CN117074471A - Sampling suction head and preparation method thereof - Google Patents
Sampling suction head and preparation method thereof Download PDFInfo
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- 238000005070 sampling Methods 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000007639 printing Methods 0.000 claims abstract description 108
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- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F30/00—Computer-aided design [CAD]
- G06F30/30—Circuit design
- G06F30/39—Circuit design at the physical level
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/12—Stencil printing; Silk-screen printing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/26—Printing on other surfaces than ordinary paper
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The application provides a preparation method of a sampling suction head and the sampling suction head, which comprises the steps of designing a model of a flexible sensing element through modeling software, and manufacturing a printing screen based on the model design; preparing a printing material of the flexible sensing element; using a full-automatic screen printer to design a printing material according to a model and printing a plurality of sensing electrode array layers on a flexible substrate layer by using a printing screen to form a plurality of flexible sensing elements; cutting a single flexible sensing element, winding the cut flexible sensing element into a cylindrical structure in a mode that a sensing electrode array layer is located at the inner side, sleeving a heat shrinkage tube at the outer side of the flexible sensing element for heating and heat shrinkage, and enabling the flexible sensing element to be attached to the inner wall of the heat shrinkage tube around the circumference of the heat shrinkage tube to assemble the sampling suction head. The sampling suction head has a simple structure, is convenient to operate and is easy to produce and manufacture on a large scale.
Description
Technical Field
The application belongs to the technical field of electrochemical sensing devices, and particularly relates to a preparation method of a sampling suction head and the sampling suction head.
Background
Electrochemical sensing has long been a leading edge technology in the chemical and biological sensor fields, playing an important role in the analytical chemistry field. As a key component of electrochemical sensors, electrodes are of great importance in determining the performance of the manufactured sensor.
Depending on the physical form of the electrochemical interface, electrodes can be divided into three categories: the first type is a conventional disk electrode, including a Glassy Carbon Electrode (GCE), a noble metal electrode (e.g., au, pt), etc. They have been widely used because of their good stability and reproducibility. The second type is a conventional planar screen-printed electrode (SPE), typically in the form of an integrated three electrode. The flat screen printed electrode SPE has the characteristics of easy use, simplicity and low cost, and is particularly suitable for daily use, such as point of care testing (POCT). The third category is homemade materials developed as self-supporting Working Electrodes (WEs), including 2D/3D carbon/metal based materials (e.g., graphene foam, gold/silver rods, etc.). Their inherently nano-functional surfaces can provide a larger sensing surface and good catalytic activity, thereby facilitating the construction of high performance electrochemical sensors.
While the above-described electrodes play a role in constructing various sensors, limitations and inherent drawbacks in the manufacturing process have prevented their use. In general, the congenital defects of the disk electrode are mainly caused by the inability to work alone, and thus the participation of separate counter and reference electrodes (CE and RE) is often required. This inevitably results in sensor redundancy, a relatively large volume of the device, a low degree of integration, and also increases the consumption of the sample solution. In addition, the redundant disc three-electrode sensing system also causes a system error caused by manual operation, and has negative influence on the accuracy and precision of the test result. In order to obtain a sensor with high sensitivity and a wide response range, most of the disk electrodes need to be decorated with functional materials, which compromises the simplicity of the sensor. In contrast, the conventional screen-printed electrode integrated three-electrode design simplifies sensor setup and miniaturizes measurement dimensions. However, the planar interface of the planar screen-printed electrode (SPE) in the related art makes the solid-liquid contact surface small, the liquid utilization rate low, and the use in an open environment. In addition, due to the small working area of conventional SPE electrodes, the limited sensing area of SPE still requires further material modification. However, for the self-supporting working electrode WE prepared by the researchers themselves, it is generally used less in the laboratory due to unavoidable individual differences, poor reproducibility and technical difficulties in mass production.
Therefore, it is necessary to provide an electrochemical sensing device that has a simple structure, is convenient to operate, has a high liquid utilization rate, and is easy to mass-produce.
Disclosure of Invention
The embodiment of the application aims to provide a preparation method of a sampling suction head and the sampling suction head, which are used for solving the technical problems of complex electrode structure and complex operation in the prior art.
In order to achieve the above purpose, the application adopts the following technical scheme:
in a first aspect, the application provides a method of preparing a sampling tip comprising the steps of:
designing a model of the flexible sensing element through modeling software, and manufacturing a printing screen based on the model design;
preparing a printing material of the flexible sensing element; wherein the printing material comprises a flexible substrate layer material and a printing paste;
using a full-automatic screen printer to design the printing material according to a model and printing a plurality of sensing electrode array layers on a flexible substrate layer by using the printing screen to form a plurality of flexible sensing elements;
cutting a single flexible sensing element, winding the cut flexible sensing element into a cylindrical structure in a mode that a sensing electrode array layer is located on the inner side, sleeving a heat shrinkage sleeve on the outer side of the flexible sensing element for heating and heat shrinkage, enabling the flexible sensing element to be attached to the inner wall of the heat shrinkage tube around the circumference of the heat shrinkage tube, and assembling the sampling suction head.
