CN112680729B - Short circuit prevention method for conductive electrode on inner surface of capillary tube or special tube - Google Patents

Short circuit prevention method for conductive electrode on inner surface of capillary tube or special tube Download PDF

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Publication number
CN112680729B
CN112680729B CN202011324722.4A CN202011324722A CN112680729B CN 112680729 B CN112680729 B CN 112680729B CN 202011324722 A CN202011324722 A CN 202011324722A CN 112680729 B CN112680729 B CN 112680729B
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electrode
capillary
tube
high molecular
short circuit
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CN112680729A (en
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孙立东
赵凯岐
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Lidong New Materials Technology (Shandong) Co.,Ltd.
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Chongqing University
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Priority to EP21893475.0A priority patent/EP4086369A4/en
Priority to PCT/CN2021/112807 priority patent/WO2022105323A1/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/26Anodisation of refractory metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/005Apparatus specially adapted for electrolytic conversion coating
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/34Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/005Contacting devices
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/10Electrodes, e.g. composition, counter electrode

Abstract

The invention provides a method for preventing short circuit of a conductive electrode on the inner surface of a capillary tube or a special tube. The high molecular polymer solution solvent to be prepared is one of N-methyl pyrrolidone (NMP) and N, N-dimethyl formamide (DMF), the solute is one of high molecular polymers such as polylactic acid (PLA), polyvinyl chloride (PVC), polyvinylidene fluoride (PVDF) and the like, and the high molecular polymer film coated on the electrode can ensure that a cathode and an anode normally react under the action of an electric field in the electrochemical reaction process, and the short circuit cannot occur even if the cathode and the anode are contacted with each other under the action of external force. The method has the advantages of convenient operation, wide applicability, low cost and the like.

