CN107459264A - A kind of method for preparing single nano-pore interface on the glass substrate - Google Patents
A kind of method for preparing single nano-pore interface on the glass substrate Download PDFInfo
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- CN107459264A CN107459264A CN201710672630.7A CN201710672630A CN107459264A CN 107459264 A CN107459264 A CN 107459264A CN 201710672630 A CN201710672630 A CN 201710672630A CN 107459264 A CN107459264 A CN 107459264A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
- C03C23/004—Other surface treatment of glass not in the form of fibres or filaments by irradiation by electrons, protons or alpha-particles
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Abstract
The present invention relates to a kind of method for preparing single nano-pore interface on the glass substrate, it is included in glass baseplate side and sets the etching liquid containing HF, opposite side is provided with alkaline electrolyte solution, the etching liquid and the alkaline electrolyte solution at least cover an etch areas, the etch areas corresponds to view field of the single nano-pore in the glass substrate surface, apply DC voltage to the etching liquid and alkaline electrolyte solution to perform etching, and conducting of the etching process to glass baseplate both sides electric current is monitored with galvanometer.This method has the characteristics of can forming single high-aspect-ratio nano-pore, preparation method is without super-clean environment and expensive equipment, prepared nano-pore interface shows the features such as significant ion concentration polarization and ion rectification, is widely used as micro-nano-fluidic control interface in micro-nano-fluidic control effect study；During the single hole interface of preparation can be widely used in cell, nano-particle or even molecule manipulation and detect.
Description
Technical field
The present invention relates to micro-nano-fluidic control technical field, and in particular to one kind prepares single nano-pore circle on the glass substrate
The method in face.
Background technology
The interface of single hole characteristic is analyzed in unicellular (micro-meter scale) and unimolecule (nanoscale), or even nucleic acid is surveyed
There is potential using value in sequence.But the processing at single duct feature interface and preparation have certain challenge, particularly
The single hole interface of nanoscale.Single nano-pore interface is broadly divided into two classes, when solid-state or artificial, second, biological.
The ion channel Forming Mechanism on cell membrane is copied in biological nano hole, by the protein molecular with hole characteristic and is assembled
Formed on to immobilized artificial membrane.Because biological nano hole stability and yardstick modulability are limited, so solid nano hole is especially closed
Note.
It has been reported that be used for prepare the solid material at single hole interface and include monocrystalline silicon, polymer, silicon nitride, graphene
With glass etc., the single hole carried out thereon is machined with a variety of methods.Such as the costliness such as heavy ion trace etching, focused ion beam
Equipment, very high requirement it is also proposed to the environment of processing.It is also to form micron and nanometer list by glass pipe end hot melt stretching
The method at hole interface, has been obtained for extensive use in membrane elastic property.By automatic drawing device can also obtain glass or
Person's quartz nanometer single hole interface.It can also be positioned using the laser of focusing in glass surface and process single hole and its array.Glass
Glass is readily available and widely used material, in the preparation of membrane elastic property and single micropore or even nano-pore
There is open report.The main method drawn using hot melt and machinery forms list in the end face of tubular glass material in the prior art
Hole interface, and complex operation, cost are high, can not prepare to form single hole interface on the surface of glass material or optional position.Such as
Where glass surface, which introduces the technology with single nanometer hole characteristic interface, has no report.
The content of the invention
(1) technical problems to be solved
In order to solve the above mentioned problem of prior art, the present invention provides one kind and prepares single nano-pore on the glass substrate
The method at interface, it is to prepare the side with single hole characteristic on the surface of glass material based on electric field-assisted wet etching
Method, method is simple to operate, easy, and the nano-pore interface prepared can incite somebody to action in nano-particle or even molecule manipulation and detection
It is used widely.
(2) technical scheme
In order to achieve the above object, the main technical schemes that the present invention uses include：
A kind of method for preparing single nano-pore interface on the glass substrate, it is included in the setting of glass baseplate side and contained
There is HF etching liquid, opposite side is provided with alkaline electrolyte solution, and the etching liquid and the alkaline electrolyte solution at least cover
One etch areas of lid, the etch areas correspond to view field of the single nano-pore in the glass substrate surface,
Apply DC voltage to the etching liquid and alkaline electrolyte solution to perform etching, and etching process is monitored to institute with galvanometer
State the current lead-through of glass baseplate both sides.
As a kind of preferred scheme for preparing single nano-pore interfacial process as described above, work as current lead-through, stop carving
Erosion, is cleaned.
