CN116695230A - Preparation device and method for high-deflection micro-shovel structure metal needle tip and electrode - Google Patents
Preparation device and method for high-deflection micro-shovel structure metal needle tip and electrode Download PDFInfo
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- CN116695230A CN116695230A CN202310930254.2A CN202310930254A CN116695230A CN 116695230 A CN116695230 A CN 116695230A CN 202310930254 A CN202310930254 A CN 202310930254A CN 116695230 A CN116695230 A CN 116695230A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 134
- 239000002184 metal Substances 0.000 title claims abstract description 134
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims description 19
- 230000007797 corrosion Effects 0.000 claims abstract description 56
- 238000005260 corrosion Methods 0.000 claims abstract description 56
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000005530 etching Methods 0.000 claims description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
- 229910052742 iron Inorganic materials 0.000 claims description 11
- 239000002826 coolant Substances 0.000 claims description 10
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 10
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 10
- 239000000110 cooling liquid Substances 0.000 claims description 9
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 31
- 239000003513 alkali Substances 0.000 description 23
- 238000005868 electrolysis reaction Methods 0.000 description 15
- 239000000463 material Substances 0.000 description 13
- 229910052721 tungsten Inorganic materials 0.000 description 13
- 239000010937 tungsten Substances 0.000 description 13
- 230000001105 regulatory effect Effects 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 239000002585 base Substances 0.000 description 7
- 229910021389 graphene Inorganic materials 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 238000003487 electrochemical reaction Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 241000270728 Alligator Species 0.000 description 2
- 241000270722 Crocodylidae Species 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- LNNWVNGFPYWNQE-GMIGKAJZSA-N desomorphine Chemical compound C1C2=CC=C(O)C3=C2[C@]24CCN(C)[C@H]1[C@@H]2CCC[C@@H]4O3 LNNWVNGFPYWNQE-GMIGKAJZSA-N 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229920005372 Plexiglas® Polymers 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
Abstract
The application provides a preparation device and a preparation method of a metal needle tip and an electrode of a high-deflection micro-shovel structure, which relate to the technical field of micro-electrode manufacturing and comprise the following steps: one end of the metal wire clamping device is connected with the positive electrode of the power supply, and the other end of the metal wire clamping device is used for clamping a metal wire to be prepared; the metal ring is sleeved on the metal wire to be prepared; the constant-current device is used for adding corrosive liquid to the metal ring; and the corrosion solution tank is connected with the negative electrode of the power supply, and the tip of the metal wire to be prepared is communicated with the corrosion solution tank to form a corrosion loop. According to the application, the corrosion loop between the tip of the metal wire to be prepared and the corrosion solution tank is established, and the corrosion solution is enabled to flow at a uniform speed at the tip of the metal needle wire based on the constant-current device, so that the surface of the prepared metal needle tip is smooth, a micro-shovel structure is presented, and a reference is provided for the preparation of experimental tools under a mesoscale.
Description
Technical Field
The application relates to the technical field of microelectrode manufacturing, in particular to a device and a method for preparing a metal needle tip and an electrode of a high-deflection micro-shovel structure.
Background
In recent years, technologies such as micro-nano processing and manufacturing and microelectrode manufacturing have been attracting attention. In particular, two-dimensional materials have been found to be particularly difficult for various processing operations (e.g., lifting, flipping, moving, bending, etc.) of two-dimensional materials (e.g., graphene, etc.). This also brings great trouble to subsequent researches (such as friction and wear, processing and manufacturing of micro-nano equipment, mechanical properties, etc.). Such as mechanically exfoliated graphene materials, are difficult to handle next in position and morphology on a substrate. The dry and wet transfer methods commonly used at present further introduce uncontrollable defects and have certain limitations in operation. In order to reduce the introduction of defects during the fabrication of micro-nano structures, it is desirable to be able to implement in situ direct manipulation of micro-nano materials (such as graphene, etc.) on a substrate to investigate the specific properties of a particular micro-nano structure. For example, crack growth, bending deformation, and the like of graphene are investigated.
