CN114682314B - Manufacturing method of self-sealing nano flow channel - Google Patents
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Abstract
The invention provides a manufacturing method of a self-sealing nano flow channel, which comprises the following steps: a) Injecting a required two-dimensional pattern of the nano flow channel structure on the monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional pattern of the nano flow channel structure on the surface; b) Etching the two-dimensional pattern of the monocrystalline silicon substrate obtained in the step A) by using a wet etching agent to obtain the monocrystalline silicon substrate with the nano flow passage structure; c) And B), depositing a layer of film on the surface and the horizontal surface of the nano flow channel structure of the monocrystalline silicon substrate obtained in the step B), and sealing the upper end of the nano flow channel structure through deposition to form a closed nano flow channel structure. The method provided by the invention can process the flow channel structure with the nanometer inner diameter, and has high manufacturing precision. The method has low cost and higher process reliability, is easy to integrate with the existing micro-channel processing technology, and can be used for manufacturing high-precision nano-fluidic chip devices.
Description
Technical Field
The invention belongs to the technical field of micro-nano processing, and particularly relates to a manufacturing method of a self-sealing nano flow channel.
Background
The nano flow channel refers to a micro flow channel structure with a structure dimension in a nano range (a few nanometers to hundreds of nanometers). The nano flow channel structure is made in the micro-fluidic chip, so that the interaction between the fluid and the nano surface can generate fluid characteristics different from the macro scale due to the common influence of effects of van der Waals force, electrostatic force, capillary force and the like. These features have important effects and wide application in techniques such as fluid handling, biosensing, protein detection, and DNA sequencing. Therefore, in order to explore the special properties of fluids in micro-nano fluidic systems, it is necessary to develop a nano flow channel processing technology that is simple, reliable, and easy to integrate with existing processing technologies.
The current nano flow channel processing technology is mainly realized by a plurality of procedures such as spin coating, electron beam lithography, coating, etching, bonding and the like by depending on the traditional semiconductor processing technology, the manufacturing mode is complex, the integration level is poor, and the processing difficulty is rapidly increased along with the reduction of the critical dimension of the flow channel structure.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for manufacturing a self-sealing nano flow channel, which can process a self-sealing flow channel structure with nano-scale inner diameter, has relatively simple processing steps, is easy to integrate with the existing micro-flow channel processing technology, and can be used for manufacturing a high-precision nano-fluidic chip device.
The invention provides a manufacturing method of a self-sealing nano flow channel, which comprises the following steps:
a) Injecting a required two-dimensional pattern of the nano flow channel structure on the monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional pattern of the nano flow channel structure on the surface;
b) Etching the two-dimensional pattern of the monocrystalline silicon substrate obtained in the step A) by using a wet etching agent to obtain the monocrystalline silicon substrate with the nano flow passage structure;
c) And B), depositing a layer of film on the surface and the horizontal surface of the nano flow channel structure of the monocrystalline silicon substrate obtained in the step B), and sealing the upper end of the nano flow channel structure through deposition to form a closed nano flow channel structure.
Preferably, the apparatus for helium ion beam implantation is selected from helium ion microscopes or ion implanters.
Preferably, the ion energy of the helium ion beam implantation is 1-200 keV.
Preferably, the monocrystalline silicon substrate comprises a P-type monocrystalline silicon substrate, an N-type doped monocrystalline silicon substrate, an intrinsic silicon wafer monocrystalline silicon substrate, an SOI wafer or a silicon thin film material.
Preferably, the wet etching agent is HF with the mass fraction of 40% and H with the mass fraction of 33% 2 O 2 The volume ratio of the mixed solution is 100:1-1:100, preferably 10:1-1:50.
Preferably, the etching time is 0.1 to 120min, preferably 2 to 30min.
Preferably, the nano flow channel structure is in a water drop shape in section and is provided with an opening at the upper end.
Preferably, the deposition is selected from chemical vapor deposition or physical vapor deposition, and the deposition equipment is selected from ALD, PECVD, LPCVD, PLD, magnetron sputtering coater, electron beam evaporation coater, thermal evaporation coater or ion beam coater.
