CN113151886B - Dynamic preparation method and device for annular bundling porous transmitting needle tip - Google Patents

Dynamic preparation method and device for annular bundling porous transmitting needle tip Download PDF

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Publication number
CN113151886B
CN113151886B CN202110454658.XA CN202110454658A CN113151886B CN 113151886 B CN113151886 B CN 113151886B CN 202110454658 A CN202110454658 A CN 202110454658A CN 113151886 B CN113151886 B CN 113151886B
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needle
solution
annular
porous
transmitting
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CN113151886A (en
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郭登帅
梁广
张永合
崔阳
赵笙罡
郭彤
周文妹
王文川
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Shanghai Engineering Center for Microsatellites
Innovation Academy for Microsatellites of CAS
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Shanghai Engineering Center for Microsatellites
Innovation Academy for Microsatellites of CAS
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/02Etching
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/02Etching
    • C25F3/08Etching of refractory metals
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F7/00Constructional 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)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention provides a dynamic preparation method and a device of an annular cluster porous transmitting needle tip, comprising the following steps: a firing pin module configured to hold an annular bundled porous firing pin; a solution module configured to carry a solution that reacts with the annular bundled porous emitter pins; and a movement device configured to drive the emitter needle module to move so as to immerse the annular cluster porous emitter needle in the solution; wherein: immersing the annular bundling porous transmitting needle into the solution for calibration, and after the annular bundling porous transmitting needle reaches the parameter requirement, driving the annular bundling porous transmitting needle to move upwards to leave the liquid level of the solution by a moving device, calibrating the up-and-down round trip times, so as to finish the needle point calibration; the annular bundling porous transmitting needle is immersed into the solution for preparation, and after the annular bundling porous transmitting needle reaches the calibrated up-and-down round trip times, the moving device drives the annular bundling porous transmitting needle to move upwards to leave the liquid level of the solution, so that the preparation of the needle point is completed.

Description

Dynamic preparation method and device for annular bundling porous transmitting needle tip
Technical Field
The invention relates to the technical field of aerospace, in particular to a dynamic preparation method and device for an annular bundling porous transmitting needle tip.
Background
The porous needle type field emission electric thruster is a novel field emission electric thruster, which combines the stability of capillary tube type and the high impedance advantage of solid needle type. The radius size of the needle point of the transmitting needle is very small, usually in the micron order, the electric field intensity of the needle point of the transmitting needle is very high, the liquid propellant is ionized by the very strong electric field of the needle point and is accelerated to be ejected out to generate thrust, and meanwhile, the propellant is transported to the needle point for supplementing the propellant under the capillary action of the pore inside the transmitting needle. In order to improve the thrust of the field emission electric thruster, a plurality of thrusters can be connected in parallel to form a cluster, or a plurality of emission needles are integrated together to form a ring, and the size and the quality of the system can be greatly reduced due to higher integration level of the emission needles, so that the field emission electric thruster has a larger development prospect in practical engineering application. As shown in fig. 1, the ring-shaped cluster emitter needle is composed of a substrate and tens of needles, wherein the tens of needles are uniformly distributed, and the interval is about 1mm and is vertical to the substrate. The annular bundling emission needle is generally formed by sintering metal powder into a whole, the needle and the substrate are not required to be connected through a clamp, the whole size is small, and the integration level is high. In order to realize the normal operation of the thruster, the needle tip size of the annular cluster transmitting needle is required to be as consistent as possible, and the radius size of the needle tip is required to be smaller than 3 microns. Therefore, the simultaneous preparation of a plurality of needle points is one of the key technology and the difficulty of the thruster.
The Chinese patent application No. CN201210313301.0, device and method for preparing metal needle tip, refers to a method for preparing metal needle tip by loading constant current source between the metal wire to be prepared and the electrode until the metal wire breaks at the contact position of electrolyte liquid level to form needle tip. The method can only prepare one needle point at a time, so that the method is not suitable for preparing the needle point of the annular bundling transmitting needle;
the Chinese patent application No. CN201910031212.9, namely a device and a method for preparing a tungsten wire needle tip with controllable length-diameter ratio, refers to a method for preparing a tungsten wire needle tip with controllable length-diameter ratio, and the method is characterized in that the tungsten wire is lifted up and down to and fro and finally broken at the liquid level to form the needle tip. The method can only prepare one needle point at a time, so that the method is not suitable for preparing the needle point of the annular bundling transmitting needle;
the invention patent of China with the application number of 201910750467.0 (automatic array type nanometer needle point electrochemical preparation platform and preparation method) mentions an automatic array type nanometer needle point electrochemical preparation platform and method, the method realizes one-time preparation of a plurality of nanometer needle points through an array type clamp, is suitable for batch preparation of single needle points, but anodes and cathodes in the preparation platform correspond to one another one by one, namely one cathode ring corresponds to one, and the distance between the needles in the annular bundling emission needle is smaller, and one cathode ring cannot be matched for each needle, so that the platform is not suitable for preparation of the needle points of the annular bundling emission needle.
The Chinese patent application No. 201911110421.9, namely a nano needle point batch production device and a preparation method, refers to a nano needle point batch production device and a preparation method, and the method is characterized in that a metal wire is corroded and broken from the middle part by an electrochemical corrosion method, and the nano needle points obtained by collecting through a collecting device can be prepared in batches, but the method adopts the idea of preparing one needle point each time, namely, the preparation of the next needle point can be started after the needle point is prepared, and the method is not suitable for the preparation of the annular bundling emission needle point.