In addition, it is also very difficult to locally conduct electricity to a particular micro-nano structure on a non-conductive substrate without damaging the micro-nano device structure. For example, a certain layer of graphene is electrically conductive on a SiO2 substrate, and interlayer conductive performance of graphene is studied. Currently, the method is mainly realized by means of AFM equipment, the cost is huge, and consumable conducting needle electrodes of the AFM equipment are easy to damage.
In recent years, many research teams at home and abroad prepare metal needle tips with different shapes, materials and needle tip curvature radius by using an electrochemical corrosion method, but the metal needle tips are mostly used in STM experiments and have the characteristics of super sharpness, longitudinal change of rigidity, small longitudinal-width ratio and large curvature change. In the micro-nano structure processing and preparing process of the two-dimensional material, the STM needle point is of a super-sharp structure, and is quite impractical. Also, we cannot simply increase the radius of curvature of the tip. Under the micrometer scale, the metal needle tip is generally in a conical shape, and has the characteristics of larger curvature radius, same rigidity in all directions, fixed radius of the handle end and the like. When micro-nano operation is performed, because the curvature radius of the needle point is larger, the contact point with the sample is uncontrollable, the actual contact point is too far away from the target contact point, and new defects (such as surface damage and fouling of the sample) or operation errors (such as folds caused by stress direction change and local stress change) are easily introduced; because the rigidity of the needle point in each direction is the same, the robustness of the contact point is poor, the positive pressure is fast to change, the control is not easy, and the sample is easy to damage; meanwhile, the needle point is arranged on the nano manipulator, the radius of the needle point handle end is fixed, the nano manipulator cannot be well fixed, uncontrollable mechanical change can be introduced in the operation process, and errors can be caused to the mechanical property research result of the research object.
On the other hand, the tip is not normally in direct contact with the sample, but is wrapped with a flexible material and then brought into contact with the sample. In order to increase the contact area of the needle tip with the flexible material, an effective contact of the flexible material with the plane of the two-dimensional material is achieved, which requires that the needle tip cannot be spherical, preferably can be a plane, and that the contact surface has a very good robustness. The ideal tip is preferably one-sided in the manipulation of two-dimensional materials, and requires some deflection to achieve a slow change in positive pressure. In addition, the contact points are required to be stable in a plane, having properties approximating the structure of a beam or plate.
Disclosure of Invention
In order to overcome the defects of the prior art, the application aims to provide a preparation device and a preparation method of a metal needle tip and an electrode of a high-deflection micro-shovel structure.
In order to achieve the above object, the present application provides the following solutions:
a preparation device of a metal needle tip and an electrode of a high-deflection micro-shovel structure comprises:
one end of the metal wire clamping device is connected with the positive electrode of the power supply, and the other end of the metal wire clamping device is used for clamping a metal wire to be prepared;
the metal ring is sleeved on the metal wire to be prepared;
the constant-current device is used for adding corrosive liquid to the metal ring;
and the corrosion solution tank is connected with the negative electrode of the power supply, and the tip of the metal wire to be prepared is communicated with the corrosion solution tank to form a corrosion loop.
Preferably, the method further comprises:
the cooling liquid pool is coated on the outer side of the etching solution pool;
and the constant temperature control system is arranged at the bottoms of the cooling liquid pool and the corrosive solution pool.
Preferably, the wire clamping device comprises:
the tinfoil paper clamping device is connected with the iron stand platform through a bracket fixing bolt;
and the tinfoil paper is connected with the tinfoil paper clamping device and used for clamping the metal wire to be prepared.
Preferably, the constant current device includes:
the injector is connected with the iron stand through an injector fixing bracket;
and the drainage tube is communicated with the injector and is used for adding corrosive liquid to the metal ring.
The application also provides a preparation method of the high-deflection micro-shovel structure metal needle tip and the electrode, which comprises the following steps:
adding sodium oxide solution into the corrosion solution tank and the constant flow device;
fixing a metal ring on the wall of the etching solution tank, so that the plane of the metal ring is parallel to the liquid level of the sodium oxide solution;
clamping one end of a metal wire to be prepared by using tin foil paper, and vertically inserting the other end of the metal wire to be prepared into the center of the metal ring;
dropwise adding sodium hydroxide solution to the metal ring by using a constant-current device to enable liquid drops to be hung on the metal ring;
and turning on a power switch, and continuously etching the metal wire to be prepared until the appearance of the metal wire to be prepared meets the requirement to obtain the metal needle tip and the electrode of the high-deflection micro-shovel structure.