Description

Short circuit prevention method for conductive electrode on inner surface of capillary tube or special tube
Technical Field
The invention relates to the field of short circuit prevention of electrode materials, in particular to a method for preventing short circuit of a conductive electrode on the inner surface of a capillary or a special pipe.
Background
Electrochemical treatment is one of branches of chemical treatment, and is widely applied to the fields of energy, biology, environment, metal material surface modification and the like. The electrochemical reaction device generally comprises a power supply, a cathode, an anode, an electrolyte and the like. The cathode and the anode are made of conductive materials to ensure the conduction of system current. In an open system, the distance between the cathode and the anode is large and can be adjusted, and the contact cannot occur due to the action of external force (such as air bubbles floating upwards, the stress of the liquid flow action on the cathode and the anode, and the like) in the reaction process. However, for a semi-closed system (such as a capillary tube and a special-shaped tube) with limited area, the distance between the cathode and the anode is small, so that the cathode and the anode are easy to contact under the action of external force, and the short circuit between the cathode and the anode is caused, so that the reaction cannot be smoothly carried out. For example, when the inner surfaces of capillary tubes or special tubes such as capillary metal tubes, needle tubes for detection, heat dissipation copper tubes for mobile phones, spiral titanium tubes for condensation and the like are subjected to super-wetting modification by adopting an electrochemical reaction method, the capillary tubes or the special tubes are used as anodes, and cathode wires need to be arranged in the capillary tubes or the special tubes, but the prior art cannot ensure that the cathode wires and the capillary tubes or the special tubes are not short-circuited in the reaction process, and even super-wetting coatings are prepared on the inner surfaces of the capillary tubes or the special tubes. Therefore, it is urgently needed to develop a short circuit prevention method for the conductive electrode on the inner surface of the capillary tube or the special tube, which avoids short circuit, is convenient to operate, has wide applicability and is low in cost.
Disclosure of Invention
The invention aims to provide a method for preventing short circuit of a conductive electrode on the inner surface of a capillary or a special pipe, which is characterized by preparing a high-molecular polymer solution; the solvent of the solution is one of N-methylpyrrolidone (NMP) and N, N-Dimethylformamide (DMF), and the solute is one of polymer materials such as polylactic acid (PLA), polyvinyl chloride (PVC), polyvinylidene fluoride (PVDF) and the like;
and cleaning the electrode penetrating into the capillary or the special-shaped tube, drying, coating a high molecular polymer solution on the surface of the electrode, and drying. After the electrode penetrates into the capillary tube or the special tube, the electrochemical treatment needs to be carried out on the capillary tube or the special tube. For example, the surface of the tube is treated by immersing the tube in an electrolyte, the penetrated electrode is used as a cathode or an anode, and the other electrode is a capillary tube or a special tube (the capillary tube, the special tube and the electrode are all made of conductive materials).
Further, the concentration of the high molecular polymer solution is 10 to 100g/L.
Further, the electrode is an electrode wire made of stainless steel, copper, iron, platinum or titanium.
Further, when coating the high molecular polymer, the coating is performed by coating the high molecular polymer solution and drying.
Further, the thickness of the polymer film coated on the electrode is 1 to 50 μm.
Further, the capillary tube or the special-shaped tube is a capillary metal tube, a needle tube for detection, a heat dissipation copper tube for a mobile phone or a spiral titanium tube for condensation.
Furthermore, the cleaning time of the electrode is 0.5-4 h, the drying temperature is 50-80 ℃, and the drying time is 2-5 h.
Further, after the high molecular polymer solution is coated, the temperature for drying the electrode is 50-80 ℃, and the drying time is 0.5-4 h.
Compared with the prior art, the invention has the following remarkable advantages and beneficial effects:
1. the problem that the anode and the cathode are easy to short circuit in a limited-area semi-closed system is solved;
2. the operation is convenient, and the process production difficulty is low;
3. wide application, and no limitation to the size and material of the cathode and anode.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a coated high molecular polymer short-circuit prevention electrode.
FIG. 2 is a scanning electron micrograph of the cathode filament coated with the high molecular weight polymer film. In the figure, (a) is a surface view of the cathode filament, (b) is a cross-sectional view of the cathode filament, (c) is a surface view of the film before the electrochemical reaction, and (d) is a surface view of the film after the electrochemical reaction.
FIG. 3 is a scanning electron micrograph of a titanium dioxide nanotube array prepared on the inner surface of a titanium tube with an inner diameter of 0.4mm by using an electrochemical anodic oxidation method according to the method of the present invention.
FIG. 4 is a statistical result of uniformity of a titanium dioxide nanotube array manufactured on the inner surface of a titanium tube with an inner diameter of 0.4mm and a length of 70mm by using an electrochemical anodic oxidation method according to the method of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, but it should not be construed that the scope of the above-described subject matter is limited to the following examples. Various substitutions and alterations can be made without departing from the technical idea of the invention and the scope of the invention is covered by the present invention according to the common technical knowledge and the conventional means in the field.
Example 1:
in the method for preventing short circuit of the conductive electrode on the inner surface of the capillary or the special pipe, a molecular polymer solution with polyvinylidene fluoride as a solute and N-methylpyrrolidone as a solvent, the concentration of which is 10g/L, needs to be prepared.
The method comprises the following steps:
(1) Sequentially carrying out ultrasonic vibration cleaning on a stainless steel wire electrode with the diameter of 0.2mm in a detergent, alcohol and deionized water for 0.5h respectively;
(2) Drying the stainless steel wire by using a nitrogen spray gun;
(3) Drying the stainless steel wire at 50 ℃ for 1h;
(4) Repeatedly coating the high molecular polymer solution on the surface of the dried stainless steel wire serving as a substrate, wherein the coating times are 20-25;
(5) Drying the stainless steel wire coated with the polyvinylidene fluoride solution at the drying temperature of 50 ℃ for 2h;
(6) Stainless steel wires are penetrated into a dry capillary titanium tube with the inner diameter of 0.4mm, a power supply is connected, and electrolyte is introduced for electrochemical treatment (anodic oxidation treatment).
The relevant performance data for this example is as follows:
in the comparative experiment, the uncoated, 0.2mm diameter stainless steel wire, which is a metal, alone as the cathode in the anodic oxidation process, left only 0.2mm due to the remaining space in the tube. When the electrolyte is introduced, the electrolyte has a scouring effect on the cathode stainless steel wire, so that the cathode stainless steel wire is easy to contact with the anode capillary titanium tube to cause short circuit. As shown in fig. 2, by coating a high molecular polymer film, the outer surface of the treated cathode stainless steel wire is coated with a high molecular polymer diaphragm with a thickness of about 20-30 μm, and the diaphragm can separate the anode and the cathode during anodic oxidation, so as to prevent short circuit and not shield an electric field, so that anodic oxidation can be performed. As shown in FIG. 3, the length of the titanium dioxide nanotube array prepared by anodic oxidation is about 3 μm, and the titanium dioxide nanotube array has the characteristics of smooth tube wall, good opening and the like. FIG. 4 presents statistics of the lengths of nanotube arrays at different positions on the inner surface of the capillary titanium type tube, and illustrates that the thickness of the prepared nano-coating is uniformly controllable. Meanwhile, the method has the advantages of convenient operation, wide application range, low cost and the like.
Example 2
The difference from the embodiment 1 is that:
1. in the step (1), the electrode is a platinum wire with the diameter of 0.4mm.
2. In the step (4), the solute of the high molecular polymer is polylactic acid (PLA), the solvent is N-methylpyrrolidone (NMP), the concentration of the solution is 20g/L, and the coating times are 20-25.
3. In the step (6), the anode is a stainless steel capillary tube with the inner diameter of 1 mm.
Example 3
The difference from the embodiment 1 is that:
1. in the step (1), the electrode is a copper wire with the diameter of 0.6mm.
2. In the step (4), the solute of the high molecular polymer is polyvinyl chloride (PVC), the solvent is N-methylpyrrolidone (NMP), the concentration of the solution is 10g/L, and the coating times are 15-20.
3. In the step (6), the anode is an aluminum alloy capillary tube with the inner diameter of 1.5mm.
Example 4
The difference from the embodiment 1 is that:
1. in the step (1), the electrode is made of iron wire with the diameter of 1mm
2. In the step (4), the solute of the high molecular polymer is polyvinylidene fluoride (PVDF), the solvent is N, N-Dimethylformamide (DMF), the concentration of the solution is 15g/L, and the coating times are 10-15.
3. In the step (6), the anode is a spiral capillary titanium heat exchange tube with the inner diameter of 2.5 mm.
Example 5
The difference from the embodiment 1 is that:
1. in the step (1), the electrode is a titanium wire with the diameter of 1.5mm.
2. In the step (6), the anode is a special-shaped copper alloy pipe with a rectangular inner section (the length is 5.5mm, and the width is 3.0 mm).
Example 6
The difference from the embodiment 1 is that:
1. in the step (1), the electrode is a titanium wire with the diameter of 0.5mm.
2. In the step (6), the anode is an L-shaped special titanium tube with the inner diameter of 3.0 mm.
Example 7
The difference from the embodiment 1 is that:
1. in the step (1), the electrode is made of iron wire with the diameter of 0.4mm.
2. In the step (6), the anode is a T-shaped stainless steel tube with the inner diameter of 2.5 mm.
Example 8
The difference from the embodiment 1 is that:
1. in the step (1), the electrode is made of iron wire with the diameter of 0.4mm.
2. In the step (6), the anode is a V-shaped stainless steel tube with the inner diameter of 2.5 mm.