Further, the stopping etching stopping applying voltage and removes etching liquid.
As a kind of preferred scheme for preparing single nano-pore interfacial process as described above, work as current lead-through, stop applying
Voltage, and carry out the overetch less than or equal to 60s.
Current lead-through as described above refers to that the electric current of the galvanometer increases suddenly.
As a kind of preferred scheme for preparing single nano-pore interfacial process as described above, the glass baseplate side
First area includes the etch areas, and the first area is corroded in the region in addition to the etch areas by resistance to HF
Material covers,
The etching liquid contacts and only contacts the material of the resistance to HF corrosion of the first area and the etch areas.
As a kind of preferred scheme for preparing single nano-pore interfacial process as described above, the alkaline electrolyte solution
For the alkaline electrolyte solution with ionic conductivity；Such as can use 0.05~1.0 moL/L Tris-HCl, 0.05~
1.0moL/L Na2CO3-NaHCO3Deng solution.The etching liquid is the HF aqueous solution or the volume ratio that mass fraction is 2~20%
For or volume ratio be HF:H2O2：HAC=2：1：1、HF:H2O2：HNO3=2：1：1 solution；The etching liquid connection is described straight
Flow the negative pole of voltage, the alkaline electrolyte solution connects the positive pole of the DC voltage, the DC voltage 0.2~
Between 200V.
As a kind of preferred scheme for preparing single nano-pore interfacial process as described above, the cleaning 1-3mol/L
Alkaline solution rinse and soak 1.5~3h, use deionized water rinsing afterwards.
Further, the cleaning is rinsed with 2.5mol/LNaOH solution and soaks 2h.
As a kind of preferred scheme for preparing single nano-pore interfacial process as described above, the glass baseplate side
First area includes the etch areas, and the first area is corroded in the region in addition to the etch areas by resistance to HF
Material covers,
The etching liquid contacts and only contacts the material of the resistance to HF corrosion of the first area and the etch areas.
As a kind of preferred scheme for preparing single nano-pore interfacial process as described above, the glass baseplate be sheet material,
Tubing or the pipe end of closing, the thickness of the glass baseplate is 25~1000 μm；The material of the resistance to HF corrosion is optical cement or poly-
Acid imide etc..
As a kind of preferred scheme for preparing single nano-pore interfacial process as described above, the etch areas can use
Photoetching, laser ablation or mechanical scribing are carried out.
Using method as described above prepare single nano-pore interface, the single hole of the formation of preparation a diameter of 2~
500nm。
(3) beneficial effect
The beneficial effects of the invention are as follows：The present invention provides the method for preparing single nano-pore interface on the glass substrate, is
Etched using electric field-assisted, being prepared in glass surface has single nanometer hole characteristic interface, prepares the single height that nano-pore has
The characteristics of depth-to-width ratio, without super-clean environment and expensive equipment, prepared nano-pore interface is shown significantly preparation method
The features such as ion concentration polarization and ion rectification, it is widely used as micro-nano-fluidic control interface in micro-nano-fluidic control effect study.
Method provided by the invention is solved and how can introduced with single nanometer hole characteristic interface in glass surface any position
The diameter of nano-pore prepared by technical problem can be between 2~500nm.Single hole interface prepared by the inventive method can answer extensively
In cell, nano-particle or even molecule are manipulated and detected.
Brief description of the drawings
Fig. 1 is the structural representation of capillary electric field-assisted etching device in the embodiment of the present invention 2；
Fig. 2 is the current curve diagram that monitoring voltage etches step in the embodiment of the present invention 2；
Fig. 3 is in the embodiment of the present invention 2 under different HF concentration, nanometer during over etching time 0s, 30s, 60s, 90s, 150s
The variation tendency of hole resistance；
Fig. 4 is the field emission scanning electron microscope figure of capillary etch areas in the embodiment of the present invention 2；
Fig. 5 is the showing in the nano-pore interface of capillary of the DNA molecular with EB fluorescence probes in the embodiment of the present invention 3
It is intended to；
Fig. 6 is band PS-SO in the embodiment of the present invention 43Current impulse of the H nano-particles at the nano-pore interface of capillary
Variation diagram；
Fig. 7 is the measurement of nano-pore resistance, and wherein a is capillary chip structural representation, and b is capillary chip I-V bent
Line chart, c are the equivalent circuit diagram of capillary chip；
Fig. 8 is the schematic diagram of nano-pore prepared by the inventive method.