Preferably, before etching, a cooling medium is added to the constant flow device and the temperature of the cooling medium is maintained at 30 ℃.
Preferably, the current output by the power supply is 20-40 mA when etching is performed.
The application also provides a high-deflection micro-shovel structure metal needle tip and an electrode, which are etched by the preparation method of the high-deflection micro-shovel structure metal needle tip and the electrode.
According to the specific embodiment provided by the application, the application discloses the following technical effects:
the application provides a preparation device and a preparation method of a metal needle tip and an electrode of a high-deflection micro-shovel structure, wherein the preparation device comprises the following steps: one end of the metal wire clamping device is connected with the positive electrode of the power supply, and the other end of the metal wire clamping device is used for clamping a metal wire to be prepared; the metal ring is sleeved on the metal wire to be prepared; the constant-current device is used for adding corrosive liquid to the metal ring; and the corrosion solution tank is connected with the negative electrode of the power supply, and the tip of the metal wire to be prepared is communicated with the corrosion solution tank to form a corrosion loop. According to the application, the corrosion loop between the tip of the metal wire to be prepared and the corrosion solution tank is established, and the corrosion solution is enabled to flow at a uniform speed at the tip of the metal needle wire based on the constant-current device, so that the surface of the prepared metal needle tip is smooth, a micro-shovel structure is presented, and a reference is provided for the preparation of experimental tools under a mesoscale.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions of the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a device for preparing a metal needle tip and an electrode of a high-deflection micro-shovel structure;
FIG. 2 is a 500-magnification image of the front surface of a tungsten tip and an electrode of the high-deflection micro-shovel structure provided by the application;
fig. 3 is a view of a high deflection micro shovel structured tungsten tip and electrode side 200 magnification image provided by the present application.
Symbol description:
the device comprises a iron stand table 1, a cooling medium 2, a metal ring 3, a metal wire 4 to be prepared, a drainage tube 5, a support fixing bolt 6, a metal wire clamping device 7, 8 tinfoil paper, a switch 9, a power supply 10, a voltage fine adjustment knob 11, a voltage rough adjustment knob 12, a conducting wire 13, a strong base solution 14, a strong base solution 15, a strong base fixing support 16, a drainage tube 17, a strong base liquid drop 18, a cooling liquid pool 19, a corrosive solution pool 20, a constant temperature control system 21 and a strong base etching liquid 22.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment may be included in at least one embodiment of the application. The appearances of such phrases in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Those of skill in the art will explicitly and implicitly appreciate that the embodiments described herein may be combined with other embodiments.
The terms "first," "second," "third," and "fourth" and the like in the description and in the claims and drawings are used for distinguishing between different objects and not necessarily for describing a particular sequential or chronological order. Furthermore, the terms "comprise" and "have," as well as any variations thereof, are intended to cover a non-exclusive inclusion. For example, inclusion of a list of steps, processes, methods, etc. is not limited to the listed steps but may alternatively include steps not listed or may alternatively include other steps inherent to such processes, methods, products, or apparatus.
In order that the above-recited objects, features and advantages of the present application will become more readily apparent, a more particular description of the application will be rendered by reference to the appended drawings and appended detailed description.
Referring to fig. 1, a device for preparing a metal needle tip and an electrode with a high-deflection micro-shovel structure comprises: wire clamping device 7, metal ring 3, constant flow device, corrosion solution tank 20, cooling liquid tank 19 and constant temperature control system 21.
A wire clamping device 7, one end of which is connected with the positive electrode of the power supply 10, and the other end of which is used for clamping the wire 4 to be prepared; a metal ring 3 sleeved on the metal wire 4 to be prepared; the constant-current device is used for adding corrosive liquid to the metal ring 3; and the corrosion solution pool 20 is connected with the negative electrode of the power supply 10, and the tip of the metal wire 4 to be prepared is communicated with the corrosion solution pool 20 to form a corrosion loop. A cooling liquid pool 19 which is coated outside the corrosive solution pool 20; and a constant temperature control system 21 arranged at the bottoms of the cooling liquid pool 19 and the corrosive solution pool 20.