Preferably, the deposited material comprises SiO 2 、SiN x 、TiO 2 、TiN、HfO 2 、Al 2 O 3 、Fe 3 O 4 AlN, ti, au, ag, pt, cr, cu, W, ni or Mo.
Preferably, the thickness of the deposited film is 5-500 nm.
Compared with the prior art, the invention provides a manufacturing method of a self-sealing nano flow channel, which comprises the following steps: a) Injecting a required two-dimensional pattern of the nano flow channel structure on the monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional pattern of the nano flow channel structure on the surface; b) Etching the two-dimensional pattern of the monocrystalline silicon substrate obtained in the step A) by using a wet etching agent to obtain the monocrystalline silicon substrate with the nano flow passage structure; c) And B), depositing a layer of film on the surface and the horizontal surface of the nano flow channel structure of the monocrystalline silicon substrate obtained in the step B), and sealing the upper end of the nano flow channel structure through deposition to form a closed nano flow channel structure. The method provided by the invention can process the flow channel structure with the nanometer inner diameter, has high manufacturing precision, and does not need to use photoresist or a sacrificial layer in the processing process. Compared with other main flow processes, the method has the advantages that the method only needs one ion implantation and one chemical wet etching, has simple manufacturing steps, does not need multiple etching, does not need a bonding process to realize flow channel sealing, and greatly reduces the process complexity. Therefore, the method has lower cost and higher process reliability, is easy to integrate with the existing micro-channel processing technology, and can be used for manufacturing high-precision nano-fluidic chip devices.
Drawings
FIG. 1 is a schematic flow chart of a method for manufacturing a self-sealing nano-channel according to the present invention;
FIG. 2 is a schematic diagram of a method for fabricating a nano-channel structure according to the present invention;
FIG. 3 is an SEM characterization image of the nano-channel structure fabricated in example 1;
FIG. 4 is a high resolution photograph of a cross section of the nano-fluidic channel structure after the processing of example 1;
FIG. 5 is a high resolution photograph of a cross section of the nano-fluidic channel structure after the processing of example 2;
FIG. 6 is a top view image of the nano-fluidic channel structure after the processing of example 3;
fig. 7 is a top view image of the nano-fluidic channel structure after the processing of example 4.
Detailed Description
The invention provides a manufacturing method of a self-sealing nano flow channel, which comprises the following steps:
a) Injecting a required two-dimensional pattern of the nano flow channel structure on the monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional pattern of the nano flow channel structure on the surface;
b) Etching the two-dimensional pattern of the monocrystalline silicon substrate obtained in the step A) by using a wet etching agent to obtain the monocrystalline silicon substrate with the nano flow passage structure;
c) And B), depositing a layer of film on the surface and the horizontal surface of the nano flow channel structure of the monocrystalline silicon substrate obtained in the step B), and sealing the upper end of the nano flow channel structure through deposition to form a closed nano flow channel structure.
The substrate selected by the invention is a monocrystalline silicon substrate, wherein the monocrystalline silicon substrate comprises a P-type monocrystalline silicon substrate, an N-type doped monocrystalline silicon substrate, an intrinsic silicon wafer monocrystalline silicon substrate, an SOI (silicon on insulator) sheet or a silicon film material.
After preparing the monocrystalline silicon substrate, injecting a required two-dimensional pattern of the nano flow channel structure on the monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional pattern of the nano flow channel structure on the surface.
The shape of the two-dimensional graph of the nano flow channel structure is not particularly limited, and the two-dimensional graph can be designed into a straight line, a curve, a rectangle, a circle or a ring shape according to the requirement.
The apparatus for helium ion beam implantation is not particularly limited, and in the present invention, a helium ion microscope or an ion implanter is preferable.
The ion energy of the helium ion beam implant is 1 to 200keV, preferably 1keV, 5keV, 10keV, 50keV, 100keV, 150keV, 200keV, or any value between 1 and 200keV.