【Description of reference numerals】
1：Polyimide coating；
2：Capillary；
3：Etch areas；
4：Slide；
5：Epoxy resin；
6：Alkaline buffer solution；
7：Dc source；
8：Microgalvanometer；
9：DNA molecular with EB fluorescence probes；
10：Fluorescence heap plot point.
Embodiment
In order to preferably explain the present invention, in order to understand, below in conjunction with the accompanying drawings, by embodiment, to this hair
It is bright to be described in detail.
Embodiment 1
A kind of method for preparing single nano-pore interface on the glass substrate, this method is will in the side of glass baseplate
Etching liquid containing HF is set, and etching liquid at least covers an etch areas, and etch areas is to prepare the position of single nano-pore
Region, that is to say, that etch areas correspond to prepare formed single nano-pore glass substrate surface view field,
The corresponding opposite side in etch areas is provided with alkaline electrolyte solution, that is to say, that in the corresponding system of the opposite side of glass baseplate
The standby opposite side that form single nano-pore sets alkaline electrolyte solution, and alkaline electrolyte solution is also at least to cover one
Etch areas；Apply DC voltage using dc source to etching liquid and alkaline electrolyte solution to perform etching, and use galvanometer
Monitor the process of etching；When the current lead-through of the glass baseplate both sides, single nano-pore is prepared and formed.
When turning on the power, in the presence of electric field, etching liquid is acted on etch areas, when hole will be got through, glass
Base material both sides solution will be turned on, and at this moment connection and the DC voltage between etching liquid and alkaline electrolyte solution can be formed back
Road, now electric current can increase generation suddenly and more become, so etching process is monitored using in galvanometer, when the electric current of galvanometer is sent out
During raw hop (electric current increases suddenly), single interface nano-pore (single hole) formation, the solution conducting of glass baseplate both sides should
Stop etching immediately, that is, close the power supply of DC voltage, stop applying voltage, and remove etching liquid immediately, rapidly with 1~
3mol/L alkaline solution rinses and soaks 1.5~3h to prevent HF overetch, finally with deionized water by the alkalescence of residual
Solution is rinsed well.
The present invention is through experimental results demonstrate when closing DC voltage, do not remove etching liquid but excessively carved immediately
Erosion, overetch can form the larger nano-pore in aperture in a short time, you can with by certain after hop occurs for electric current
In time, control etching liquid etch period makes the aperture increases of nano-pore, more than continue after certain time etching can cause it is whole
Individual interfacial failure and make single nano-pore have no way of establishing.Show to refer in 60s in certain time through many experiments.I.e. in 60s
The interior control overetch time can increase the aperture of nano-pore.
Preferably, etching liquid is mainly the solution containing HF, can be the HF aqueous solution, volume that mass fraction is 2~20%
Than for HF:H2O2：HAC=2：1：1 or HF:H2O2：HNO3=2：1：1 solution.
Alkaline electrolyte solution is not contain etching liquid but the alkaline electrolyte solution with ionic conductivity；As preferably
Ground can use 0.05moL/L Tris-HCl, 0.05moL/L Na2CO3-NaHCO3Deng.
When applying DC voltage, dc source provides between 0.2~200V scopes can be selected in voltage, preferably 30~
60V；The negative pole connection etching liquid of dc source, the positive pole connection alkaline electrolyte solution of dc source, dc source and etching
Microgalvanometer is additionally provided between liquid, the electric current of whole electric field is monitored.
Preferably, sheet material, tubing or the pipe end of closing can be selected in the shape of glass baseplate, wherein, the pipe end of closing refers to one
End seal is closed, and is etched in blind end, the thickness of glass baseplate is preferably 25~1000 μm.In order to preferably obtain single receive
Metre hole, the part that can be contacted in glass baseplate side with etching liquid i.e. first area are first covered by corrosion-resistant material, especially
The material covering of resistance to HF corrosion, it is etch areas that only the local location of perforate is wanted in exposure in first area.Wherein resistance to HF is rotten
Optical cement, polyimides or polymer film etc. can be selected in the material of erosion.The local location of perforate is needed to use for exposure afterwards
Photoetching, laser ablation or mechanical scribing are carried out.
The nano-pore (single hole) of the present invention is formed in the side of etch areas, the diameter of the nano-pore of formation 2~
Between 500nm.
