CN114682314A - Manufacturing method of self-sealing nano flow channel - Google Patents
Manufacturing method of self-sealing nano flow channel Download PDFInfo
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- CN114682314A CN114682314A CN202210365627.1A CN202210365627A CN114682314A CN 114682314 A CN114682314 A CN 114682314A CN 202210365627 A CN202210365627 A CN 202210365627A CN 114682314 A CN114682314 A CN 114682314A
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Abstract
The invention provides a method for manufacturing a self-sealing nano flow channel, which comprises the following steps: A) injecting a required two-dimensional graph of the nano-flow channel structure on a monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional graph 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 a nano flow channel structure; C) depositing a layer of thin 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 be used for processing the flow channel structure with the nanoscale inner diameter, and the manufacturing precision is high. 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 the structure scale in the nanometer range (several nanometers to several hundred nanometers). The nano flow channel structure is made in the microfluidic chip, so that the fluid and the nano surface interact, and the fluid characteristics different from the macro scale can be generated due to the common influence of van der waals force, electrostatic force, capillary acting force and other effects. These features have important implications and wide application in fluid manipulation, biosensing, protein detection, and DNA sequencing technologies. Therefore, in order to explore the special properties of the fluid in the micro-nano fluidic system, it is necessary to develop a nano flow channel processing technology which is simple, reliable and easy to integrate with the existing processing technology.
The processing technology of the current nano flow channel is mainly based on the traditional semiconductor processing technology and is realized by a plurality of procedures of glue homogenizing, electron beam lithography, film coating, etching, bonding and the like, the manufacturing mode is complex, the integration level is poor, and the processing difficulty is rapidly increased along with the reduction of the key size 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 a nano 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 flow control chip device.
The invention provides a method for manufacturing a self-sealing nano flow channel, which comprises the following steps:
A) injecting a required two-dimensional graph of the nano-flow channel structure on a monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional graph 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 a nano flow channel structure;
C) depositing a layer of thin 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 equipment for helium ion beam implantation is selected from a helium ion microscope or an ion implanter.
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%2O2The volume ratio of the mixed solution of (1) to (100: 1) - (1: 100, preferably 10: 1) - (1: 50.
Preferably, the corrosion time is 0.1-120 min, preferably 2-30 min.
Preferably, the nano flow channel structure is in a water drop shape in cross section shape and has 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 SiO2、SiNx、TiO2、TiN、HfO2、Al2O3、Fe3O4AlN, 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 method for manufacturing a self-sealing nano flow channel, which comprises the following steps: A) injecting a required two-dimensional graph of the nano-flow channel structure on a monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional graph 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 a nano flow channel structure; C) depositing a layer of thin 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 be used for processing the flow channel structure with the nanoscale inner diameter, the manufacturing precision is high, and photoresist or a sacrificial layer is not required to be used in the processing process. The invention only needs one-time ion implantation and one-time chemical wet etching, has simple manufacturing steps compared with other mainstream processes, does not need multiple times of etching, does not need to realize flow channel sealing through a bonding process, 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 nanochannel according to the present invention;
FIG. 2 is a schematic view of a fabrication method of a nanochannel structure according to the present invention;
FIG. 3 is an SEM representation of the nanofluidic structure processed and fabricated in example 1;
FIG. 4 is a high resolution image of the processed cross section of the nano-channel structure in example 1;
FIG. 5 is a high resolution image of the processed cross section of the nano-channel structure in example 2;
FIG. 6 is a top view image of the nano-flow channel structure after processing in example 3;
fig. 7 is a top view image of the nanofluidic structure of example 4 after processing.
Detailed Description
The invention provides a method for manufacturing a self-sealing nano flow channel, which comprises the following steps:
A) injecting a required two-dimensional graph of the nano-flow channel structure on a monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional graph 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 a nano flow channel structure;
C) depositing a layer of thin 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 thin film material.
And (3) after preparing the monocrystalline silicon substrate, injecting a required two-dimensional graph of the nano flow channel structure into the monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional graph of the nano flow channel structure on the surface.
The shape of the two-dimensional graph of the nano-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 according to the requirement.
The equipment for the 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 implantation is 1 to 200keV, preferably 1keV, 5keV, 10keV, 50keV, 100keV, 150keV, 200keV, or any value between 1 to 200 keV.
And after obtaining the monocrystalline silicon substrate with the two-dimensional graph of the nano flow channel structure on the surface, corroding the two-dimensional graph of the obtained monocrystalline silicon substrate by using a wet etching agent to obtain the monocrystalline silicon substrate with the nano flow channel structure.
Wherein the wet etching agent is HF with the mass fraction of 40% and H with the mass fraction of 33%2O2The volume ratio of the mixed solution (b) is 100:1 to 1:100, preferably 10:1 to 1:50, and more preferably any value between 10:1, 5:1, 1:5, 1:10, 1:20, 1:30, 1:40, 1:50, or 10:1 to 1: 50.
The etching time is 0.1-120 min, preferably 2-30 min, and more preferably 2, 5, 10, 15, 20, 25, 30, or any value between 2-30 min.