And after the monocrystalline silicon substrate with the nano-runner structure two-dimensional pattern on the surface is obtained, etching the obtained monocrystalline silicon substrate on the two-dimensional pattern by using a wet etching agent to obtain the monocrystalline silicon substrate with the nano-runner structure.
Wherein the wet etching agent comprises 40% of HF by mass and 33% of H by mass 2 O 2 The volume ratio of the mixed solution of (2) is 100:1 to 1:100, preferably 10:1 to 1:50, more preferably10:1, 5:1, 1:1, 1:5, 1:10, 1:20, 1:30, 1:40, 1:50, or any value between 10:1 and 1:50.
The etching time is 0.1 to 120 minutes, preferably 2 to 30 minutes, more preferably 2, 5, 10, 15, 20, 25, 30, or any value between 2 and 30 minutes.
After the corrosion is completed, the formed nano flow channel structure is in a water drop shape in section and is provided with an opening at the upper end.
In the present invention, the inner diameter of the nano flow channel structure is 30 to 500nm, preferably 30, 50, 100, 150, 200, 250, 300, 350, 400, 450, 500, or any value between 30 and 500nm, and the center depth is 100 to 800nm, preferably 100, 200, 300, 400, 500, 600, 700, 800, or any value between 100 and 800.
And B), depositing a layer of film on the surface and the horizontal surface of the nano-runner structure of the monocrystalline silicon substrate obtained in the step B) after the monocrystalline silicon substrate with the nano-runner structure is obtained, and sealing the upper end of the nano-runner structure through deposition to form a closed nano-runner structure.
The deposition is selected from chemical vapor deposition or physical vapor deposition, and the deposition equipment is selected from ALD, PECVD, LPCVD, PLD, a magnetron sputtering coating machine, an electron beam evaporation coating machine, a thermal evaporation coating machine or an ion beam coating machine.
The deposition material comprises SiO 2 、SiN x 、TiO 2 、TiN、HfO 2 、Al 2 O 3 、Fe 3 O 4 AlN, ti, au, ag, pt, cr, cu, W, ni or Mo, preferably SiO 2 、Al 2 O 3 Pt or Cu.
The deposited film thickness is 5 to 500nm, preferably 5, 10, 50, 100, 200, 300, 400, 500, or any value between 5 and 500nm. The thin film comprises a thin film on the surface of the nano flow channel structure and a thin film on the surface of the monocrystalline silicon substrate.
Referring to fig. 1 to 2, fig. 1 is a schematic flow chart of a method for manufacturing a self-sealing nano flow channel according to the present invention.
FIG. 2 is a schematic diagram of a method for fabricating a nano-channel structure according to the present invention. In fig. 2, first, a desired two-dimensional pattern of a nano flow channel structure is implanted on the surface of a single crystal silicon substrate 1 by using a helium ion beam 2, and the single crystal silicon directly below the implantation point is denatured by the interaction of helium ions and silicon, thereby forming an amorphized region 3 having a water-drop shape in cross section. And then selectively corroding the region 3 by using a wet etching agent to obtain the nano flow channel structure 4 with the cross section of a water drop shape and an upper end opening. And finally, depositing a layer of film 5 on the surface of the sample by using a chemical/physical vapor deposition method, and closing the upper end opening of the nano flow channel structure to obtain a closed nano flow channel structure 6.
The method provided by the invention can process the flow channel structure with the nanometer inner diameter, has high manufacturing precision, and does not need to use photoresist or a sacrificial layer in the processing process. Compared with other main flow processes, the method has the advantages that the method only needs one ion implantation and one chemical wet etching, has simple manufacturing steps, does not need multiple etching, does not need a bonding process to realize flow channel sealing, and greatly reduces the process complexity. Therefore, the method has lower cost and higher process reliability, is easy to integrate with the existing micro-channel processing technology, and can be used for manufacturing high-precision nano-fluidic chip devices.
In order to further understand the present invention, the following description will explain the method for manufacturing a self-sealing nano-channel according to the present invention by referring to examples, and the scope of the present invention is not limited by the following examples.