Embodiment 2
The present embodiment is to use device as shown in Figure 1 on the basis of embodiment 1, passes through electric field-assisted hydrofluoric acid wet method
The method that etching capillary wall prepares single hole and sign.Specific implementation method is as follows：
1st, take 5.0cm grow outer wall coating polyimide coating 1 quartz capillary 2 (internal diameter of capillary can use 50
~250 μm), 1mm polyimide coating is peelled off in the centre on the surface of capillary 2 as etch areas 3.This capillary 1 is consolidated
It is scheduled on 2.0mm × 7.5mm slide 4, the centre position of slide 4 affixes 1cm × 1cm adhesive tape, capillary wall
Etch areas be placed on the centre in adhesive tape region.Liquid storage tank (A, B, C) at capillary both ends and intermediate etch uses ring
Oxygen tree fat 5 is fixed.
2nd, 0.05 moL/L Tris-HCl are irrigated in as above fixed capillary both ends liquid storage tank (A, C) and capillary
Alkaline electrolyte solution 6, the liquid storage tank (B) in intermediate etch region 3 adds etching liquid, specifically uses mass fraction as 5%
The HF aqueous solution, it is 45V to apply dc source 7 its voltage between capillary one end and intermediate etch liquid, the negative pole of dc source
Etching liquid, the alkaline electrolyte solution of positive pole connection liquid storage tank (A) are connected, and etching process is monitored with microgalvanometer 8.Carving
During erosion at the beginning, due to there is glass baseplate stop, two terminal circuits are different, electric current 0, when single nano-pore is formed, glass
The solution connection of glass base material both sides is conductive, and the interface conducting also etched in time, electric current can increase suddenly, i.e., hop occurs for electric current,
Now, etching is terminated immediately, closes power supply, removes etching liquid.As shown in Fig. 2 the electric current that step is etched for monitoring voltage is bent
Line.And rinse capillary with 2.5mol/L NaOH solutions rapidly and soak 2h to prevent HF overetch, finally use deionization
Water rinses the NaOH of residual well stand-by.
3rd, to the conducting interface etched, the resistance of nano-pore is measured.The capillary stand-by to step 2 passes through control again
The method for continuing etching is just being regulated and controled to the yardstick of nano-pore.Do not apply voltage, fixed capillary both ends liquid storage tank and hair
Perfusion 0.05moL/L Tris-HCl alkaline electrolyte solution in tubule, pour into respectively in liquid storage tank B mass fraction for 5%,
10%HF etching liquid continues to etch 30s to existing nano-pore, soaks 2h using 2.5mol/L NaOH afterwards, rinses, point
Ce Liang not nano-pore resistance value.Similarly continue to etch the resistance value that 60s, 90s, 150s measure nano-pore.Obtained through trying many experiments
Know, nanometer bore dia and nano-pore resistance are inversely proportional, and i.e. nano-pore is smaller, and its resistance value is bigger.As shown in figure 3, etching liquid
Under 5%, 10%HF concentration, the variation tendency of nano-pore resistance during over etching time 0s, 30s, 60s, 90s, 150s, 201s.
It can be seen that preceding 60s nano-pores resistance variations steepness is big, the resistance value of nano-pore tends to be steady until nano-pore collapses after 60s
Resistance value is zero, is collapsed in the present embodiment and refers to that capillary is broken.As can be seen here, overetch can make the hole of nano-pore
Footpath increases to a certain extent, and a kind of method that the overetch time is the aperture for increasing nano-pore is controlled in 60s.
4th, the sign of solid-state single hole：The etching interface of capillary after being rinsed well to above-mentioned steps 2 carries out Flied emission and swept
Electronic Speculum (SEM) is retouched, as a result as shown in Figure 4.Wherein, the overall pattern of capillary-pipe film etch areas as shown in Figure 4 B, side it is local
Fig. 4 A are the enlarged drawing at the B1 in Fig. 4 B, and side Local map 4C is the enlarged drawing at the B2 in Fig. 4 B, and cross section is local step by step
4D → 4E of amplification → 4F scanning figure, wherein Fig. 4 D are cross section enlarged drawing at B1 in Fig. 4 B, etch institute as can be seen from Figure
Into single hole be in bowl taper, nano-pore is towards the side not being etched.Although etching surface forms multiple micropores and is distributed in etching
Region, but it is only single hole that its is penetrating, the diameter about 20nm of STH in pipe.