After the corrosion is finished, the formed nano flow channel structure is in a water drop shape in cross section shape and is provided with an opening at the upper end.
In the invention, the inner diameter of the nano flow channel structure is 30-500 nm, preferably 30, 50, 100, 150, 200, 250, 300, 350, 400, 450, 500 or any value between 30-500 nm, and the center depth is 100-800 nm, preferably 100, 200, 300, 400, 500, 600, 700, 800 or any value between 100-800 nm.
After obtaining the monocrystalline silicon substrate with the nano flow channel structure, 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 deposition is selected from chemical vapor deposition or physical vapor deposition, and the deposition equipment is selected from ALD, PECVD, LPCVD, PLD, magnetron sputtering coating machine, electron beam evaporation coating machine, thermal evaporation coating machine or ion beam coating machine.
The deposition material comprises SiO2、SiNx、TiO2、TiN、HfO2、Al2O3、Fe3O4AlN, Ti, Au, Ag, Pt, Cr, Cu, W, Ni or Mo, preferably SiO2、Al2O3Pt or Cu.
The thickness of the deposited film is 5-500 nm, preferably 5, 10, 50, 100, 200, 300, 400, 500, or any value between 5-500 nm. 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. 1-2, fig. 1 is a schematic flow chart of a manufacturing method of a self-sealing nanochannel provided by the invention.
Fig. 2 is a schematic diagram of a method for fabricating a nanochannel structure according to the present invention. In fig. 2, first, a two-dimensional pattern of a desired nano-channel structure is implanted into a surface of a single-crystal silicon substrate 1 by using a helium ion beam 2, and the single-crystal silicon immediately below the implantation point is denatured by the interaction between helium ions and silicon, thereby forming an amorphized region 3 having a droplet-shaped cross section. And selectively corroding the region 3 by using a wet etching agent to obtain the nano flow channel structure 4 with a water drop-shaped section and an opening at the upper end. And finally, depositing a layer of film 5 on the surface of the sample by using a chemical/physical vapor deposition method, and closing an opening at the upper end of the nano flow channel structure to obtain a closed nano flow channel structure 6.
The method provided by the invention can be used for processing the flow channel structure with the nanoscale inner diameter, the manufacturing precision is high, and photoresist or a sacrificial layer is not required to be used in the processing process. The invention only needs one-time ion implantation and one-time chemical wet etching, has simple manufacturing steps compared with other mainstream processes, does not need multiple times of etching, does not need to realize flow channel sealing through a bonding process, 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.
For further understanding of the present invention, the following describes a method for manufacturing a self-sealing nanochannel according to the present invention with reference to the following embodiments, and the scope of the present invention is not limited by the following embodiments.
Example 1:
step 1: a helium ion beam is used to implant a two-dimensional pattern of a desired nanofluidic structure on a single-crystal silicon substrate.
Step 2: and (3) corroding the sample obtained in the step (1) by using a wet etching agent to form a nano flow channel structure with a water drop-shaped cross section and an opening at the upper end.
And step 3: and (3) putting the sample obtained in the step (2) into chemical/physical vapor deposition equipment, and depositing a layer of film to seal the upper end of the water-drop-shaped nano flow channel to form a closed nano flow channel structure.
Referring to fig. 3, fig. 3 is an SEM representation of the nanofluidic structure fabricated in example 1. And the step 1, the step 2 and the step 3 are sequentially performed from top to bottom.
Wherein, the helium ion beam implantation in the step 1 is to implant high-energy helium ions into a specific position area of the sample by using a helium ion microscope. The ion energy was 30 keV. The substrate material is monocrystalline silicon.
Wherein, the wet etching agent in the step 2 is 40 percent of HF and 33 percent of H2O2Mixing the solution according to the volume ratio of 1: 5. The etching time is 10min, the cross section of the obtained nano flow channel structure is shown in fig. 4, and fig. 4 is a high-resolution imaging photo of the cross section of the nano flow channel structure processed in example 1, wherein the inner diameter of the nano flow channel is 150nm, and the center depth of the flow channel is 250 nm.
Wherein, the thin film deposition equipment used in the step 3 is ALD, and the deposited thin film material is SiO2The deposition thickness was 60 nm.
Example 2:
step 1: a helium ion beam is used to implant a two-dimensional pattern of a desired nanofluidic structure on a single-crystal silicon substrate.
Step 2: and (3) corroding the sample obtained in the step (1) by using a wet etching agent to form a nano flow channel structure with a water drop-shaped cross section and an opening at the upper end.
And step 3: and (3) putting the sample obtained in the step (2) into chemical/physical vapor deposition equipment, and depositing a layer of film to seal the upper end of the water-drop-shaped nano flow channel to form a closed nano flow channel structure.
Wherein, the helium ion beam implantation in step 1 is to implant high-energy helium ions into a specific position area of the sample by using a helium ion microscope. The ion energy was 30 keV. The substrate material is monocrystalline silicon.