Among these, the etching solution tank 20 is another container which does not react with strong alkali or reacts weakly, including glass, plexiglas, and the like. The etching solution tank 20 is used for storing a strong alkali etching solution, and the strong alkali etching solution includes, but is not limited to, sodium hydroxide with a concentration ranging from 2.5 to 7 mol/L. The coolant medium of the thermostatic control system 21 is other energy storage medium materials including water, as well as other auxiliary devices and materials that maintain the electrochemical reaction temperature at 30 ° (±5°).
Furthermore, the positive electrode device and the negative electrode device which participate in the electrochemical reaction are positioned above the liquid level of the strong alkali etching liquid, the positive electrode is close to the negative electrode, the positive electrode and the negative electrode are connected through the strong alkali liquid drops, a small part of the positive electrode of the electrode device which participates in the electrochemical reaction is inserted into the liquid level of the strong alkali etching liquid, and the negative electrode corrosion electrolytic wire ring is directly inserted into the strong alkali etching liquid. The cathode corrosion electrolysis wire ring is prepared into other geometric shapes including a round shape, the cathode corrosion electrolysis wire ring is close to and lifts up the liquid level of the strong alkali etching liquid, and the anode is inserted into the lifted-up liquid level of the strong alkali etching liquid.
Further, the wire holding device 7 of the present application includes: a tinfoil paper holder and a tinfoil paper 8.
The tinfoil paper clamping device is connected with the iron stand 1 through a bracket fixing bolt 6; and the tinfoil paper 8 is connected with the tinfoil paper clamping device and is used for clamping the metal wire 4 to be prepared.
The constant flow device comprises other methods and devices for quantitatively sucking/dripping the strong alkali etching liquid or changing the position of the liquid level of the strong alkali etching liquid by using other variable capacity devices including syringes with different specifications.
In an embodiment of the present application, a constant current device includes: a syringe 14 and a drainage tube 5.
A syringe 14 connected to the iron stand 1 via a syringe fixing bracket 16; and the drainage tube 5 is communicated with the injector 14 and is used for adding corrosive liquid to the metal ring 3.
It should be noted that, the power supply 10 of the present application is an adjustable dc voltage-stabilized power supply 10, and the adjustable dc voltage-stabilized power supply 10 adopts micheng MS3010D: the voltage range of the direct current stabilized power supply 10 is 1-10V under the CV mode, the etching effect is optimal when the voltage is 4.04V through experimental exploration, and the metal wire is preferably a semi-cylindrical tungsten wire and the metal ring is preferably a high-purity tungsten wire ring.
The corrosion solution tank, the constant flow device and the constant temperature control system 21 are integrated, and the purpose of the corrosion solution tank, the constant flow device and the constant temperature control system is to maintain the temperature of the strong alkali corrosion solution at the corrosion temperature of 30 ℃ all the time so as to improve the corrosion efficiency and reduce the crystallization generated by the electrochemical reaction. The constant-current control device consists of the drainage clamping device, the drainage tube 5 and the injector, wherein the drainage tube 5 guides out the corrosion solution, the injector is pushed by constant force to enable the corrosion solution to flow through the cathode to corrode the electrolytic wire coil, the constant solution flow rate is kept, bubbles generated by corrosion are guided out, the influence on the needle point is reduced, and the quality of the metal needle point is improved. The metal wire is split into two halves, so that a rough plane or a plurality of intersecting planes can be obtained, and the overall shape of the metal wire is in a semi-cylindrical shape or other similar semi-cylindrical shapes.
The metal wire handle end of the metal needle point is wound and welded by copper wires or other metal wires so as to change the radius of the metal wire handle end, thereby achieving other preparation methods stably connected with the nanometer manipulator.
According to the application, 5-6 layers of tinfoil paper are tightly wrapped at the position of 1-2 cm of the end of the metal wire handle to be prepared, so that the contact and conduction of the tinfoil paper and the metal wire are ensured, and the tinfoil paper wrapping layer has enough rigidity. The tinfoil is clamped by crocodile clips and fixed on a stand.
