CN109632899A - A kind of nano-pore manufacturing method of controllable precise - Google Patents
A kind of nano-pore manufacturing method of controllable precise Download PDFInfo
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Abstract
The present invention relates to the technical fields of nanoprocessing, more specifically, it is related to a kind of nano-pore manufacturing method of controllable precise, it include: installation first electrode silk and second electrode silk, in one end insertion sap cavity of the first electrode silk, need to form the position of nano-pore on the end thereof contacts chip of the second electrode silk；In the hydrophilic-structure of the surface of second electrode silk processing channel form, and using the surface of salting liquid wetting second electrode silk；The other end of first electrode silk and the other end of second electrode silk are powered and apply voltage at the both ends of chip；When the aperture of nano-pore is constantly extended to required aperture, stop applying voltage immediately；Clean chip and drying.The present invention is not only able to achieve the accurate positioning of nano-pore, and it is able to achieve the accurate manufacture of the nano-pore in required aperture, manufacturing method is simple and efficient, applied widely, solves the problems, such as that electrical breakdown manufacture nano-pore can not be accurately positioned, focused ion beam manufactures Aperture uncertainty.
Description
Technical field
The present invention relates to the technical fields of nanoprocessing, more particularly, to a kind of nano-pore manufacturer of controllable precise
Method.
Background technique
According to the composition material of nano-pore, nano-pore technology be can be roughly divided into two types.One is related to biomaterial
" biological nano hole ", another kind is " solid nano hole " relevant to semiconductor material.Biological nano hole and solid nano hole
The most common DNA sequencing method being used in conjunction with is the variation detected in DNA transport process by the ionic current of nano-pore, and
The nucleotide of four seed types is identified from the variation of particle electric current.Due to the architectural difference very little of each nucleic acid molecule, it is
It extracts and is changed by the ionic current that the nucleotide of four seed types generates, the diameter of nano-pore must be with the diameter of DNA identical
On the order of magnitude；In addition to this, in order to spatially distinguish each nucleotide in DNA, the Hou Su of nano-pore also must and nucleosides
The distance between acid is in same order.
Although biological nano hole provides bigger sensitivity and lower noise characteristic, since its fragile lipid is double
Layer structure, and be limited under very special operating condition and use, and need to be very small molecule by it；And
Solid nano hole provides higher durability, better thermodynamic property, more flexible dimension and shape adjustment capability, has
Conducive to mass production and reduce production cost.Usually focused ion beam or electronic beam drilling, aperture and hole are used in film surface
Pattern can by adjusting light beam parameters or it is subsequent using scanning electron microscope (SEM) or transmission electron microscope (TEM) into
Row shrinkage cavity, reaming and the variation of hole pattern.But since the difference of ion beam type using the uncertainty of parameter is difficult essence
True controllable electric beamlet and shaped ion beam are shaped to the nano-pore in required aperture.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of nano-pore manufacturing method of controllable precise,
The accurate manufacture of the nano-pore in aperture needed for can be realized the accurate positioning of nano-pore and realizing, manufacturing method are simple and efficient,
It has wide range of applications.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of nano-pore manufacturing method of controllable precise is provided, the nano-pore is opened on chip, and the chip is fixed
In liquid pool, the liquid pool is equipped with the sap cavity filled with salting liquid；The manufacturing method the following steps are included:
S10., first electrode silk and second electrode silk be installed, in one end insertion sap cavity of the first electrode silk, described the
It needs to form the position of nano-pore on the end thereof contacts chip of two wire electrodes；
S20. in the hydrophilic-structure of the surface of second electrode silk processing channel form, and using the second electricity of salting liquid wetting
The surface of polar filament；
S30. the other end of the other end of first electrode silk and second electrode silk, which is powered, applies voltage at the both ends of chip；
S40. when the aperture of nano-pore is constantly extended to required aperture, stop applying voltage immediately；
S50. chip and drying are cleaned.