Embodiment 3
The present embodiment shows using the concentration polarization effect on the single hole interface prepared in embodiment 2, further exists
As confirmed the yardstick of its perforate in nanoscale on the basis of SEM in embodiment 2.1 μ g/mL ethidium bromides (EB) are irrigated in pipe
With 1 × tbe buffer solution of 3.1ng/ μ L double-stranded DNAs (dsDNA), then apply voltage, outside connection positive pole on interface
(+), middle connection negative pole (-) in capillary, divided with the dsDNA with fluorescence for being inverted microscopic imaging fluorescence method observation EB marks
Concentration polarization behavior of the son under electric field action on this interface.EB presents red under the exciting of green glow after being combined with dsDNA
Color.Its structural representation at the beginning, is visited as shown in figure 5, in the case where applying voltage 100v electric field driven with the fluorescence of EB marks
Pin dsDNA molecules are not seen in capillary, in 50s, it can be found that the electricity of DNA molecular 9 of electronegative band EB fluorescence probes
To positive pole (+) migration on the outside of pipe in the presence of, but can not be by nano-pore, but formed in the concentration of micro-nano interface glimmering
Light heap plot point 10, and a yellow spotting is revealed as under the background of details in a play not acted out on stage, but told through dialogues, it is single hole situation specifically as shown in Figure 5 a.Mostly
In the case of number, in capillary micro-nano interface it is seen that a fluorescence heap plot point, and seldom see as shown in Figure 5 b simultaneously
Two fluorescence heap plot points, three fluorescence heap plot points were met simultaneously not on the standby interface of this legal system.This example demonstrates that this hole
Yardstick in nanoscale so that there occurs concentration polarization effect, the position in hole is also show by fluorescence probe, and visualize
It is single hole in most cases that ground, which demonstrates the hole turned on interface,.
Embodiment 4
The present embodiment using etching in situ on capillary wall nano-pore, using two electrode systems of electrochemical workstation,
The single hole interface both sides prepared in example 2 apply a transmembrane voltage to show that powered nano-particle passes through this single hole
Current impulse caused by interface, from showing its single hole characteristic on the other hand.At the standby quartz glass tube interface of this legal system
Inner side loaded ribbon 89nm electronegative nano-particle aaerosol solution (i.e. 1.14 × 107Particlas/mL PS-SO3H nanometers
Particle), film loads 0.1mol/L KCl solution outside, passes through list to nano-particle under using inner side as the 6V voltages driving of negative pole
Hole interface causes current impulse change and detected.Testing result, as Fig. 6 A can be seen that non-Ghana's rice corpuscles suspend it is molten
Before liquid, the current impulse change of i-t curves is had no；Fig. 6 B are addition 1.14 × 107Particlas/mL PS-SO3H nanometers
During particle, there is negative current pulse.This shows that electronegative nano-particle is under the driving of electric field out of quartz glass tube
By, due to barrier effect, causing resistance to increase, therefore negative-going pulse occur during single hole interface.
Embodiment 5
Outside processing is characterized with SEM to the single hole and pattern at interface, also by determining interface under given supporting electrolyte
Electrical conductivity and characterized by the size of the model device to hole at interface.Specific method is as follows.
As shown in Figure 7a, the single nano-pore interface both sides perfusion 1mol/ that in embodiments of the present invention prepared by methods described
L KCl solution, 3 parts can be divided into by the resistance at interface：The resistance of liquid storage tank, resistance and interface inside capillary
Resistance.Resistance caused by each liquid storage tank can be ignored, and its equivalent circuit is as shown in Figure 7 c.Using CHI760 electrochemistry
Electric current between each liquid storage tank of work station measure under different voltages, obtains Fig. 7 b voltage (V)-electric current (I) curve, resistance
RAB、RBC、RACIt is the slope of tri- straight lines of AB, BC and AC respectively, it follows that the resistance at interface：Rnano=(RAB+RBC-RAC)/
2。
Formed, its pattern approximate cone-shape, shown in bowl-shape bottom according to scanning electron microscope (SEM) photograph observation nano-pore in embodiment 2
It is intended to as shown in Figure 8.
The diameter d of taper nano-pore can be estimated by equation below：
Wherein,
d：The diameter of nano-pore；
k：Under certain temperature, the electrical conductivity of electrolyte solution；
H：The depth of nano-pore, i.e. thickness；
Rnano：The resistance of nano-pore；
D：Big opening end diameter.
The thickness H of nano-pore etching is about 1/2 times of hole opening diameter, then the diameter of nano-pore can be estimated with formula below
Calculate；
Therefore according to as above deriving, its interface resistance value of 28 sample measures and single nanometer for being prepared to the inventive method
Wherein, with embodiment 2, difference is preparation method in the aperture in hole：1. represent 75 μm of id (inflated diameter) containing " # "
Capillary, other are 100 μm of id capillary；2. it is 5%HF etching liquids that all samples, which are mass fraction, 45V is electric
Pressure etching；3. electrolyte solution used is 1mol/L KCl during measuring resistance, at 25 DEG C, k=0.1118S/cm.