Through investigation, no needle point preparation method suitable for the porous emission needle exists at present, and the existing multi-needle point simultaneous preparation method is not suitable for preparing the needle point of the annular bundling porous emission needle.
Disclosure of Invention
The invention aims to provide a dynamic preparation method and a dynamic preparation device for an annular cluster porous transmitting needle tip, which are used for solving the problem that the existing needle tip preparation method is not suitable for preparing the annular cluster porous transmitting needle tip.
In order to solve the technical problems, the invention provides a dynamic preparation device of an annular bundling porous emission needle tip, which comprises:
a firing pin module configured to hold an annular bundled porous firing pin;
a solution module configured to carry a solution that reacts with the annular bundled porous emitter pins; and
the movement device is configured to drive the transmitting needle module to move so as to enable the annular cluster porous transmitting needle to be immersed in the solution; wherein:
immersing the annular bundling porous transmitting needle into the solution for calibration, and after the annular bundling porous transmitting needle reaches the parameter requirement, driving the annular bundling porous transmitting needle to move upwards to leave the liquid level of the solution by a moving device, calibrating the up-and-down round trip times, so as to finish the needle point calibration;
the annular bundling porous transmitting needle is immersed into the solution for preparation, and after the annular bundling porous transmitting needle reaches the calibrated up-and-down round trip times, the moving device drives the annular bundling porous transmitting needle to move upwards to leave the liquid level of the solution, so that the preparation of the needle point is completed.
Optionally, in the dynamic preparation device of the annular cluster porous emission needle tip, the movement device includes:
a linkage configured to secure the firing pin module to the motion control module via the linkage;
a bracket configured to be vertically fixed on the base;
the motion control module is configured to be vertically fixed on the bracket and can drive the connecting rod to move up and down along the bracket; and
and the support block is configured to strengthen the support and prevent the support from shaking.
Optionally, in the dynamic preparation device of the annular cluster porous emission needle tip, the connecting rod comprises a transverse connecting rod and a vertical connecting rod, wherein:
the transverse connecting rod is horizontally arranged and fixed on the vertical connecting rod; the vertical connecting rod is vertically arranged and fixed on the motion control module.
Optionally, in the dynamic preparation device of the annular cluster porous emission needle tip, the motion control module comprises a screw nut mechanism, a driver and a controller, wherein:
the screw nut mechanism is vertically fixed on the bracket; the driver and the controller are fixed on the base.
Optionally, in the dynamic preparation device of the annular cluster porous emission needle tip, the solution module includes:
a solution tank configured to be horizontally fixed on the base;
the solution is configured to be contained in the solution tank, the liquid level of the solution is higher than that of the stainless steel ring, and the solution is NaOH solution;
a cathode support configured to be fixed within the solution tank and to form a support for the stainless steel ring;
a stainless steel ring configured to connect to a negative electrode of a power source to act as a cathode for an electrochemical reaction.
Optionally, in the dynamic preparation device of the annular cluster porous emission needle tip, adjusting the relative position between the motion control module and the solution module so that the annular cluster porous emission needle is coaxial with the stainless steel ring;
the motion control module drives the connecting rod to do lifting movement along the bracket so as to drive the transmitting needle module to do lifting movement, so that the annular cluster porous transmitting needle is immersed in the solution or separated from the solution level;
the upward movement limit position includes: the annular cluster porous transmitting needle is positioned at a certain distance above the liquid level of the solution;
the descent movement limit position includes: the annular cluster porous emission needle is positioned below the liquid level of the solution and is not contacted with the bottom of the solution tank;
the material of the annular cluster porous transmitting needle comprises tungsten or rhenium;
the annular cluster porous transmitting needle is connected with the positive electrode of the power supply to serve as the anode of the electrochemical reaction.
Optionally, in the dynamic preparation device of the annular cluster porous transmitting needle tip, the inner diameter of the stainless steel ring is 40mm, and the thickness of the stainless steel ring is 1mm;
the diameter of the base of the annular cluster porous transmitting needle is 9mm;
and 25 tungsten emission needles or rhenium emission needles with the length of 5mm and the diameter of 0.5mm are uniformly distributed on the substrate of the annular cluster porous emission needle.
The invention also provides a preparation method realized by the dynamic preparation device of the annular cluster porous emission needle tip, which comprises the following steps of:
immersing the annular cluster porous transmitting needle into the liquid level of the solution for a certain depth, and loading voltage between the annular cluster porous transmitting needle and the stainless steel ring;
the motion control module drives the annular cluster porous transmitting needle to do up-and-down reciprocating motion leaving the liquid level and immersing the liquid level at a certain speed;
and recording the change relation between the radius size of each annular cluster porous transmitting needle and the up-down reciprocating frequency under the conditions of different inter-electrode voltages, solution concentrations, immersion liquid level depths and reciprocating motion rates, and finally obtaining the preparation parameters which can enable the radius size of all needle points to be smaller than 3 microns, thereby completing the calibration process.
Optionally, in the dynamic preparation method of the annular cluster porous emission needle tip, the preparation parameters include the calibrated voltage, the calibrated concentration solution, the calibrated depth, the calibrated reciprocating motion rate and the calibrated up-and-down round trip times;
the calibrated voltage is 5V, the calibrated concentration solution is 1mol/L, the calibrated depth is 1mm, the calibrated reciprocating speed is 0.5mm/s, and the calibrated up-and-down round trip times are 220 times.