The nano-pore manufacturing method of controllable precise of the invention forms the position of nano-pore needed for being moved to second electrode silk
It sets and is processed, realize the accurate positioning of nano-pore；Size by monitoring real-time current controls nano-pore aperture, needed for realization
The accurate manufacture of the nano-pore in aperture；The present invention solves electrical breakdown manufacture nano-pore and can not be accurately positioned, focused ion beam system
Make the problem of Aperture uncertainty.
Preferably, the chip surface is equipped with membrane structure, and the membrane structure is selected from nanoscale single thin film, micron
Grade single thin film, micron order multi-layer compound film, one of nanoscale multi-layer compound film, the membrane structure with a thickness of
5nm~100nm.The present invention can be in meter level single thin film, micron order single thin film, micron order multi-layer compound film, nanoscale
Nano-pore is prepared on multi-layer compound film, it is applied widely.
Preferably, the membrane structure is selected from silicon nitride film, silicon oxide film or nitridation silicon/oxidative silicon/silicon nitride three
One of layer film.
Preferably, in step S10, the first electrode silk, second electrode silk are selected from one of silver, copper, gold, aluminium, tungsten
Or it is a variety of compound, the first electrode silk, second electrode silk diameter of section be 100nm~10 μm.Silver, copper, gold, aluminium, tungsten
And its good conductivity of alloy, convenient for the application of subsequent voltage.
Preferably, in step S20, in second electrode silk table face, the mode of processing is selected from laser processing, focused ion beam adds
One of work, transmission electron microscope or multiple combinations；The hydrophilic-structure is selected from one of triangle, diamond shape, rectangular
Or a variety of combination.The setting of hydrophilic-structure infiltrates convenient for salting liquid in second electrode silk table face.
Preferably, in step S20, the salting liquid is selected from sodium chloride solution, Klorvess Liquid, lithium chloride solution, chlorination
One of calcium solution, lanthanum chloride solution or a variety of mixing；The PH of the salting liquid is 6.0~8.0, and salting liquid PH, which is adjusted, to be used
Buffer is selected from one of Tris-HCl buffer, HEPES buffer solution, PBS buffer solution.In salting liquid be added dropwise buffer with
Adjust the PH of salting liquid.
Preferably, in step S30, the voltage is constant voltage, the pulse voltage at same time interval or different time
The pulse voltage at interval, the voltage are 0.1V to 30V.
Preferably, in step S40, the real-time current for flowing through first electrode silk and second electrode silk is obtained, passes through electricity in real time
The variation of stream judges the form of nano-pore:
A. real-time current remains unchanged, and nano-pore is not yet formed；
B. real-time current mutates, and nano-pore is formed；
C. real-time current is gradually increased, and nano-pore aperture is continuously increased；
D. real-time current increases to setting electric current, and required nano-pore completes the process.
Preferably, in step S50, the cleaning of chip is rinsed using deionized water at least 5 times of degassing, and the drying of chip is adopted
It is dried with the suction of aspirator.
Preferably, the one end of one end and second electrode silk far from chip of the first electrode silk far from chip is connected with
Current amplifier, the current amplifier connect PC by USB interface.
Compared with prior art, the beneficial effects of the present invention are:
(1) the nano-pore manufacturing method of controllable precise of the invention forms nano-pore needed for being moved to second electrode silk
Position processed, realize the accurate positioning of nano-pore；Size by monitoring real-time current controls nano-pore aperture, realizes
The accurate manufacture of the nano-pore in required aperture；Manufacturing method is simple and efficient, and solving electrical breakdown manufacture nano-pore can not be accurate
Positioning, focused ion beam manufacture the problem of Aperture uncertainty.
(2) present invention can in silicon nitride film, silicon oxide film and other micron orders or nanoscale single thin film or
Nano-pore is prepared on silicon nitride/silicon/silicon nitride three-layer thin-film and other micron orders or nanoscale multi-layer compound film, is applicable in model
It encloses extensively.
Detailed description of the invention
Fig. 1 is the flow diagram of the nano-pore manufacturing method of controllable precise of the invention.
Fig. 2 is the structural schematic diagram of first electrode silk of the invention.
Fig. 3 is the structural schematic diagram of second electrode silk of the invention.
