The excitation source can be used in a dripping mode to effectively control the dripping amount of water and favorably control the position and the quantity of formed microfluidic channels. As described above, the size and the transmission direction of the microfluidic channel can be effectively controlled by controlling the stress in the thin film, i.e., the microfluidic channel can be effectively controlled by adjusting the performance parameters of the thin film. Therefore, the microfluidic channel can be controllably prepared by controlling the preparation method.
Fig. 3 shows a microfluidic channel prepared according to an exemplary embodiment of the present application. As shown, the film and the two-dimensional material can be deformed by releasing the stress in the inorganic film in a humid environment, and a plurality of microfluidic channels with the same direction are generated.
Fig. 4 is a schematic process diagram illustrating a method for manufacturing a microfluidic channel according to another embodiment of the present application, which is substantially the same as the process shown in fig. 1, except that after the two-dimensional material 20 is formed on the substrate 10 and before the inorganic thin film 30 is deposited on the two-dimensional material 20, the method further includes step S220: a protective layer 40 is deposited over the two-dimensional material 20.
Since the two-dimensional material 20 has a thickness only in atomic scale, for example, a single layer of molybdenum disulfide has a thickness of only 0.6-0.9nm, it is easily damaged in the plasma environment of magnetron sputtering, and for this purpose, an intermediate layer may be deposited between the two-dimensional material and the inorganic thin film, which may serve as a protective layer for the two-dimensional material and may also serve as an adhesion layer between the two-dimensional material and the subsequently deposited inorganic thin film. In one example, the material of the protective layer may be a chemically stable metal material, such as a noble metal material, e.g., gold, platinum, etc.
In order not to affect the stress transfer of the inorganic thin film, it is preferable that the thickness of the protective layer 40 is below 5nm, and it can be directionally deposited on the two-dimensional thin film material by a process such as electron beam evaporation deposition to serve as a protective layer of the two-dimensional material and an adhesion layer between the two-dimensional material and the inorganic material.
Steps S210, S230, and S240 shown in fig. 4 are substantially the same as steps S110, S120, and S130 described above with respect to fig. 1, for example, an inorganic thin film with a certain thickness may be deposited on the protective layer by magnetron sputtering, and will not be described herein again.
In order to further control the stress in the inorganic thin film and the topography of the microfluidic channels, the inorganic thin film on the two-dimensional material/protective layer may be patterned to control the area and direction in which the microfluidic channels are formed.
In one embodiment, the patterning process may be performed by way of a mask exposure. For example, a layer of photoresist (photoresist) may be coated on the two-dimensional material/protective layer, the obtained sample is exposed, for example, by ultraviolet light irradiation, to denature the positive photoresist, and then developed and fixed, so that the inorganic thin film deposited in the region where no photoresist exists can be in direct contact with the two-dimensional material/protective layer, so that the stress in the thin film can be transferred to the two-dimensional material thin film, and thus the microfluidic channel will be defined in the photoresist-free region and spread in a certain direction in the region.
The microfluidic channel prepared by the method is simple and convenient to operate, the size of the channel is controllable, and the inner wall of the prepared microfluidic channel is provided with the atomically flat surface, so that the microfluidic channel is beneficial to transmission of fluid in the microfluidic pipeline.
Another embodiment of the present invention provides a microfluidic device, referring to fig. 1 and 4, which may include: a substrate; a two-dimensional material disposed on the substrate; an inorganic thin film disposed over the two-dimensional material; and a microfluidic channel formed between an interface of the two-dimensional material and the substrate. The microfluidic channel can be obtained by the method described above, and has an atomically flat inner wall, wherein the upper part of the inner wall is made of a two-dimensional material, the lower part of the inner wall is made of a substrate, and the flat inner wall is beneficial to small-sized fluid transmission and can be used in the fields of life science, chemical engineering, environmental monitoring and the like. In addition, as shown in fig. 4, the microfluidic device may further include an optional protective layer, and the material and the preparation method thereof are described in detail with reference to the foregoing description, which is not repeated herein.
The following will further explain the preparation method and application of the microfluidic channel of the present invention with reference to the specific examples and the accompanying drawings.
Example 1
The preparation process of the microfluidic channel is as follows:
annealing the sapphire substrate at 1000 ℃, wherein the surface of the annealed sapphire substrate is flat and has steps with atomic level flatness; growing a single-layer molybdenum sulfide film on the annealed sapphire substrate through chemical vapor deposition epitaxy; depositing 3nm gold on the molybdenum sulfide film through electron beam evaporation to serve as a protective layer of the molybdenum sulfide and an adhesion layer between the molybdenum sulfide and the film deposited subsequently; continuously depositing ITO with the thickness of 50nm on the surface of the sample by utilizing magnetron sputtering; deionized water is used as an excitation source, water is dripped between the molybdenum sulfide two-dimensional material and the substrate, and when the water begins to enter the interface between the substrate and the two-dimensional material, the stress balance of the two-dimensional material is broken, so that the two-dimensional material is deformed, and a microflow channel is further generated.