The application also provides a preparation method of the high-deflection micro-shovel structure metal needle tip and the electrode, which comprises the following steps:
step 1: adding sodium oxide solution into the corrosion solution tank and the constant flow device;
step 2: fixing a metal ring on the wall of the etching solution tank, so that the plane of the metal ring is parallel to the liquid level of the sodium oxide solution;
step 3: clamping one end of a metal wire to be prepared by using tin foil paper, and vertically inserting the other end of the metal wire to be prepared into the center of the metal ring;
step 4: dropwise adding sodium hydroxide solution to the metal ring by using a constant-current device to enable liquid drops to be hung on the metal ring; before etching, a cooling medium was added to the constant flow device, and the temperature of the cooling medium was maintained at 30 ℃.
In practical application, the application also needs to carry out the following preparation work before etching:
1) Taking a section of metal wire, cutting the metal wire along the central axis to form a semi-cylindrical shape, and cutting the metal wire into small sections of 3-4 cm.
2) According to the requirement of the manipulator connector, a metal wire with the diameter of 0.1-0.5 mm is selected to be tightly wound around the handle end, and the handle end is welded into a cylinder shape by soldering.
3) And folding and wrapping the welded handle end of the metal needle point by using tin foil.
4) Preparing a proper amount of sodium hydroxide solution with the concentration of 5mol/L for standby.
5) 80mL of the prepared sodium oxide solution is taken and placed in a corrosive solution tank.
6) Connect drainage tube and syringe to inhale 3mol sodium oxide solution in the syringe through the drainage tube for later use.
7) 100ml of clean water is injected into a constant temperature control system and is used as a cooling medium, a power supply is connected, and the temperature is regulated to 30 ℃.
8) And (3) installing and adjusting the position of the negative electrode corrosion electrolysis wire ring, wherein the negative electrode corrosion electrolysis wire ring is installed on the wall of the corrosion solution tank, and the circle plane is parallel to the liquid level of the strong alkali etching solution and is 1-2 cm away.
9) And clamping the folded tinfoil paper by using crocodile pliers fixed on the iron stand. The unwrapped metal needle tip is vertically inserted into the center of the negative electrode corrosion electrolysis wire ring.
10 The needle point clamping device is regulated to enable the needle point to be inserted into the negative electrode corrosion electrolysis wire ring to extend into the negative electrode corrosion electrolysis wire ring by 1-5 mm.
11 The constant-current control device is fixed on the wall of the corrosion solution tank, the drainage tube is obliquely above the negative corrosion electrolysis wire ring, the pushed sodium hydroxide solution is expected to be just hung in the negative corrosion electrolysis wire ring and not fall down, but the drainage tube is not contacted with the negative corrosion electrolysis wire ring.
12 Connecting wires according to an electrical rule, connecting a red power supply anode and connecting a binding post of a tinfoil clamping device; and the black power supply negative electrode is connected with a binding post of the negative electrode corrosion electrolysis wire coil clamping device.
13 Dropping sodium hydroxide alkali solution on the negative electrode corrosion electrolysis coil to hang the liquid drop on the negative electrode corrosion electrolysis coil and keep the liquid drop connected with the needle point.
14 Checking circuit, eliminating short circuit/open circuit fault, regulating regulated DC voltage-stabilized power supply to CV mode, and regulating coarse and fine knobs of power supply voltage to minimum.
Step 5: and (3) turning on a power switch (when etching is performed, the current output by a power supply is 20-40 mA), and continuously etching the metal wire to be prepared until the appearance of the metal wire to be prepared meets the requirement to obtain the metal needle tip and the electrode of the high-deflection micro-shovel structure.
Further, step 5 in the present application includes:
15 Opening the adjustable direct current stabilized power supply switch, and adjusting the voltage to 4.04V.
16 A current display screen is observed, the reasonable current range is 20-40 mA, and the voltage value is reasonably adjusted according to the reaction rate.
17 The liquid drops are observed, the transparent liquid drops are rapidly changed into milky white which is uniformly filled by small bubbles, the bubbles become larger gradually and uneven along with the advancement of the electrolysis reaction time, and the liquid drops become smaller gradually.