It is as shown in table 1 to measure result, by formula Rnano=(RAB+RBC-RACThe He of)/2Nanometer is calculated
The diameter in hole is 3.2 between 34nm.It can further be expanded on this basis by rear etching, can finally obtained a diameter of
500nm nano-pore.
The interface resistance value and the aperture of single nano-pore that table 1 determines
The method with single hole characteristic is prepared on the surface of glass material present invention introduces a kind of, prepared by this method
During single hole interface can be widely used in cell, nano-particle or even molecule manipulation and detect.
The above described is only a preferred embodiment of the present invention, be not the limitation that other forms are done to the present invention,
Any person skilled in the art is changed or is modified as equivalent variations possibly also with the technology contents of the disclosure above
Equivalent embodiment.But it is every without departing from technical solution of the present invention content, the technical spirit according to the present invention is to above example
Any simple modification, equivalent variations and the remodeling made, still fall within the protection domain of technical solution of the present invention.
Claims (10)
- A kind of 1. method for preparing single nano-pore interface on the glass substrate, it is characterised in that it is included in glass baseplate one Side sets the etching liquid containing HF, and opposite side is provided with alkaline electrolyte solution, and the etching liquid and the alkaline electrolyte are molten Liquid at least covers an etch areas, and the etch areas corresponds to throwing of the single nano-pore in the glass substrate surface Shadow zone domain, DC voltage is applied to the etching liquid and alkaline electrolyte solution and performed etching, and it is etched with galvanometer monitoring Journey to the glass baseplate both sides current lead-through.
- 2. the method as described in claim 1, it is characterised in that work as current lead-through, stop etching, cleaned.
- 3. method as claimed in claim 2, it is characterised in that the stopping etching being off applying voltage and removes etching Liquid.
- 4. the method as described in claim 1, it is characterised in that work as current lead-through, stop applying voltage, and be less than or waited In 60s overetch.
- 5. the method as described in claim 1,2 or 4, it is characterised in that the current lead-through refers to the electric current of the galvanometer Increase suddenly.
- 6. the method as described in claim 1, it is characterised in that the alkaline electrolyte solution is 0.05~1.0moL/L Tris-HCl solution or 0.05~1.0moL/L Na2CO3-NaHCO3Solution, the etching liquid are that mass fraction is 2~20% The HF aqueous solution or volume ratio are HF:H2O2：HAC=2：1：1、HF:H2O2：HNO3=2：1：1 solution；The etching liquid connects institute State the negative pole of DC voltage, the alkaline electrolyte solution connects the positive pole of the DC voltage, the DC voltage 0.2~ Between 200V.
- 7. the method as described in claim 1, it is characterised in that the cleaning is rinsed and soaked with 1~3mol/L alkaline solution 1.5~3h is steeped, uses deionized water rinsing afterwards.
- 8. the method as described in claim 1, it is characterised in that the first area of the glass baseplate side includes the etching Region, the first area cover in the material that the region in addition to the etch areas is corroded by resistance to HF,The etching liquid contacts and only contacts the material of the resistance to HF corrosion of the first area and the etch areas.
- 9. method as claimed in claim 8, it is characterised in that the glass baseplate is sheet material, tubing or the pipe end of closing, institute The thickness for stating glass baseplate is 25~1000 μm；The material of the resistance to HF corrosion is optical cement or polyimides.
- 10. using the single nano-pore interface of the method preparation as any one of claim 1-9, wherein what is prepared single receives A diameter of 2~500nm of metre hole.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112179954A (en) * | 2020-09-27 | 2021-01-05 | 西北工业大学 | Method for preparing nano-fluid diode responding to pH and temperature based on gelatin modified solid-state nano-pores |
| CN115724591A (en) * | 2021-08-31 | 2023-03-03 | 广东艾檬电子科技有限公司 | Micropore machining method based on electric field control |
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| CN104671668A (en) * | 2014-12-30 | 2015-06-03 | 西北大学 | Preparation method of single micro/nano hole based on glass materials |
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| CN115724591A (en) * | 2021-08-31 | 2023-03-03 | 广东艾檬电子科技有限公司 | Micropore machining method based on electric field control |
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