Optionally, in the method for dynamically preparing the annular cluster porous emission needle tip, the preparing the annular cluster porous emission needle by immersing the annular cluster porous emission needle in the solution comprises the following steps:
and loading a calibrated voltage between the anode and the cathode, immersing the transmitting needle into a calibrated concentration solution to a calibrated depth, driving the annular cluster porous transmitting needle to do up-and-down reciprocating motion away from the liquid surface and immersed into the liquid surface at a calibrated reciprocating motion rate by the motion control module, and automatically driving the annular cluster porous transmitting needle to move upwards away from the liquid surface by the motion control module until the up-and-down reciprocating motion times reach the calibrated up-and-down reciprocating motion times, wherein the needle point preparation process is finished.
The inventors of the present invention have found through studies that, in a method of forming a needle tip by loading a constant current source or a constant voltage source between a needle to be prepared and an electrode until the needle breaks at a contact point of an electrolyte liquid surface, a manner of breaking the needle in the middle to form the needle tip is adopted, and a manner of breaking the needle from the middle is not suitable for simultaneous preparation of a plurality of needle tips. In the process of preparing the needle point by the electrochemical corrosion method, the concentration distribution of the electrolyte is uneven caused by the combination of factors such as surface tension, electrochemical reaction product falling, electrostatic force absorption of the reaction product and the like, so that the reaction of the transmitting needle at the liquid level is fastest, the transmitting needle at the liquid level is in a neck shape, as shown in figure 2, and the transmitting needle is finally broken at the position under the pulling action of the gravity of the transmitting needle at the lower end along with the progress of electrochemical corrosion, so that the needle point is formed. However, for the porous type emitting needle sintered from powder particles, there is a certain difference in the internal particle size and distribution uniformity, which inevitably causes a difference in the electrochemical reaction rate of each emitting needle, resulting in a difference in the breaking timing of the lower emitting needle and a large difference in the size of each needle tip; on the other hand, the difference in electrochemical reaction rate of each of the needles causes the difference in diameter change of the lower end needle, the abrupt diameter change causes the change in surface tension, and thus the "neck" position may be changed, as shown in fig. 3, the secondary or multiple occurrences of the "neck" position will cause the needles to be re-corroded at new sites, resulting in a difference in breaking time of several minutes or even several tens minutes of different needles, and in this time difference, the already formed needle tip will be further electrochemically corroded to become blunt, and finally the needle tip meeting the required size cannot be prepared.
The method for forming the needle point by carrying out up-and-down reciprocating lifting movement on the transmitting needle and finally breaking the transmitting needle at the liquid level is characterized in that a 'neck' is firstly generated on the transmitting needle at the liquid level, then the transmitting needle is carried out small-amplitude up-and-down reciprocating lifting movement by taking the 'neck' as a center point, and the transmitting needle near the 'neck' is corroded through electrochemical reaction until the transmitting needle breaks. Similar to the process of preparing the needle tip by the intermediate breaking mode, the difference of particles in the porous transmitting needle can lead to different breaking time of the transmitting needle, and is not suitable for preparing the annular bundling porous transmitting needle tip.
In addition, the spacing between the emitting needles in the annular bundling emitting needles is smaller, and the emitting needles are influenced by peripheral emitting needles in the process of preparing the needle points, so that the existing method and device cannot meet the preparation of the needle points of the annular bundling porous emitting needles.
The inventors of the present invention also found in the study that: the dynamic preparation device of the annular cluster porous transmitting needle tip (the stainless steel ring is a cathode connected with a power supply cathode and horizontally placed in NaOH solution), the annular cluster porous transmitting needle is an anode connected with a power supply anode, is coaxial with the stainless steel ring, is vertically immersed into the NaOH solution for a certain depth and performs up-and-down reciprocating motion), has the following conditions: the change of interelectrode voltage, solution concentration, immersed liquid level depth and reciprocating motion rate parameters can influence the reaction rate of all parts of the emitting needle under the liquid level while the emitting needle under the liquid level of the solution is subjected to electrochemical reaction to gradually dissolve and thin under the action of an electric field between an anode and a cathode and the solution.
The inventors have analyzed to conclude that: unlike the process of preparing a single needle tip, the reaction rate of each needle in the annular cluster porous needle is affected by the interelectrode voltage, the solution concentration and the immersion liquid level depth, and the reaction rate of the annular cluster porous needle is affected by the adjacent needles, because each needle is adjacent to the adjacent needle, the electric field distribution between the needle and the stainless steel ring and the reaction rate of different parts at the lower end of the needle are affected.
Further, the inventor of the present invention found through a great number of experiments that by making the annular cluster porous emitter needle reciprocate away from the liquid surface and immerse in the liquid surface, on one hand, the contact time between the lower end of the emitter needle and the solution is increased to increase the electrochemical reaction time, and on the other hand, the up-and-down reciprocation of the emitter needle drives the electrochemical reaction product to move so as to change the electric field distribution near the emitter needle at the lower end, the result that no neck is generated at the liquid surface and the reaction rate at the lower end of the emitter needle increases with the depth, namely the reaction rate at the tail end of the emitter needle is fastest, can be obtained.
Thus, the required needle tip size can be finally obtained with the progress of time; meanwhile, as the reaction rates of different needle points are slightly different, in order to prevent the needle points which have reached the size requirement from being corroded continuously in the solution and becoming blunt, when the parameters for preparing the needle points are selected, lower working voltage and/or solution concentration should be selected to reduce the size difference of the needle points caused by different reaction rates of the needle points; in addition, in order to prevent the liquid level from severely fluctuating due to the upward and downward movement of the firing pin, a lower upward and downward reciprocation rate of the firing pin should be selected.