18 When the bubbles start to grow, the injector is pushed slowly, new strong base etching liquid flows into the liquid drops, the bubbles become smaller again and become uniform again.
19 Repeating the steps for a plurality of times, when the tip of the needle point falls off, immediately cutting off the power supply, taking down the needle point/electrode, and lightly flushing with clear water along the axial direction.
20 And (3) observing the needle tip/electrode morphology under an optical microscope, and judging whether the needle tip/electrode morphology meets the preparation requirements. If not, repeating the steps.
The metal needle tip and the electrode prepared by the application are integrally characterized by a shovel structure, and the tip has the mechanical property of a plate or a beam. The shovel rod is a semicircular column, the shovel end is flat, the curvature change in the height direction of the tip is large, and the curvature change in the plane direction is slower, so that the shovel-like structural characteristics are formed. The whole length is 3-4 cm, the length of the handle end is 0.5-1 cm, the transverse width of the cross section of the needle point is 5-20 micrometers, the height is 0.1-0.5 micrometers, and the metal needle point and the electrode of the micro-shovel structure comprise nickel, iron, chromium and other metal needle points and electrodes including tungsten. The shape of the metal needle tip and the electrode tip of the micro-shovel structure is flat, but not limited to flat, and also comprises but not limited to ellipse, rectangle, trapezoid, circle, sphere, zigzag, wave and other geometric shapes. The micro-shovel structure metal tips and electrodes include, but are not limited to, shovel-like structures, as well as other shovel-like or fork-like structures. The metal tip and electrode of the micro-shovel structure include, but are not limited to, one or more planes (concave or convex), and are not limited to, one or more planes (concave or convex) where the planes pass through the central axis. The metal needle tip with the micro-shovel structure and the electrode operation object comprise other two-dimensional materials including graphene.
The preparation method of the application is further described by taking the preparation of a tungsten metal needle tip and an electrode with a high-deflection micro-shovel structure as an example:
preparing experimental equipment: iron stand, 100mL of 5mol/L sodium hydroxide solution, 20cm of fine copper with phi of 0.1-0.5 mm, one roll of phi 2.5mm tungsten wire, one constant temperature electric soldering iron, 20cm of welding wire, one 100mL beaker, one pair of tweezers, 1 sheet of 7x7cm2 tinfoil paper, one pair of diagonal pliers, a constant temperature control system, one 5mol injector (without a needle), 10cm of phi 8mm drainage tube and a plurality of alligator clips.
Shoveling the tungsten metal needle tip and electrode crude: a section of tungsten wire with the diameter of 0.5mm is cut by using a diagonal pliers according to the requirement. The tungsten filament is cut along the central axis to form a semi-cylindrical shape, and is cut into small sections of 3 cm to 4 cm. According to the requirement of the manipulator connector, a thin copper wire with phi of 0.1-0.5 mm is selected to be tightly wound around the handle end (in fig. 1, the upper end of the semi-cylindrical tungsten wire 4 is wrapped by the tinfoil paper 8), and is welded into a cylinder shape by a welding wire. The welded handle end of the metal needle point is wrapped by the tinfoil paper in a folding way, so that the structure of the tinfoil paper 8 and the semi-cylindrical tungsten wire 4 in fig. 1 is formed.
Preparation of a negative electrode high purity tungsten filament ring 3: one end of a high-purity tungsten wire with the diameter of 0.01mm and the length of 70mm is fixed on an alligator clip of an external lead of an adjustable direct current stabilized power supply, and the other end is wound into a ring with the diameter of 2.5 mm. Is fixed above the etching solution tank 20.
80mL of the prepared sodium oxide solution (strong base solution 22) was placed in the etching solution tank 20. The drainage tube 5 and the syringe 14 are connected, and 3mol of sodium oxide solution is sucked into the syringe 14 through the drainage tube 5 for standby. 100ml of clean water is injected into a cooling liquid pool 19 of a constant temperature control system and used as a cooling medium 2, and the power supply is turned on, so that the temperature is regulated to 30 ℃.