Fig. 5 shows a SEM cross-sectional view of the microfluidic channel prepared as above, and it can be seen that the film is separated from the substrate due to the deformation, and at the same time, since the bonding force between the gold and the two-dimensional material is greater than the bonding force between the two-dimensional material and the substrate, the two-dimensional material will deform together with the film to form the microfluidic channel, the height of the channel is about 1 μm, and the deformed two-dimensional material constitutes the upper tube wall of the microfluidic channel, which has an atomically flat surface with the annealed substrate surface.
Fig. 6 shows the process of transferring fluid in the microfluidic channel prepared in this example, wherein the liquid used is an aqueous solution of sodium fluorescein, and it can be seen that the sodium fluorescein solution can be smoothly transferred in the microfluidic channel by capillary action as shown by the arrows.
Example 2
Annealing the sapphire substrate at 1200 ℃; growing a single-layer molybdenum sulfide film on the annealed sapphire substrate through molecular beam epitaxy; depositing gold with the thickness of 3 nanometers on the molybdenum sulfide film through electron beam evaporation to serve as a protective layer of the molybdenum sulfide and an adhesion layer between the molybdenum sulfide and a stress film to be provided subsequently; processing a sample by ultraviolet exposure patterning, and after developing and fixing, directly contacting the area film without the photoresist with gold serving as an adhesion layer, so that the stress in the film can be transferred to molybdenum sulfide, and a microfluidic channel is limited in the area to be formed and spread; and continuously depositing 70 nm of ITO on the surface of the sample by magnetron sputtering. And then, placing the obtained two-dimensional material/gold/ITO heterojunction film in a humid environment to excite the film and the two-dimensional material to deform, so as to realize the generation of a microfluidic channel.
Fig. 7 is a schematic diagram of a microfluidic channel that propagates along a designated area obtained by patterning as above, and it can be seen that the microfluidic channel propagates along the designated area (shown as a six-square boundary) after the thin film is patterned by means of the uv exposure of the present example.
As used herein, words such as "including," "comprising," "having," and the like are open-ended words that mean "including, but not limited to," and are used interchangeably herein. The words "or" and "as used herein mean, and are used interchangeably with, the word" and/or, "unless the context clearly dictates otherwise. The word "such as" is used herein to mean, and is used interchangeably with, the phrase "such as but not limited to".
The previous description of the disclosed aspects is provided to enable any person skilled in the art to make or use the present application. Various modifications to these aspects will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other aspects without departing from the scope of the application. It will be appreciated by those skilled in the art that certain changes, modifications, substitutions and alterations can be made to the embodiments described above without departing from the principles and spirit of the invention. Thus, the present application is not intended to be limited to the aspects shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A preparation method of a microfluidic channel based on a two-dimensional material comprises the following steps:
obtaining a two-dimensional material on a substrate;
depositing an inorganic thin film on the two-dimensional material by magnetron sputtering or vapor deposition; and
releasing stress in the inorganic thin film to deform the two-dimensional material, thereby forming a microfluidic channel between the two-dimensional material and the substrate interface,
wherein the releasing the stress in the inorganic thin film such that the two-dimensional material deforms comprises:
placing the film in a humid environment or contacting the film with water to excite the two-dimensional material to generate deformation,
wherein the obtaining a two-dimensional material on a substrate comprises: growing a two-dimensional material on the substrate by a deposition method, an epitaxy method or a deposition method, or transferring a two-dimensional material onto the substrate.
2. The method of claim 1, wherein the substrate comprises sapphire, silicon nitride, or copper foil.
3. The method of claim 1, wherein the method further comprises:
and pre-treating the substrate before the growth of the two-dimensional material so as to enable the surface of the substrate to be flat.
4. The method of claim 1, wherein the two-dimensional material comprises a single layer or multiple layers of two-dimensional material.
5. The method of claim 1, wherein the inorganic thin film comprises silicon, a metal, or a metal oxide.
6. The method of any preceding claim, wherein the method further comprises:
depositing a protective layer on the two-dimensional material prior to depositing an inorganic thin film on the two-dimensional material.
7. The method of claim 6, wherein the method further comprises:
and patterning the inorganic thin film in a mask exposure mode to control the area and the direction of the formed microfluidic channel.
8. A microfluidic device comprising:
a substrate;
a two-dimensional material disposed on the substrate;
an inorganic thin film disposed over the two-dimensional material; and
and the microfluidic channel is formed between the two-dimensional material and the interface of the substrate, wherein the microfluidic channel is formed by releasing stress in the inorganic thin film to deform the two-dimensional material, and the releasing of the stress in the inorganic thin film to deform the two-dimensional material comprises placing the thin film in a humid environment or contacting the thin film with water to excite the two-dimensional material to deform.
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