Based on the insight, the invention provides a dynamic preparation method and a dynamic preparation device for the needle tip of the annular cluster porous transmitting needle, and the transmitting needle module for clamping the annular cluster porous transmitting needle is driven by a motion device to move so as to enable the annular cluster porous transmitting needle to be immersed in a solution, thereby realizing uniform movement of multiple needles of the annular cluster porous transmitting needle and synchronous preparation; in addition, the annular bundling porous transmitting needle is immersed into the solution for calibration, after the annular bundling porous transmitting needle meets the parameter requirement, the moving device drives the annular bundling porous transmitting needle to move upwards to leave the liquid level of the solution, the up-and-down round trip times are calibrated, the needle point calibration is completed, the optimal preparation parameter is obtained before the preparation is realized, and the preparation effect is enabled to reach the best effect; further, the annular bundling porous transmitting needle is immersed into the solution for preparation, and after the annular bundling porous transmitting needle reaches the calibrated up-and-down round trip times, the moving device drives the annular bundling porous transmitting needle to move upwards to leave the liquid level of the solution, so that the preparation of the needle point is completed.
Therefore, the invention creatively proposes that the ring-shaped cluster porous transmitting needle is immersed into the solution for calibration before the preparation, so that the optimal preparation parameters are obtained, and the defects easily occurring in the existing preparation method are prevented.
The inventor of the invention has explored and obtained interelectrode voltage, solution concentration, immersed solution depth, up-and-down reciprocating motion rate and motion times which can prepare the needle tip meeting the requirements through a large number of experiments, and has verified the dynamic preparation method and device of the annular cluster porous transmitting needle tip. The method can realize the simultaneous preparation of a plurality of needle points of the annular clustered porous transmitting needle, the size of the processed needle points meets the requirement, the consistency is better, the method is simple, only the up-and-down reciprocating movement times of the transmitting needle are controlled, and the degree of automation is high.
Drawings
FIG. 1 is a schematic view of a prior art and inventive annular cluster porous emitter needle;
FIG. 2 is a schematic view of a "neck" during the preparation of a needle tip by the prior electrochemical etching method;
FIG. 3 is a schematic view of the change in position of the "neck" during the preparation of a needle tip by the prior electrochemical etching method;
FIG. 4 is a schematic diagram of a dynamic preparation apparatus for an annular cluster porous emitter needle tip of the present invention;
the figure shows: 10-a base; a 20-solution module; 21-a solution tank; 22-solution; 23-cathode support; 24-stainless steel rings; 30-a firing pin module; 31-an annular cluster porous transmitting needle; 32-a clamp; 40-transverse connecting rods; 50-vertical connecting rods; 60-supporting; 70-a motion control module; 71-a screw nut mechanism; 72-a driver; 73-a controller; 80-supporting blocks.
Detailed Description
It should be noted that the components in the figures may be shown exaggerated for illustrative purposes and are not necessarily to scale. In the drawings, identical or functionally identical components are provided with the same reference numerals.
In the present invention, unless specifically indicated otherwise, "disposed on …", "disposed over …" and "disposed over …" do not preclude the presence of an intermediate therebetween. Furthermore, "disposed on or above" … merely indicates the relative positional relationship between the two components, but may also be converted to "disposed under or below" …, and vice versa, under certain circumstances, such as after reversing the product direction.
In the present invention, the embodiments are merely intended to illustrate the scheme of the present invention, and should not be construed as limiting.
In the present invention, the adjectives "a" and "an" do not exclude a scenario of a plurality of elements, unless specifically indicated.
It should also be noted herein that in embodiments of the present invention, only a portion of the components or assemblies may be shown for clarity and simplicity, but those of ordinary skill in the art will appreciate that the components or assemblies may be added as needed for a particular scenario under the teachings of the present invention.
It should also be noted herein that, within the scope of the present invention, the terms "identical", "equal" and the like do not mean that the two values are absolutely equal, but rather allow for some reasonable error, that is, the terms also encompass "substantially identical", "substantially equal". By analogy, in the present invention, the term "perpendicular", "parallel" and the like in the table direction also covers the meaning of "substantially perpendicular", "substantially parallel".
The numbers of the steps of the respective methods of the present invention are not limited to the order of execution of the steps of the methods. The method steps may be performed in a different order unless otherwise indicated.
The dynamic preparation method and the device of the annular cluster porous transmitting needle tip provided by the invention are further described in detail below with reference to the accompanying drawings and specific embodiments. Advantages and features of the invention will become more apparent from the following description and from the claims. It should be noted that the drawings are in a very simplified form and are all to a non-precise scale, merely for convenience and clarity in aiding in the description of embodiments of the invention.
In addition, features of different embodiments of the invention may be combined with each other, unless otherwise specified. For example, a feature of the second embodiment may be substituted for a corresponding feature of the first embodiment, or may have the same or similar function, and the resulting embodiment would fall within the disclosure or scope of the disclosure.
The invention provides a dynamic preparation method and a dynamic preparation device for an annular cluster porous transmitting needle tip, which aim to solve the problem that the existing needle tip preparation method is not suitable for preparing the annular cluster porous transmitting needle tip.