The position of the cathode high-purity tungsten wire ring 3 is installed and adjusted, the cathode high-purity tungsten wire ring 3 is installed on the wall of the corrosion solution tank 20, and the circle plane is parallel to the liquid level of the strong alkali etching solution 22 and is 1-2 cm apart. The needle tip clamping device (tinfoil paper clamping device 7 and tinfoil paper 8) is adjusted to enable the needle tip to be inserted into the high-purity tungsten wire ring 3 and extend deep into the tungsten wire ring by 1-5 mm. The drainage tube 5 is fixed on the wall of the corrosion solution tank 20, the drainage tube 5 is obliquely above the negative electrode high-purity tungsten wire ring 3, and the sodium hydroxide solution of the strong alkali solution 15 in the pushed syringe is expected to just hang in the negative electrode high-purity tungsten wire ring 3 without falling down, but the drainage tube 5 is not contacted with the negative electrode high-purity tungsten wire ring 3. A sodium hydroxide alkali solution 18 is dripped on the high-purity tungsten filament ring 3, so that the liquid drop is hung on the high-purity tungsten filament ring 3 and keeps being communicated with the tip of the semi-cylindrical tungsten filament 4.
In the corrosion loop of the present application, the regulated dc regulated power supply 10 employs the micheng MS3010 type D: 0-30V/0-10A direct current stabilized voltage supply. Before the power switch 9 is turned on, the voltage coarse adjustment knob 12 and the voltage fine adjustment knob 11 are both adjusted to be minimum counterclockwise. At this time, the regulated dc voltage regulator 10 is in CV mode. The power switch 9 is pressed after checking that the circuit connection is correct, as shown by the electrical rules connecting the wires 13. The voltage coarse adjustment knob 12 is adjusted in a clockwise manner until the adjustable direct current stabilized power supply 10 displays a voltage value of about 3.5V, the voltage coarse adjustment knob 11 is adjusted in a clockwise manner until the voltage is 4.04V, the current value is between 0 and 150mA at this time, the optimal current is about 20mA, and if the voltage value is larger or smaller, the voltage value can be adjusted in a fine manner according to requirements.
Observing the strong alkali liquid drops 18, the transparent liquid drops rapidly change into milky white evenly filled by small bubbles, the bubbles gradually become larger and uneven with the advancement of the electrolysis reaction time, and the strong alkali liquid drops 18 gradually become smaller. When the bubble starts to grow, the injector 14 is pushed slowly, the strong alkali solution 15 in the injector flows into the strong alkali liquid drop 18 through the drainage tube 5, the strong alkali liquid drop 18 grows and even drops, new liquid drops are formed, the bubble becomes smaller again, and the bubble becomes uniform again. And repeating the steps for a plurality of times until the tip of the needle tip of the semi-cylindrical tungsten wire 4 falls off, immediately cutting off the power supply, taking down the needle tip/electrode, and lightly flushing the needle tip/electrode with clear water along the axial direction.
The adjustable direct-current stabilized power supply 10 outputs a constant voltage of 1-10V, and can display the current value in the corrosion loop in real time in the experimental process, and the current magnitude is positively correlated with the bubble quantity generated by the strong alkali liquid drops 18 in the high-purity tungsten wire ring 3. In the early stage of etching, the etching speed is high, the current value is changed greatly, and the current value is reduced rapidly from about 120 mA. With the advancement of etching time, the current value is gradually stabilized at about 20 mA. When the voltage is about to end, the current value is 1mA, and the voltage value can be reduced to 1V through the voltage coarse adjustment knob 12 and the voltage fine adjustment knob 11. At this time, the current value was further reduced, and even the display value was 0mA, but the tip of the semi-cylindrical tungsten wire 4 was not detached, and the reaction was continued. And immediately closing the switch 9 until the needle tip of the semi-cylindrical tungsten wire 4 is observed to fall off, and cutting off the power supply.
The tip/electrode (tinfoil 8, semi-cylindrical tungsten filament 4) was removed and the tip of semi-cylindrical tungsten filament 4 was gently rinsed axially with clear water. Observing under an optical microscope, and judging whether the needle tip/electrode morphology meets the preparation requirement. And if the etching is not in accordance with the requirements, re-etching.