Claims (6)

1. A method for preventing short circuit of conductive electrode on inner surface of capillary or special pipe is characterized in that high molecular polymer solution is prepared; the solvent of the solution is one of N-methyl pyrrolidone (NMP) and N, N-dimethyl formamide (DMF), and the solute is one of high molecular materials such as polylactic acid (PLA), polyvinyl chloride (PVC), polyvinylidene fluoride (PVDF) and the like;
cleaning an electrode penetrating into a capillary or a special-shaped tube, drying, and coating a high molecular polymer on the surface of the electrode; the concentration of the high molecular polymer solution is 10 to 100g/L; the thickness of the high molecular polymer film coated on the electrode is 1-50 μm.
2. The method for preventing short circuit of conductive electrode on inner surface of capillary or special pipe according to claim 1, wherein: the electrode is an electrode wire made of stainless steel, copper, iron, platinum or titanium.
3. The method for preventing short circuit of conductive electrode on inner surface of capillary or special pipe according to claim 1, wherein: when coating the high molecular polymer, coating the high molecular polymer solution and drying.
4. The method for preventing short circuit of conductive electrode on inner surface of capillary or special pipe according to claim 1, wherein: the capillary tube or the special-shaped tube is a capillary metal tube, a needle tube for detection, a heat dissipation copper tube for a mobile phone or a spiral titanium tube for condensation.
5. The method for preventing short circuit of conductive electrode on inner surface of capillary or special pipe according to claim 1, wherein: the cleaning time of the electrode is 0.5-4 h, the drying temperature is 50-80 ℃, and the drying time is 2-5 h.
6. The method for preventing short circuit of conductive electrode on inner surface of capillary or special pipe according to claim 1, wherein: after the high molecular polymer solution is coated, the temperature for drying the electrode is 50-80 ℃, and the drying time is 0.5-4 h.
CN202011324722.4A 2020-11-23 2020-11-23 Short circuit prevention method for conductive electrode on inner surface of capillary tube or special tube Active CN112680729B (en)

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Application Number Priority Date Filing Date Title
CN202011324722.4A CN112680729B (en) 2020-11-23 2020-11-23 Short circuit prevention method for conductive electrode on inner surface of capillary tube or special tube
EP21893475.0A EP4086369A4 (en) 2020-11-23 2021-08-16 Method for preventing short circuiting between inner surface of capillary tube or special-shaped tube and conductive electrode
PCT/CN2021/112807 WO2022105323A1 (en) 2020-11-23 2021-08-16 Method for preventing short circuiting between inner surface of capillary tube or special-shaped tube and conductive electrode

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CN112680729B (en) * 2020-11-23 2022-10-14 重庆大学 Short circuit prevention method for conductive electrode on inner surface of capillary tube or special tube

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