In order to realize the above-mentioned thought, the invention provides a dynamic preparation method and device of the needle tip of the annular cluster porous transmitting needle, comprising: a firing pin module configured to hold an annular bundled porous firing pin; a solution module configured to carry a solution that reacts with the annular bundled porous emitter pins; and a movement device configured to drive the emitter needle module to move so as to immerse the annular cluster porous emitter needle in the solution; wherein: immersing the annular bundling porous transmitting needle into the solution for calibration, and after the annular bundling porous transmitting needle reaches the parameter requirement, driving the annular bundling porous transmitting needle to move upwards to leave the liquid level of the solution by a moving device, calibrating the up-and-down round trip times, so as to finish the needle point calibration; the annular bundling porous transmitting needle is immersed into the solution for preparation, and after the annular bundling porous transmitting needle reaches the calibrated up-and-down round trip times, the moving device drives the annular bundling porous transmitting needle to move upwards to leave the liquid level of the solution, so that the preparation of the needle point is completed.
The invention provides a dynamic preparation device of an annular cluster porous transmitting needle tip, as shown in fig. 4, comprising: a firing pin module 30 configured to hold a plurality of annular bundled porous firing pins 31 by a firing pin fixture 32; a solution module 20 configured to carry a solution 22 that reacts with the annular bundled porous emitter pins 31; and a movement means configured to move the emitter needle module 30 so that the ring-shaped cluster porous emitter needle 31 is immersed in the solution 22; wherein: immersing the annular bundling porous emission needle 31 into the solution 22 for calibration, and after the annular bundling porous emission needle 31 meets the parameter requirement, driving the annular bundling porous emission needle 31 to move upwards to leave the solution level by a moving device, calibrating the up-and-down round trip times, so as to finish the needle point calibration; the annular cluster porous emission needle 31 is immersed into the solution 22 for preparation, and after the annular cluster porous emission needle 31 reaches the calibrated up-and-down round trip times, the movement device drives the annular cluster porous emission needle 31 to move upwards to leave the solution liquid level, so that the preparation of the needle point is completed.
In one embodiment of the present invention, in the dynamic preparation device of the annular cluster porous emission needle tip, the movement device includes: a linkage configured such that the firing pin module 30 is secured to the motion control module 70 by the linkage; a bracket 60 configured to be vertically fixed on the base 10; the motion control module 70 is configured to be vertically fixed on the bracket 60 and can drive the connecting rod to move up and down along the bracket 60; and a support block 80 configured to reinforce the bracket 60 from shaking. In the dynamic preparation device of the annular cluster porous transmitting needle tip, the connecting rod comprises a transverse connecting rod 40 and a vertical connecting rod 50, wherein: the transverse connecting rod 40 is horizontally arranged and fixed on the vertical connecting rod 50; the vertical link 50 is vertically disposed and fixed to the motion control module 70.
In one embodiment of the present invention, in the apparatus for dynamically preparing a needle tip of the annular cluster porous emission needle, the motion control module 70 includes a screw nut mechanism 71, a driver 72, and a controller 73, wherein: the screw nut mechanism 71 is vertically fixed on the bracket 60; the driver 72 and the controller 73 are fixed to the base 10.
In one embodiment of the present invention, in the apparatus for dynamically preparing a tip of the annular cluster porous emission needle, the solution module 20 includes: a solution tank 21 configured to be horizontally fixed on the base 10; a solution 22 configured to be contained in the solution tank 21, the solution level being higher than the stainless steel ring 24, wherein the solution is a NaOH solution; a cathode holder 23 configured to be fixed in the solution tank 21 and to form a support for the stainless steel ring 24; stainless steel ring 24 is configured to connect to a negative electrode of a power source to act as a cathode for an electrochemical reaction.
In one embodiment of the present invention, in the dynamic preparation device of the needle tip of the annular cluster porous emission needle, the relative position between the motion control module 70 and the solution module 20 is adjusted so that the annular cluster porous emission needle 31 is coaxial with the stainless steel ring 24; the motion control module 70 drives the connecting rod to move up and down along the bracket 60 so as to drive the emitting needle module 30 to move up and down, so that the annular cluster porous emitting needle 31 is immersed in the solution 22 or leaves the solution level; the upward movement limit position includes: the annular cluster porous emission needle 31 is positioned at a certain distance above the liquid level of the solution; the descent movement limit position includes: the annular cluster porous emission needle 31 is positioned below the solution level and does not contact the bottom of the solution tank 21; the material of the annular cluster porous transmitting needle 31 comprises tungsten or rhenium; the annular cluster porous emission needle 31 is connected with the positive electrode of a power supply to serve as an anode of an electrochemical reaction.
In one embodiment of the present invention, in the dynamic preparation device of the annular cluster porous emission needle tip, the inner diameter of the stainless steel ring 24 is 40mm, and the thickness of the stainless steel ring 24 is 1mm; the base diameter of the annular cluster porous transmitting needle 31 is 9mm; the substrate of the annular cluster porous transmitting needle 31 is uniformly distributed with 25 tungsten transmitting needles or rhenium transmitting needles with the length of 5mm and the diameter of 0.5 mm.
The invention also provides a preparation method realized by the dynamic preparation device of the annular cluster porous emission needle tip, which comprises the steps of: immersing the annular cluster porous transmitting needle 31 into the solution liquid surface for a certain depth, and loading voltage between the annular cluster porous transmitting needle 31 and the stainless steel ring 24; the motion control module 70 drives the annular cluster porous transmitting needle 31 to do up-and-down reciprocating motion away from the liquid level and immersed in the liquid level at a certain speed; the change relation between the radius size of each annular cluster porous transmitting needle 31 and the up-down reciprocating times under the conditions of different inter-electrode voltages, solution concentrations, immersion liquid level depths and reciprocating motion rates is recorded, and finally, the preparation parameters capable of enabling the radius size of all needle points to be smaller than 3 microns are obtained, and the calibration process is completed.