Fig. 4 is the structural schematic diagram after second electrode silk wetting of the invention.
Status diagram when Fig. 5 is the nano-pore manufacture of controllable precise of the invention.
Status diagram when Fig. 6 is the nano-pore formation of controllable precise of the invention.
In attached drawing: 1- chip；2- liquid pool；21- sap cavity；3- first electrode silk；4- second electrode silk；41- hydrophilic-structure；5-
Membrane structure；6- nano-pore.
Specific embodiment
The present invention is further illustrated With reference to embodiment.Wherein, attached drawing only for illustration,
What is indicated is only schematic diagram, rather than pictorial diagram, should not be understood as the limitation to this patent；Reality in order to better illustrate the present invention
Example is applied, the certain components of attached drawing have omission, zoom in or out, and do not represent the size of actual product；To those skilled in the art
For, the omitting of some known structures and their instructions in the attached drawings are understandable.
Embodiment one
It is as shown in Figure 1 the embodiment of 6 manufacturing method of nano-pore of controllable precise of the invention, the nano-pore 6 opens up
In on chip 1, the chip 1 is fixed in liquid pool 2, and the liquid pool 2 is equipped with the sap cavity 21 filled with salting liquid；The manufacturer
Method the following steps are included:
S10., first electrode silk 3 and second electrode silk 4 are installed, one end of the first electrode silk 3 is inserted into sap cavity 21, institute
State needs to form the position of nano-pore 6 on the end thereof contacts chip 1 of second electrode silk 4；
S20. in the hydrophilic-structure 41 of the surface of the second electrode silk 4 processing channel form, and using salting liquid wetting the
The surface of two wire electrodes 4；
S30. the other end of the other end of first electrode silk 3 and second electrode silk 4, which is powered, applies electricity at the both ends of chip 1
Pressure；
S40. when the aperture of nano-pore 6 is constantly extended to required aperture, stop applying voltage immediately；
S50. chip 1 and drying are cleaned.
1 surface of chip of the present embodiment is equipped with membrane structure 5, and the membrane structure 5 is selected from nanoscale single thin film, micro-
One of meter level single thin film, micron order multi-layer compound film, nanoscale multi-layer compound film, the thickness of the membrane structure 5
Degree is 5nm~100nm.The membrane structure 5 of the present embodiment is selected from silicon nitride film, silicon oxide film or nitridation silicon/oxidative silicon/nitrogen
One of SiClx three-layer thin-film.The present invention can be in silicon nitride film, silicon oxide film and other micron orders or nanoscale list
Nanometer is prepared on layer film or silicon nitride/silicon/silicon nitride three-layer thin-film and other micron orders or nanoscale multi-layer compound film
Hole 6, it is applied widely.In addition, one end and second electrode silk 4 far from chip 1 of first electrode silk 3 are separate in the present embodiment
One end of chip 1 is connected with current amplifier, and the current amplifier connects PC by USB interface, convenient for passing through
The process of PC operation nano-pore 6.
In step S10, the first electrode silk 3, second electrode silk 4 are selected from one of silver, copper, gold, aluminium, tungsten or a variety of
It is compound, the first electrode silk 3, second electrode silk 4 diameter of section be 100nm~10 μm.Silver, copper, gold, aluminium, tungsten and its
The good conductivity of alloy, convenient for the application of subsequent voltage.
In step S20, on 4 surface of second electrode silk, the mode of processing is selected from laser processing, focused ion beam processing, transmission
One of electron microscope or multiple combinations；The hydrophilic-structure 41 is selected from one of triangle, diamond shape, rectangular or a variety of
Combination.The setting of hydrophilic-structure 41 infiltrates convenient for salting liquid on 4 surface of second electrode silk.
In step S20, the salting liquid be selected from sodium chloride solution, Klorvess Liquid, lithium chloride solution, calcium chloride solution,
One of lanthanum chloride solution or a variety of mixing；The PH of the salting liquid is 6.0~8.0, and buffer is used in salting liquid PH adjusting
Selected from one of Tris-HCl buffer, HEPES buffer solution, PBS buffer solution.Buffer is added dropwise in salting liquid to adjust salt
The PH of solution.
