CN110297019B

CN110297019B - Preparation, sealing, opening and assembling of pen-tube type portable probe and design method thereof

Info

Publication number: CN110297019B
Application number: CN201910560527.2A
Authority: CN
Inventors: 齐建涛; 李振轩; 赵晶晶; 王思权; 张智松; 丁一航
Original assignee: China University of Petroleum East China
Current assignee: China University of Petroleum East China
Priority date: 2019-06-26
Filing date: 2019-06-26
Publication date: 2021-08-06
Anticipated expiration: 2039-06-26
Also published as: CN110297019A

Abstract

The invention discloses a pen-type portable probe preparation, sealing, opening, assembling and design method, which adopts a multi-technology coupling method such as a potentiostat, an XYZ level meter and the like to prepare a tungsten wire probe (the necking length is 300-5 microns, and the tip diameter is 1-5 microns), and utilizes an asphalt sealing and opening technology to finish different functions of portable transportation and stable use. The 3D printing pen tube front end, the pen tube rear end and the pen cap part are used for achieving pen tube type assembly and use, and safe transportation and use of the probe are guaranteed.

Description

Preparation, sealing, opening and assembling of pen-tube type portable probe and design method thereof

Technical Field

The invention relates to a pen-tube type portable probe preparation, sealing, opening, assembling and design method.

Background

Electrochemical and physical information of local corrosion micro-areas are important parameters for representing metal corrosion rate, but the test precision is limited due to the irregularity of local corrosion areas and the limitation of mesoscopic size. Recently developed techniques of scanning electrochemical microscopy and scanning vibrating electrode have become hot spots for micro-area electrochemical research, however, the key of these techniques lies in the preparation and use of micro-area electrode probes. The patent provides a pen-holder type portable probe preparation, sealing, opening, assembling and design method thereof, which are beneficial to probe protection and use and greatly improve the safety life of micro-area testing.

Disclosure of Invention

The invention relates to a pen tube type portable probe preparation, sealing, opening, assembling and designing method thereof.

Aiming at a hypersensitive tungsten wire electrode (the diameter of 0.1-0.5 mm), etching for 5-20s in a potassium hydroxide solution (0.1-0.3M) by using a potentiostat (10-12V, the current density of 0.1-0.3A), observing the necking process of the tungsten wire electrode at the liquid level by using a movable camera until no bubbles exist, finishing the etching, and finishing the preparation of a needle point. The diameter of the tip is 1-5 microns, and the length of the constriction is 500 microns.

The method for sealing the needle point comprises the steps of melting asphalt on the resistance wire by using a constant potential rectifier (2-4V,6-9A), enabling the needle point of the assembled pen-type probe to face upwards, controlling the probe to move from bottom to top by using an XYZ level meter, and penetrating through the melted asphalt to realize packaging and storage. In addition, the tip was completely encapsulated with asphalt using an optical microscope test, and if not, encapsulation was repeated.

The specific size of the front end (1) of the pen tube is as follows: the thickness of the shell at the front end of the pen tube is 1.1mm, and M5-specification internal threads are processed on the inner wall of the shell and can be connected with M5 external threads at the rear end (2) of the pen tube.

The specific size of the rear end (2) of the pen tube is as follows: the thickness of the shell at the rear end of the pen tube is 0.8mm, and M5 external threads are processed on the outer wall of the shell and can be matched with M5 internal threads at the front end (1) of the pen tube.

Specific dimensions of the pen cap part: the thickness of the shell is 0.8 mm. The function is to protect the electrode tip from being deformed by impact when the electrode is not in use.

The method for opening the probe tip is that a potentiostat (2-4V,10-11.0A) is used for burning a resistance wire in red, the tip of an assembled pen-type probe is upward, an XYZ level meter controls the probe to move from bottom to top and to be close to the red burning resistance wire, burnt smoke is found at the tip or burnt smell is smelled, namely the tip opening is successful, the tip is removed, and the potentiostat is closed.

The invention has the following advantages:

(1) 3D printing can be realized by a pen-tube type portable probe assembling mode, and the pen-tube type portable probe is economical, efficient and convenient to carry;

(2) the needle tip part is sealed by asphalt, so that the safe service life of transportation and use is effectively prolonged;

(3) the needle point opening mode is efficient and convenient, and the accuracy and the high efficiency of experimental tests are facilitated.

Drawings

FIG. 1 is a barrel front end;

FIG. 2 is a rear end of the barrel;

FIG. 3 is a pen cap portion;

FIG. 4 is a schematic view of the barrel front end and barrel rear end mated by M5 threads.

In the figure: r3.8-the outer protruding radius of the pen tube is 3.8 mm; r3.1-the outer radius of the front section of the pen tube is 2.5 mm; r3.3-radius of the fillet at the tail part of the pen tube, 3.3 mm; r1.7-tail opening radius, 1.7 mm; r4.6-external radius of left view of pen cap, 4.6 mm; r3.8-inner radius of left view of pen cap, 3.8mm

Detailed Description

The front end, the rear end and the cap part of the pen barrel are printed according to the part drawing 3D.

Aiming at a hypersensitive tungsten wire electrode (0.25mm in diameter), a potentiostat (10-12V, the current density of 0.1-0.3A) is used for etching for 5-20s in a potassium hydroxide solution (0.1-0.3M), a movable camera is used for observing the necking process of the tungsten wire electrode at the liquid level until no bubbles exist, the etching is finished, and the preparation of the needle point is finished. The diameter of the tip is 1-5 microns, and the length of the constriction is 500 microns.