As shown in fig. 2 and 3, the front and side surfaces of the tungsten tip/electrode were prepared. It is evident that the tip/electrode tip is flat, overall in a micro-shovel configuration, with a higher deflection than a cylindrical tip.
According to the specific embodiment provided by the application, the application discloses the following technical effects:
according to the application, the corrosion loop between the tip of the metal wire to be prepared and the corrosion solution tank is established, and the corrosion solution is enabled to flow at a uniform speed at the tip of the metal needle wire based on the constant-current device, so that the surface of the prepared metal needle tip is smooth, a micro-shovel structure is presented, and a reference is provided for the preparation of experimental tools under a mesoscale.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the method disclosed in the embodiment, since it corresponds to the device disclosed in the embodiment, the description is relatively simple, and the relevant points are referred to the device part description.
The principles and embodiments of the present application have been described herein with reference to specific examples, the description of which is intended only to assist in understanding the methods of the present application and the core ideas thereof; also, it is within the scope of the present application to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the application.
Claims (8)
1. The utility model provides a preparation facilities of high deflection micro shovel structure metal needle point and electrode which characterized in that includes:
one end of the metal wire clamping device is connected with the positive electrode of the power supply, and the other end of the metal wire clamping device is used for clamping a metal wire to be prepared;
the metal ring is sleeved on the metal wire to be prepared;
the constant-current device is used for adding corrosive liquid to the metal ring;
and the corrosion solution tank is connected with the negative electrode of the power supply, and the tip of the metal wire to be prepared is communicated with the corrosion solution tank to form a corrosion loop.
2. The device for preparing the metal needle tip and the electrode of the high-deflection micro-shovel structure according to claim 1, further comprising:
the cooling liquid pool is coated on the outer side of the etching solution pool;
and the constant temperature control system is arranged at the bottoms of the cooling liquid pool and the corrosive solution pool.
3. The device for manufacturing the metal needle tip and the electrode with the high-deflection micro-shovel structure according to claim 2, wherein the metal wire clamping device comprises:
the tinfoil paper clamping device is connected with the iron stand platform through a bracket fixing bolt;
and the tinfoil paper is connected with the tinfoil paper clamping device and used for clamping the metal wire to be prepared.
4. The device for preparing the metal needle tip and the electrode with the high-deflection micro-shovel structure according to claim 3, wherein the constant-current device comprises:
the injector is connected with the iron stand through an injector fixing bracket;
and the drainage tube is communicated with the injector and is used for adding corrosive liquid to the metal ring.
5. A preparation method of a metal needle tip and an electrode of a high-deflection micro-shovel structure is characterized by comprising the following steps:
adding sodium oxide solution into the corrosion solution tank and the constant flow device;
fixing a metal ring on the wall of the etching solution tank, so that the plane of the metal ring is parallel to the liquid level of the sodium oxide solution;
clamping one end of a metal wire to be prepared by using tin foil paper, and vertically inserting the other end of the metal wire to be prepared into the center of the metal ring;
dropwise adding sodium hydroxide solution to the metal ring by using a constant-current device to enable liquid drops to be hung on the metal ring;
and turning on a power switch, and continuously etching the metal wire to be prepared until the appearance of the metal wire to be prepared meets the requirement to obtain the metal needle tip and the electrode of the high-deflection micro-shovel structure.
6. The method for manufacturing the metal needle tip and the electrode with the high-deflection micro-shovel structure according to claim 5, wherein before etching, a cooling medium is added into the constant-current device, and the temperature of the cooling medium is kept at 30 ℃.
7. The method for manufacturing the metal needle tip and the electrode with the high-deflection micro-shovel structure according to claim 6, wherein the current output by a power supply is 20-40 mA when etching is performed.
8. A high-deflection micro-shovel structure metal needle tip and an electrode, which are characterized by being etched by the preparation method of the high-deflection micro-shovel structure metal needle tip and the electrode according to any one of claims 5-7.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118016376A (en) * | 2024-04-08 | 2024-05-10 | 国开启科量子技术(安徽)有限公司 | Method for preparing needle electrode of ion trap |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118016376A (en) * | 2024-04-08 | 2024-05-10 | 国开启科量子技术(安徽)有限公司 | Method for preparing needle electrode of ion trap |
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