In step S30, the voltage is the arteries and veins of constant voltage, the pulse voltage at same time interval or different time intervals
Voltage is rushed, the voltage is 0.1V to 30V.
In step S40, the real-time current for flowing through first electrode silk 3 and second electrode silk 4 is obtained, the change of real-time current is passed through
Change the form for judging nano-pore 6:
A. real-time current remains unchanged, and nano-pore 6 is not yet formed；
B. real-time current mutates, the formation of nano-pore 6；
C. real-time current is gradually increased, and 6 aperture of nano-pore is continuously increased；
D. real-time current increases to setting electric current, and required nano-pore 6 completes the process.
In step S50, the cleaning of chip 1 uses deionized water at least 5 times flushings of degassing, and the drying of chip 1 is using suction
The suction of gas device is dried.
Embodiment two
It is as shown in Figures 2 to 6 the second embodiment of the nano-pore manufacturing method of controllable precise of the invention, the present embodiment
It is specific as follows for the Application Example of embodiment one:
Step S10 is first carried out, first electrode silk 3 and second electrode silk 4, first electrode silk 3 and second electrode silk 4 are installed
Structure it is as shown in Figure 2 to Figure 3, in one end of the first electrode silk 3 insertion sap cavity 21, one end of the second electrode silk 4
It needs to form the position of nano-pore 6 on contact chip 1；In the present embodiment, first electrode silk 3 and second electrode silk 4 are by electric conductivity
The good silver of energy is made, and the diameter of section of first electrode silk 3 and second electrode silk 4 is 1 μm.
Then step S20 is executed, in the hydrophilic-structure 41 of the surface of the second electrode silk 4 processing channel form, in this reality
It applies in example, 4 surface manufacturing condition of second electrode silk is focused ion beam processing, and hydrophilic-structure 41 is triangular structure.Using salt
For solution by the moistened surface of second electrode silk 4, the salting liquid in the present embodiment is sodium chloride brine, and the pH of salting liquid is 7.5,
The buffer used is HEPES buffer solution；As shown in Figure 3 to Figure 4.When it is implemented, configuration 1M sodium chloride solution, is used in combination
20mMHEPES buffer adjusts the pH value to 7.5, draws the configured salting liquid using liquid-transfering gun, be added dropwise
4 surface of second electrode silk placed vertically, makes its complete wetting.
Then step S30 and step S40 is executed, the other end of first electrode silk 3 and the other end of second electrode silk 4 are logical
Electricity applies voltage at the both ends of chip 1, as shown in Figure 5.The present embodiment is when implementing, in first electrode silk 3 and second electrode silk 4
Both ends connect current amplifier, current amplifier connects PC by USB interface；Using current amplifier in chip 1
Both ends apply constant 5V voltage, obtain real-time current, after a period of time, real-time current mutates, the formation of nano-pore 6, after
Continuous to apply voltage, the real-time current of acquisition is gradually increased, represents 6 aperture of nano-pore and constantly expand, use formula
The conductance in required aperture can be exported, the constant voltage is 5V, can extrapolate required electric current；It is increased to the electric current described
When required electric current, stop the voltage immediately, can be obtained the nano-pore 6 in required aperture, as shown in Figure 6.
Step S50 is finally executed, chip 1 and drying are cleaned.The present embodiment uses clean Teflon round end when implementing
Tweezers carefully take out the chip 1 from the liquid pool 2, are put into clean beaker；It will using clean glass pipet
The deionized water of 50 milliliters of degassings, which is added in the beaker, rinses the chip 1, water is sucked out, and repeat at least 5 times；Institute is used
It states clean Teflon round end tweezers and carefully takes out the chip 1 from the beaker；Gently suction is inhaled using aspirator
It is dried to its edge；It is completely dried, is deposited into clean from adsorption box to the chip 1.