In one embodiment of the invention, in the dynamic preparation method of the annular cluster porous emission needle tip, the preparation parameters comprise the calibrated voltage, the calibrated concentration solution, the calibrated depth, the calibrated reciprocating motion rate and the calibrated up-and-down round trip times; the calibrated voltage is 5V, the calibrated concentration solution is 1mol/L, the calibrated depth is 1mm, the calibrated reciprocating speed is 0.5mm/s, and the calibrated up-and-down round trip times are 220 times.
In one embodiment of the present invention, in the dynamic preparation method of the annular cluster porous emission needle tip, the immersing of the annular cluster porous emission needle 31 into the solution for preparation includes: the calibrated voltage is loaded between the anode and the cathode, the transmitting needle is immersed into the calibrated concentration solution to the calibrated depth, the motion control module 70 drives the annular cluster porous transmitting needle 31 to do up-and-down reciprocating motion away from the liquid surface and immersed into the liquid surface at the calibrated reciprocating motion rate, until the up-and-down reciprocating motion times reach the calibrated up-and-down reciprocating motion times, the motion control module 70 automatically drives the annular cluster porous transmitting needle 31 to move upwards away from the liquid surface, and the needle point preparation process is finished.
The inventors of the present invention have found through studies that, in a method of forming a needle tip by loading a constant current source or a constant voltage source between a needle to be prepared and an electrode until the needle breaks at a contact point of an electrolyte liquid surface, a manner of breaking the needle in the middle to form the needle tip is adopted, and a manner of breaking the needle from the middle is not suitable for simultaneous preparation of a plurality of needle tips. In the process of preparing the needle point by the electrochemical corrosion method, the concentration distribution of the electrolyte is uneven caused by the factors such as surface tension, electrochemical reaction product falling, electrostatic force on the absorption of the reaction product and the like, so that the reaction of the transmitting needle at the liquid level is fastest, the transmitting needle at the liquid level is in a neck shape, as shown in figure 2, and the transmitting needle is finally broken at the position under the pulling action of the gravity of the transmitting needle at the lower end along with the progress of electrochemical corrosion, so that the needle point is formed. However, for the porous type emitting needle sintered from powder particles, there is a certain difference in the internal particle size and distribution uniformity, which inevitably causes a difference in the electrochemical reaction rate of each emitting needle, resulting in a difference in the breaking timing of the lower emitting needle and a large difference in the size of each needle tip; on the other hand, the difference in electrochemical reaction rate of each of the needles causes the difference in diameter change of the lower end needle, the abrupt diameter change causes the change in surface tension, and thus the "neck" position may be changed, as shown in fig. 3, the secondary or multiple occurrences of the "neck" position will cause the needles to be re-corroded at new sites, resulting in a difference in breaking time of several minutes or even several tens minutes of different needles, and in this time difference, the already formed needle tip will be further electrochemically corroded to become blunt, and finally the needle tip meeting the required size cannot be prepared.
The method for forming the needle point by carrying out up-and-down reciprocating lifting movement on the transmitting needle and finally breaking the transmitting needle at the liquid level is characterized in that a 'neck' is firstly generated on the transmitting needle at the liquid level, then the transmitting needle is carried out small-amplitude up-and-down reciprocating lifting movement by taking the 'neck' as a center point, and the transmitting needle near the 'neck' is corroded through electrochemical reaction until the transmitting needle breaks. Similar to the process of preparing the needle tip by the intermediate breaking method, the difference of particles inside the porous emission needle will cause the breaking time of the emission needle to be different, which is not suitable for preparing the needle tip of the annular cluster porous emission needle 31.
In addition, the spacing between the individual emission needles in the annular cluster emission needle is small, and the individual emission needles are affected by each other by the peripheral emission needles during the preparation of the needle tip, so that the existing method and apparatus cannot satisfy the preparation of the needle tip of the annular cluster porous emission needle 31.
The inventors of the present invention also found in the study that: the dynamic preparation device of the annular cluster porous transmitting needle tip (the stainless steel ring 24 is a cathode connected with a power supply cathode and horizontally placed in the NaOH solution 22), the annular cluster porous transmitting needle 31 is an anode connected with a power supply anode, is coaxial with the stainless steel ring 24, is vertically immersed into the NaOH solution for a certain depth and performs up-and-down reciprocating motion), has the following conditions: the change of interelectrode voltage, solution concentration, immersed liquid level depth and reciprocating motion rate parameters can influence the reaction rate of all parts of the emitting needle under the liquid level while the emitting needle under the liquid level of the solution is subjected to electrochemical reaction to gradually dissolve and thin under the action of an electric field between an anode and a cathode and the solution.
The inventors have analyzed to conclude that: unlike the process of preparing a single needle tip, the reaction rate of each needle in the ring-shaped cluster porous needle 31 is affected by the interelectrode voltage, the solution concentration, and the immersion liquid level depth, and the reaction rate of the ring-shaped cluster porous needle 31 is affected more by the adjacent needles because each needle is adjacent to the adjacent needle, affecting the electric field distribution between the needle and the stainless steel ring 24 and thus affecting the reaction rates of different parts of the lower end of the needle.
Further, the inventors of the present invention have found through a great number of experiments that by reciprocating the annular cluster porous emitter pins 31 away from the liquid surface and immersed in the liquid surface, on the one hand, the contact time between the lower ends of the emitter pins and the solution is increased to increase the electrochemical reaction time, and on the other hand, the up-and-down reciprocating motion of the emitter pins drives the electrochemical reaction products to move so as to change the electric field distribution near the emitter pins at the lower ends, the result that "necks" are not generated at the liquid surface and the reaction rate at the lower ends of the emitter pins increases with the depth, that is, the reaction rate at the tail ends of the emitter pins is fastest, can be obtained.