Example 1:
step 1: helium ion beam is used to implant the desired two-dimensional pattern of nano-channel structures on a monocrystalline silicon substrate.
Step 2: and (3) corroding the sample obtained in the step (1) by using a wet etching agent to form a nano runner structure with a water drop-shaped cross section and an opening at the upper end.
Step 3: and (3) placing the sample obtained in the step (2) into chemical/physical vapor deposition equipment, and depositing a layer of film to enable the upper end of the drop-shaped nano flow channel to be closed, so as to form a closed nano flow channel structure.
Referring to fig. 3, fig. 3 is an SEM characterization image of the nano-channel structure fabricated in example 1. Step 1, step 2 and step 3 are sequentially carried out from top to bottom.
The helium ion beam implantation in the step 1 is to implant high-energy helium ions into a specific position area of a sample by using a helium ion microscope. The ion energy was 30keV. The substrate material is monocrystalline silicon.
Wherein, the wet etching agent in the step 2 is 40 percent HF and 33 percent H 2 O 2 The solution was mixed in a volume ratio of 1:5. The etching time is 10min, the section of the obtained nano flow channel structure is shown in fig. 4, fig. 4 is a high-resolution imaging photograph of the section of the nano flow channel structure after the processing of the embodiment 1 is completed, the inner diameter of the nano flow channel is 150nm, and the center depth of the flow channel is 250nm.
Wherein, the thin film deposition equipment used in the step 3 is ALD, and the deposited thin film material is SiO 2 The deposition thickness was 60nm.
Example 2:
step 1: helium ion beam is used to implant the desired two-dimensional pattern of nano-channel structures on a monocrystalline silicon substrate.
Step 2: and (3) corroding the sample obtained in the step (1) by using a wet etching agent to form a nano runner structure with a water drop-shaped cross section and an opening at the upper end.
Step 3: and (3) placing the sample obtained in the step (2) into chemical/physical vapor deposition equipment, and depositing a layer of film to enable the upper end of the drop-shaped nano flow channel to be closed, so as to form a closed nano flow channel structure.
The helium ion beam implantation in the step 1 is to implant high-energy helium ions into a specific position area of a sample by using a helium ion microscope. The ion energy was 30keV. The substrate material is monocrystalline silicon.
Wherein, the wet etching agent in the step 2 is 40 percent HF and 33 percent H 2 O 2 The solution was mixed in a volume ratio of 10:1. The etching time is 1min, the section of the obtained nano flow channel structure is shown in fig. 5, fig. 5 is a high-resolution imaging photograph of the section of the nano flow channel structure after the processing of the embodiment 2 is completed, the inner diameter of the nano flow channel is 30nm, and the center depth of the flow channel is 150nm.
Wherein the thin film deposition equipment used in the step 3 is ALD, and the deposited thin film material is Al 2 O 3 The deposition thickness was 30nm.
Example 3:
step 1: helium ion beam is used to implant the desired two-dimensional pattern of nano-channel structures on a monocrystalline silicon substrate.
Step 2: and (3) corroding the sample obtained in the step (1) by using a wet etching agent to form a nano runner structure with a water drop-shaped cross section and an opening at the upper end.
Step 3: and (3) placing the sample obtained in the step (2) into chemical/physical vapor deposition equipment, and depositing a layer of film to enable the upper end of the drop-shaped nano flow channel to be closed, so as to form a closed nano flow channel structure.
The helium ion beam implantation in the step 1 is to implant high-energy helium ions into a specific position area of a sample by using a helium ion microscope. The injection pattern is a straight line, the top view of the obtained nano flow channel structure is shown in fig. 6, and fig. 6 is a top view imaging photograph of the nano flow channel structure after the processing of example 3 is completed. The ion energy was 10keV. The substrate material is monocrystalline silicon. The inner diameter of the nano flow channel is 100nm, and the center depth of the flow channel is 100nm.
Wherein, the wet etching agent in the step 2 is 40 percent HF and 33 percent H 2 O 2 The solutions were mixed in a volume ratio of 1:50. The etching time was 120min.