By above step, the present invention provides a kind of 6 manufacturing methods of nano-pore of controllable precise, and nanometer both may be implemented
The accurate positioning in hole 6, and can realize the accurate manufacture of the nano-pore 6 in required aperture, manufacturing method is simple and efficient, applied widely
It is general, solve the problems, such as that electrical breakdown manufacture nano-pore 6 can not be accurately positioned, focused ion beam manufactures Aperture uncertainty.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (10)
1. a kind of nano-pore manufacturing method of controllable precise, the nano-pore are opened on chip, the chip is fixed on liquid pool
In, the liquid pool is equipped with the sap cavity filled with salting liquid；It is characterized in that, the manufacturing method the following steps are included:
S10., first electrode silk and second electrode silk are installed, one end of the first electrode silk is inserted into sap cavity, second electricity
It needs to form the position of nano-pore on the end thereof contacts chip of polar filament；
S20. in the hydrophilic-structure of the surface of second electrode silk processing channel form, and second electrode silk is soaked using salting liquid
Surface；
S30. the other end of the other end of first electrode silk and second electrode silk, which is powered, applies voltage at the both ends of chip；
S40. when the aperture of nano-pore is constantly extended to required aperture, stop applying voltage immediately；
S50. chip and drying are cleaned.
2. the nano-pore manufacturing method of controllable precise according to claim 1, which is characterized in that the chip surface is laid with
Have a membrane structure, the membrane structure be selected from nanoscale single thin film, micron order single thin film, micron order multi-layer compound film,
One of nanoscale multi-layer compound film, the membrane structure with a thickness of 5nm~100nm.
3. the nano-pore manufacturing method of controllable precise according to claim 2, which is characterized in that the membrane structure is selected from
One of silicon nitride film, silicon oxide film or nitridation silicon/oxidative silicon/silicon nitride three-layer thin-film.
4. the nano-pore manufacturing method of controllable precise according to claim 1, which is characterized in that in step S10, described
One wire electrode, second electrode silk are selected from one of silver, copper, gold, aluminium, tungsten or a variety of compound, the first electrode silk, second
The diameter of section of wire electrode is 100nm~10 μm.
5. the nano-pore manufacturing method of controllable precise according to claim 1, which is characterized in that in step S20, second
The mode of wire electrode surface processing is selected from one of laser processing, focused ion beam processing, transmission electron microscope or a variety of
Combination；The hydrophilic-structure is selected from one of triangle, diamond shape, rectangular or a variety of combinations.
6. the nano-pore manufacturing method of controllable precise according to claim 1, which is characterized in that in step S20, the salt
Solution is selected from one of sodium chloride solution, Klorvess Liquid, lithium chloride solution, calcium chloride solution, lanthanum chloride solution or a variety of
Mixing；The PH of the salting liquid is 6.0~8.0, and salting liquid PH adjusting is selected from Tris-HCl buffer, HEPES with buffer
One of buffer, PBS buffer solution.
7. the nano-pore manufacturing method of controllable precise according to claim 1, which is characterized in that in step S30, the electricity
Pressure be constant voltage, the pulse voltage at same time interval or different time intervals pulse voltage, the voltage be 0.1V extremely
30V。
8. the nano-pore manufacturing method of controllable precise according to claim 1, which is characterized in that in step S40, obtain stream
Real-time current through first electrode silk and second electrode silk judges the form of nano-pore by the variation of real-time current:
A. real-time current remains unchanged, and nano-pore is not yet formed；
B. real-time current mutates, and nano-pore is formed；
C. real-time current is gradually increased, and nano-pore aperture is continuously increased；
D. real-time current increases to setting electric current, and required nano-pore completes the process.
9. the nano-pore manufacturing method of controllable precise according to claim 1, which is characterized in that in step S50, chip
Cleaning is rinsed using deionized water at least 5 times of degassing, and the drying of chip is dried using the suction of aspirator.
10. the nano-pore manufacturing method of controllable precise according to any one of claims 1 to 9, which is characterized in that described
The one end of one end and second electrode silk far from chip of one wire electrode far from chip is connected with current amplifier, and the electric current is put
Big device connects PC by USB interface.
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