Wherein, the wet etching agent in the step 2 is 40 percent of HF and 33 percent of H2O2Mixing the solution according to the volume ratio of 10: 1. The etching time was 1min, the cross section of the obtained nano flow channel structure was as shown in fig. 5, and fig. 5 is a high resolution imaging photograph of the cross section of the nano flow channel structure after the processing of example 2, the inner diameter of the nano flow channel was 30nm, and the center depth of the flow channel was 150 nm.
Wherein, the thin film deposition equipment used in the step 3 is ALD, and the deposited thin film material is Al2O3The deposition thickness was 30 nm.
Example 3:
step 1: a helium ion beam is used to implant a two-dimensional pattern of a desired nanofluidic structure on a single-crystal silicon substrate.
Step 2: and (3) corroding the sample obtained in the step (1) by using a wet etching agent to form a nano flow channel structure with a water drop-shaped cross section and an opening at the upper end.
And step 3: and (3) putting the sample obtained in the step (2) into chemical/physical vapor deposition equipment, and depositing a layer of film to seal the upper end of the water-drop-shaped nano flow channel to form a closed nano flow channel structure.
Wherein, the helium ion beam implantation in the step 1 is to implant high-energy helium ions into a specific position area of the sample by using a helium ion microscope. The injection pattern is a straight line, the top view of the obtained nano-channel structure is shown in fig. 6, and fig. 6 is a top-view imaging photo of the nano-channel structure after the processing of example 3. The ion energy was 10 keV. The substrate material is monocrystalline silicon. The inner diameter of the nano flow channel is 100nm, and the central depth of the flow channel is 100 nm.
Wherein, the wet etching agent in the step 2 is 40 percent of HF and 33 percent of H2O2Mixing the solution according to the volume ratio of 1: 50. The etching time was 120 min.
Wherein the film deposition equipment used in the step 3 is an electron beam evaporation coating machine, the deposited film material is Pt, and the deposition thickness is 5 nm.
Example 4:
step 1: a helium ion beam is used to implant a two-dimensional pattern of a desired nanofluidic structure on a single-crystal silicon substrate.
Step 2: and (3) corroding the sample obtained in the step (1) by using a wet etching agent to form a nano flow channel structure with a water drop-shaped cross section and an opening at the upper end.
And 3, step 3: and (3) putting the sample obtained in the step (2) into chemical/physical vapor deposition equipment, and depositing a layer of film to seal the upper end of the water-drop-shaped nano flow channel to form a closed nano flow channel structure.
Wherein, the helium ion beam implantation in the step 1 is to implant high-energy helium ions into a specific position area of the sample by using an ion implanter. The injection pattern is a serpentine curve, the top view of the obtained nano-channel structure is shown in fig. 7, and fig. 7 is a top-view image of the nano-channel structure after the processing of example 4. The ion energy was 150 keV. 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 of HF and 33 percent of H2O2Mixing the solution according to the volume ratio of 1: 20. The etching time was 30 min.
Wherein the film deposition equipment used in the step 3 is a magnetron sputtering coating machine, the material of the deposited film is Cu, and the deposition thickness is 200 nm.
The method provided by the invention can be used for processing the self-closed flow channel structure with the nanoscale inner diameter, has the advantages of simple steps, high processing efficiency and accurately adjustable and controllable process parameters, is easy to integrate with the existing micro-flow channel processing technology, and can be used for manufacturing high-precision nano-fluidic chip devices with the nanoscale inner diameter and the nanoscale positioning precision.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for manufacturing a self-sealing nano flow channel is characterized by comprising the following steps:
A) injecting a required two-dimensional graph of the nano-flow channel structure on a monocrystalline silicon substrate by using helium ion beams to obtain the monocrystalline silicon substrate with the two-dimensional graph 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 a nano flow channel structure;
C) depositing a layer of thin 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.
2. The method of claim 1, wherein the helium ion beam implantation equipment is selected from a helium ion microscope or an ion implanter.
3. The method according to claim 1, wherein the ion energy of the helium ion beam implantation is 1 to 200 keV.
4. The manufacturing method 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.
5. The method according to claim 1, wherein the wet etchant comprises 40% by mass of HF and 33% by mass of H2O2The volume ratio of the mixed solution of (1) to (100: 1) to (1: 100).
6. The method according to claim 1, wherein the etching time is 0.1 to 120 min.
7. The method of claim 1, wherein the nanofluidic structure has a droplet-shaped cross-section with an open top.
8. The method of claim 1, wherein the deposition is selected from chemical vapor deposition or physical vapor deposition and the deposition equipment is selected from ALD, PECVD, LPCVD, PLD, magnetron sputter coater, electron beam evaporation coater, thermal evaporation coater or ion beam coater.
9. The method of manufacturing of claim 1, wherein the deposited material comprises SiO2、SiNx、TiO2、TiN、HfO2、Al2O3、Fe3O4AlN, Ti, Au, Ag, Pt, Cr, Cu, W, Ni or Mo.
10. The method of claim 1, wherein the deposited film has a thickness of 5 to 500 nm.
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