And observing the needle point by using a movable camera, winding the insulating white adhesive tape at the tail end of the necking (the distance from the needle point is about 1 mm), then taking the tungsten wire down from the clamp, and penetrating the tungsten wire into the front end of the pen tube until the fixing point of the white adhesive tape is finished. The interior of the pen tube is filled with epoxy resin and a curing agent (10:1), and the filling depth is the diameter-variable part (1) at the front end of the pen tube.

Asphalt on the resistance wire is melted by a constant potential rectifier (2-4V,6-9A), the tip of the assembled pen-type probe is upward, the probe is controlled by an XYZ level meter to move from bottom to top and penetrate through the melted asphalt, and packaging and storage are realized. In addition, the tip was completely encapsulated with asphalt using an optical microscope test, and if not, encapsulation was repeated.

The rear end (2) of the pen tube is screwed up in a matching way.

And (4) screwing the pen tube cap (3) at the front end of the pen tube in a matching manner, and completing the preparation of the pen tube type portable probe (4).

Before the sample is tested, the pen cap needs to be disassembled to expose the packaged needle point. Then, a constant potential rectifier (2-4V,10-11.0A) is used for burning the resistance wire, the needle point of the assembled pen-type probe is upward, the XYZ level instrument controls the probe to move from bottom to top and to be close to the red burning resistance wire, burnt smoke or burnt smell smells are found to appear at the needle point, namely the opening of the needle point is successful, the needle point is removed, and the constant potential rectifier is closed.

Claims

1. A preparation method of a pen-holder type portable probe is characterized by comprising the following specific parts:

a. the preparation method of the probe comprises the following steps: aiming at a hypersensitive tungsten wire electrode with the diameter of 0.1-0.5mm, under the conditions that the voltage is 10-12V and the current density is 0.1-0.3A, a potentiostat is used for etching for 5-20s in a potassium hydroxide solution with the concentration of 0.1-0.3M, a movable camera is used for observing the necking process of the tungsten wire electrode at the liquid level until no bubbles exist, the etching is finished, and the preparation of a needle point is finished; the diameter of the tip of the needle tip is 1-5 microns, and the length of the necking is 300-500 microns;

b. observing the needle point by using a movable camera, winding an insulating white adhesive tape at the tail end of the necking, wherein the distance between the insulating white adhesive tape and the needle point is about 1mm, then taking a tungsten filament down from the clamp, penetrating the tungsten filament into the front end of the pen tube until the fixing point of the white adhesive tape is finished, filling the interior of the pen tube with epoxy resin and a curing agent, wherein the filling depth is the diameter-variable part of the front end (1) of the pen tube, and thus obtaining the assembled pen tube type probe needle point;

c. the needle tip sealing method comprises the following steps: under the conditions that the voltage is 2-4V and the current density is 6-9A, asphalt on the resistance wire is melted by a constant potential rectifier, the tip of the assembled pen-type probe is upward, the probe is controlled by an XYZ level meter to move from bottom to top and penetrate through the melted asphalt to realize packaging and storage, in addition, the tip of the probe is completely wrapped by the asphalt by using an optical microscope test, and if the tip of the probe is not completely wrapped, the packaging needs to be repeated;

d. screwing the rear end (2) of the pen tube to the front end of the pen tube in a matching manner; the pen tube cap (3) is screwed on the front end of the pen tube in a matching way, and the pen tube type portable probe is prepared (4);

the specific size of the front end (1) of the pen tube is as follows: the thickness of the shell at the front end of the pen tube is 1.1mm, the length of the diameter-variable part at the front end of the pen tube is 4.6mm, the outer radius of the front section of the pen tube is 3.1mm, and the inner wall of the front section of the pen tube is provided with M5-sized internal threads which can be connected with M5 external threads at the rear end (2) of the pen tube;

the rear end (2) of the pen tube has the specific size: the thickness of the shell at the rear end of the pen tube is 0.8mm, and M5 external threads are processed on the outer wall of the shell and can be matched with M5 internal threads at the front end (1) of the pen tube;

the specific size of the pen tube cap part is as follows: the thickness of the shell is 0.8mm, and the function is to protect the tip of the electrode from being deformed due to impact when the electrode is not used;

e. the method for opening the probe tip comprises the following steps: under the conditions that the voltage is 2-4V and the current density is 10-11.0A, a constant potential rectifier is used for burning the resistance wire, the needle point of the assembled pen-type probe is upward, an XYZ level meter controls the probe to move from bottom to top and to be close to the red burning resistance wire, burnt smoke appears at the needle point or burnt smell is smelled, namely the opening of the needle point is successful, the needle point is removed, and the constant potential rectifier is closed.

2. The method for preparing a pen-type portable probe according to claim 1, wherein the pen-type portable probe tip is prepared by etching a tungsten wire electrode in an alkaline solution, and mainly cooperating with an optical camera to capture the necking process of the tungsten wire electrode at the liquid level of the alkaline solution, and by observing the bubble generation speed and size at the interface, the progress of necking, namely the decrease of bubbles and the decrease of speed, is judged, which means that the etching is about to be finished, and at the finishing moment, the interface needs to be quickly pulled away, and a potentiostat is closed to prevent the damage of the probe tip.