Thus, the required needle tip size can be finally obtained with the progress of time; meanwhile, as the reaction rates of different needle points are slightly different, in order to prevent the needle points which have reached the size requirement from being corroded continuously in the solution and becoming blunt, when the parameters for preparing the needle points are selected, lower working voltage and/or solution concentration should be selected to reduce the size difference of the needle points caused by different reaction rates of the needle points; in addition, in order to prevent the liquid level from severely fluctuating due to the upward and downward movement of the firing pin, a lower upward and downward reciprocation rate of the firing pin should be selected.
Based on the insight, the invention provides a dynamic preparation method and a dynamic preparation device for the needle tip of an annular cluster porous transmitting needle, wherein a transmitting needle module 30 for clamping the annular cluster porous transmitting needle 31 is driven by a motion device to move, so that the annular cluster porous transmitting needle 31 is immersed in a solution, the uniform movement of multiple needles of the annular cluster porous transmitting needle 31 is realized, and the synchronous preparation is realized; in addition, the annular bundling porous emission needle 31 is immersed into the solution for calibration, after the annular bundling porous emission needle 31 meets the parameter requirement, the movement device drives the annular bundling porous emission needle 31 to move upwards to leave the liquid level of the solution, the up-and-down round trip times are calibrated, the needle point calibration is completed, the optimal preparation parameters are obtained before preparation, and the preparation effect is enabled to reach the best effect; further, the annular cluster porous transmitting needle 31 is immersed into the solution for preparation, and after the annular cluster porous transmitting needle 31 reaches the calibrated up-and-down round trip times, the moving device drives the annular cluster porous transmitting needle 31 to move upwards to leave the liquid level of the solution, so that the preparation of the needle point is completed.
Therefore, the invention creatively proposes that the ring-shaped cluster porous transmitting needle 31 is immersed into the solution for calibration before preparation, so that the optimal preparation parameters are obtained, and the defects easily occurring in the existing preparation method are prevented.
The inventor of the invention has explored and obtained interelectrode voltage, solution concentration, immersed solution depth, up-and-down reciprocating motion rate and motion times which can prepare the needle tip meeting the requirements through a large number of experiments, and has verified the dynamic preparation method and device of the annular cluster porous transmitting needle tip. The method can realize the simultaneous preparation of a plurality of needle points of the annular cluster porous transmitting needle 31, the size of the processed needle points meets the requirement, the consistency is better, the method is simple, only the up-and-down reciprocating movement times of the transmitting needle are controlled, and the degree of automation is high.
Specifically, the calibration process includes: the annular cluster porous emission needle 31 is immersed into the liquid level of the NaOH solution 22 to a certain depth, voltage is applied between the anode emission needle 31 and the cathode ring 24, the motion control module 70 drives the annular cluster porous emission needle 31 to reciprocate up and down away from the liquid level and immersed into the liquid level at a certain speed, and the change relation between the radius size of each emission needle and the up and down reciprocating times is recorded under different inter-pole voltages, solution concentrations, immersed liquid level depths and reciprocating motion speeds, wherein the radius size of each emission needle is measured under a microscope. Finally, the preparation parameters of which the radius of the needle tip is smaller than 3 micrometers are 5V, 1mol/L, 1mm, 0.5mm/s and 220 times, thereby completing the calibration process.
Further, the preparation process comprises the following steps: 5V voltage is loaded between the anode emission needle 31 and the cathode ring 24, the emission needle is immersed in NaOH solution with the concentration of 1mol/L to the depth of 1mm, the motion control module 70 drives the annular cluster porous emission needle 31 to do up-and-down reciprocating motion which leaves the liquid surface and is immersed in the liquid surface at the speed of 0.5mm/s until the up-and-down reciprocating motion times reach 220, the motion control module 70 automatically drives the annular cluster porous emission needle 31 to move upwards to leave the liquid surface, and the needle point preparation process is finished.
In summary, the above embodiments describe in detail different configurations of the method and apparatus for dynamically preparing an annular clustered porous emitter needle tip, and of course, the present invention includes, but is not limited to, the configurations listed in the above embodiments, and any contents of changing the configurations provided in the above embodiments fall within the scope of the present invention. One skilled in the art can recognize that the above embodiments are illustrative.
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 system disclosed in the embodiment, the description is relatively simple because of corresponding to the method disclosed in the embodiment, and the relevant points refer to the description of the method section.
The above description is only illustrative of the preferred embodiments of the present invention and is not intended to limit the scope of the present invention, and any alterations and modifications made by those skilled in the art based on the above disclosure shall fall within the scope of the appended claims.