Wherein, the thin film deposition equipment used in the step 3 is an electron beam evaporation coating machine, the deposited thin film material is Pt, and the deposited thickness is 5nm.
Example 4:
step 1: helium ion beam is used to implant the desired two-dimensional pattern of nano-channel structures on a monocrystalline silicon substrate.
Step 2: and (3) corroding the sample obtained in the step (1) by using a wet etching agent to form a nano runner structure with a water drop-shaped cross section and an opening at the upper end.
Step 3: and (3) placing the sample obtained in the step (2) into chemical/physical vapor deposition equipment, and depositing a layer of film to enable the upper end of the drop-shaped nano flow channel to be closed, so as to form a closed nano flow channel structure.
The helium ion beam implantation in the step 1 is to implant high-energy helium ions into a specific position area of a sample by using an ion implanter. The injection pattern is a serpentine curve, the top view of the obtained nano-runner structure is shown in fig. 7, and fig. 7 is a top view imaging photograph of the nano-runner structure after the processing of example 4 is completed. The ion energy was 150keV. The substrate material is monocrystalline silicon. The inner diameter of the nano flow channel is 500nm, and the central depth of the flow channel is 800nm
Wherein, the wet etching agent in the step 2 is 40 percent HF and 33 percent H 2 O 2 The solution was mixed in a volume ratio of 1:20. The etching time was 30min.
Wherein, the film deposition equipment used in the step 3 is a magnetron sputtering coating machine, the deposited film material is Cu, and the deposition thickness is 200nm.
The method provided by the invention can process the self-sealing flow channel structure with the nano-scale inner diameter, has the advantages of simple steps, high processing efficiency, accurate regulation and control of technological parameters, easiness in integration with the existing micro-flow channel processing technology, and can be used for manufacturing high-precision nano-flow control chip devices with the nano-scale inner diameter and the nano-scale positioning precision.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (4)
1. The manufacturing method of the self-sealing nano flow channel is characterized by comprising the following steps of:
a) Injecting a required two-dimensional pattern of the nano flow channel structure on the monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional pattern of the nano flow channel structure on the surface;
the helium ion beam implantation equipment is selected from a helium ion microscope or an ion implanter, and the ion energy of the helium ion beam implantation is 1-200 keV;
b) Corroding the two-dimensional graph of the monocrystalline silicon substrate obtained in the step A) by using a wet etching agent to obtain the monocrystalline silicon substrate with a nano flow channel structure, wherein the nano flow channel structure is in a water drop shape in cross section and is provided with an opening at the upper end, the inner diameter of the nano flow channel structure is 150-500 nm, and the central depth is 250-800 nm;
the wet etching agent is a mixed solution of HF with the mass fraction of 40% and H2O2 with the mass fraction of 33%, the volume ratio is 100:1-1:100, and the etching time is 0.1-120 min
C) Depositing a layer of film on the surface and the horizontal surface of the nano flow channel structure of the monocrystalline silicon substrate obtained in the step B), and sealing the upper end of the nano flow channel structure through deposition to form a closed nano flow channel structure; the thickness of the deposited film is 5-500 nm;
the manufacturing method does not require the use of photoresist or a sacrificial layer.
2. The method of manufacturing according to claim 1, wherein the single crystal silicon substrate comprises a P-type single crystal silicon substrate, an N-type doped single crystal silicon substrate, an intrinsic silicon wafer single crystal silicon substrate, an SOI wafer, or a silicon thin film material.
3. The method of claim 1, wherein the deposition is selected from chemical vapor deposition or physical vapor deposition, and the apparatus for deposition is selected from ALD, PECVD, LPCVD, PLD, magnetron sputter coater, electron beam evaporation coater, thermal evaporation coater, or ion beam coater.
4. The method of manufacturing according to claim 1, wherein the deposited material comprises SiO 2 、SiN x 、TiO 2 、TiN、HfO 2 、Al 2 O 3 、Fe 3 O 4 AlN, ti, au, ag, pt, cr, cu, W, ni or Mo.
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