Claims (8)

1. A method of manufacturing by a dynamic manufacturing apparatus for an annular bundled porous emitter needle tip, the dynamic manufacturing apparatus comprising:
a firing pin module configured to hold an annular bundled porous firing pin;
a solution module configured to carry a solution that reacts with the annular bundled porous emitter pins; and
the movement device is configured to drive the transmitting needle module to move so as to enable the annular cluster porous transmitting needle to be immersed in the solution; wherein:
immersing the annular bundling porous transmitting needle into the solution for calibration, and after the annular bundling porous transmitting needle reaches the parameter requirement, driving the annular bundling porous transmitting needle to move upwards to leave the liquid level of the solution by a moving device, calibrating the up-and-down round trip times, so as to finish the needle point calibration;
immersing the annular bundling porous emission needle into the solution for preparation, and driving the annular bundling porous emission needle to move upwards to leave the liquid level of the solution by the movement device after the annular bundling porous emission needle reaches the calibrated up-down round trip times, so as to finish the preparation of the needle point;
wherein immersing the annular cluster porous emitter needle into the solution for calibration comprises:
immersing the annular cluster porous transmitting needle into the liquid level of the solution for a certain depth, and loading voltage between the annular cluster porous transmitting needle and the stainless steel ring;
the motion control module drives the annular cluster porous transmitting needle to do up-and-down reciprocating motion leaving the liquid level and immersing the liquid level at a certain speed;
recording the change relation between the radius size of each annular cluster porous transmitting needle and the up-down reciprocating frequency under the conditions of different inter-pole voltages, solution concentrations, immersion liquid level depths and reciprocating motion rates, and finally obtaining the preparation parameters which can enable the radius size of all needle points to be smaller than 3 microns, thereby completing the calibration process;
the preparation parameters comprise calibrated voltage, calibrated concentration solution, calibrated depth, calibrated reciprocating motion rate and calibrated up-and-down round trip times;
wherein immersing the annular cluster porous emitter needle into the solution for preparation comprises:
and loading a calibrated voltage between the anode and the cathode, immersing the transmitting needle into a calibrated concentration solution to a calibrated depth, driving the annular cluster porous transmitting needle to do up-and-down reciprocating motion away from the liquid surface and immersed into the liquid surface at a calibrated reciprocating motion rate by the motion control module, and automatically driving the annular cluster porous transmitting needle to move upwards away from the liquid surface by the motion control module until the up-and-down reciprocating motion times reach the calibrated up-and-down reciprocating motion times, wherein the needle point preparation process is finished.
2. The method of manufacturing according to claim 1, wherein the movement means comprises:
a linkage configured to secure the firing pin module to the motion control module via the linkage;
a bracket configured to be vertically fixed on the base;
the motion control module is configured to be vertically fixed on the bracket and can drive the connecting rod to move up and down along the bracket; and
and the support block is configured to strengthen the support and prevent the support from shaking.
3. The method of manufacturing of claim 2, wherein the links comprise transverse links and vertical links, wherein:
the transverse connecting rod is horizontally arranged and fixed on the vertical connecting rod; the vertical connecting rod is vertically arranged and fixed on the motion control module.
4. The method of manufacturing of claim 2, wherein the motion control module comprises a lead screw nut mechanism, a driver, a controller, wherein:
the screw nut mechanism is vertically fixed on the bracket; the driver and the controller are fixed on the base.
5. The method of preparing as claimed in claim 2, wherein the solution module comprises:
a solution tank configured to be horizontally fixed on the base;
the solution is configured to be contained in the solution tank, the liquid level of the solution is higher than that of the stainless steel ring, and the solution is NaOH solution;
a cathode support configured to be fixed within the solution tank and to form a support for the stainless steel ring;
a stainless steel ring configured to connect to a negative electrode of a power source to act as a cathode for an electrochemical reaction.
6. The method of manufacturing according to claim 5, wherein the relative position between the motion control module and the solution module is adjusted such that the annular bundled porous emitter needle is coaxial with the stainless steel ring;
the motion control module drives the connecting rod to do lifting movement along the bracket so as to drive the transmitting needle module to do lifting movement, so that the annular cluster porous transmitting needle is immersed in the solution or separated from the solution level;
the upward movement limit position includes: the annular cluster porous transmitting needle is positioned at a certain distance above the liquid level of the solution;
the descent movement limit position includes: the annular cluster porous emission needle is positioned below the liquid level of the solution and is not contacted with the bottom of the solution tank;
the material of the annular cluster porous transmitting needle comprises tungsten or rhenium;
the annular cluster porous transmitting needle is connected with the positive electrode of the power supply to serve as the anode of the electrochemical reaction.
7. The method of manufacturing according to claim 6, wherein the inner diameter of the stainless steel ring is 40mm, and the thickness of the stainless steel ring is 1mm;
the diameter of the base of the annular cluster porous transmitting needle is 9mm;
and 25 tungsten emission needles or rhenium emission needles with the length of 5mm and the diameter of 0.5mm are uniformly distributed on the substrate of the annular cluster porous emission needle.
8. The method of claim 1, wherein the voltage is 5V, the concentration of the solution is 1mol/L, the depth is 1mm, the reciprocating rate is 0.5mm/s, and the number of up-and-down trips is 220.
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CN102586854A (en) * 2012-02-24 2012-07-18 西安交通大学 High-efficiency automatic tungsten needle manufacturing device and method
CN106501555A (en) * 2016-12-01 2017-03-15 西安交通大学 A kind of preparation facilitiess of ultralow roughness tungsten tipped probe and method
CN109706515A (en) * 2019-01-11 2019-05-03 中国电子科技集团公司第三十八研究所 A kind of preparation facilities and preparation method of the tungsten wire needle point of controllable draw ratio

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20010076680A (en) * 2000-01-27 2001-08-16 이억기 Method for manufacturing a probe using electrolytic processing
CN102586854A (en) * 2012-02-24 2012-07-18 西安交通大学 High-efficiency automatic tungsten needle manufacturing device and method
CN106501555A (en) * 2016-12-01 2017-03-15 西安交通大学 A kind of preparation facilitiess of ultralow roughness tungsten tipped probe and method
CN109706515A (en) * 2019-01-11 2019-05-03 中国电子科技集团公司第三十八研究所 A kind of preparation facilities and preparation method of the tungsten wire needle point of controllable draw ratio

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