According to a preferred embodiment, the step of designing a model of the flexible sensor element by modeling software and creating a printing screen based on the model design further comprises:
the model based on the flexible sensing element is used for respectively manufacturing a frame wire screen plate, an electrode lead screen plate, an insulating layer screen plate, a working electrode screen plate, a counter electrode screen plate and a reference electrode screen plate,
the electrode lead screen plate is provided with printing holes for connecting electrode leads and lead wires, the insulating layer screen plate is provided with printing holes for insulating layers, the working electrode screen plate and the counter electrode screen plate are provided with printing holes for working electrodes and counter electrodes, and the reference electrode screen plate is provided with printing holes for reference electrodes.
According to a preferred embodiment, in the step of preparing the printed material of the flexible sensor element, the flexible substrate layer material comprises a polyimide film, and the printing paste comprises an insulating ink, a conductive silver paste, a silver chloride paste, a carbon paste ink, and a carbon nanotube paste.
According to a preferred embodiment, the polyimide film has a thickness of 0.05 to 0.075mm.
According to a preferred embodiment, the step of using a fully automatic screen printer to pattern the printing material and print a plurality of the sensing electrode array layers on the flexible substrate layer using the printing screen to form a plurality of flexible sensing elements further comprises:
printing insulating ink on the surface of the flexible substrate layer by utilizing the frame wire mesh plate to form the frame wire of each flexible sensing element;
printing conductive silver paste in the outer frame line of each flexible sensing element by utilizing the electrode lead screen plate so as to form electrode leads and lead connection points;
printing insulating ink above the electrode lead of each flexible sensing element by utilizing the insulating layer screen plate to form an insulating layer;
printing carbon paste ink and carbon nano tube paste on the insulating layer of each flexible sensing element by utilizing the working electrode and the counter electrode screen plate to form a working electrode and a counter electrode;
silver chloride paste is printed on the insulating layer of each flexible sensing element by using the reference electrode screen plate to form a reference electrode.
According to a preferred embodiment, the step of using a fully automatic screen printer to pattern the printing material and print a plurality of the sensing electrode array layers on the flexible substrate layer using the printing screen to form a plurality of flexible sensing elements further comprises:
and after each layer of printing is finished, putting the printing layers into an oven, and drying the printing layers for 15 to 20 minutes at the temperature of between 70 and 80 ℃.
According to a preferred embodiment, the cutting is performed on the single flexible sensing element, the cut flexible sensing element is wound into a cylindrical structure in a manner that the sensing electrode array layer is located at the inner side, a heat shrinkage sleeve is sleeved at the outer side of the flexible sensing element for heating and heat shrinkage, so that the flexible sensing element is attached to the inner wall of the heat shrinkage tube around the circumference of the heat shrinkage tube, and the step of assembling the sampling suction head further comprises:
winding the flexible sensing element; and positioning a sensing electrode array layer on the inner wall of the flexible sensing element;
nesting a mold inside the flexible sensing element;
nesting a heat shrink tube outside the flexible sensing element;
heating and shrinking; stretching the lower end of the heat shrinkage tube into a cone shape by means of stress;
the inner mold is removed.
According to a preferred embodiment, the heat shrinkage temperature is 110-120 ℃ and the heat shrinkage time is 40-80 s when heating and shrinking.
In a second aspect, the application also provides a sampling suction head, which is prepared by the preparation method, and comprises a sampling element and a flexible sensing element, wherein the flexible sensing element is wound into a cylindrical structure, a sensing electrode array layer is printed on the inner wall of the flexible sensing element of the cylindrical structure, the sampling element is sleeved on the outer side of the flexible sensing element, the flexible sensing element is attached to the inner wall of the sampling element around the circumference of the sampling element,
the flexible sensing element comprises a flexible substrate layer and a sensing electrode array layer, wherein the sensing electrode array layer is printed on one side of the flexible substrate layer.
According to a preferred embodiment, the sensing electrode array layer comprises an electrode lead, a lead connection point, an insulating layer and an electrode unit, wherein the electrode lead and the lead connection point are printed on the surface of the flexible substrate layer, one end of the electrode lead is connected with the lead connection point, the other end of the electrode lead is connected with the electrode unit, and the insulating layer covers the electrode lead; the electrode unit includes three working electrodes, a reference electrode and a counter electrode.
Based on the technical scheme, the preparation method of the sampling suction head and the sampling suction head have at least the following beneficial technical effects:
according to the preparation method, a full-automatic screen printer is used for printing a printing material according to the design of a model and printing a plurality of sensing electrode array layers on a flexible substrate layer by utilizing a printing screen to form a plurality of flexible sensing elements, so that a single flexible sensing element is cut, the flexible sensing element is wound into a cylinder shape, and the flexible sensing element and a heat shrinkage tube are heated and shrunk to assemble the sampling suction head. The manufacturing method of the application is convenient to operate and easy for mass production and manufacture.
The sampling suction head prepared by the preparation method provided by the application has a simple structure, is convenient for realizing large-scale manufacture, adopts the flexible sensing element with a cylindrical structure and the thermal shrinkage tube to heat and shrink the sampling suction head, the sensing electrode array layer of the flexible sensing element is positioned on the inner wall of the flexible sensing element and is attached to the inner wall of the thermal shrinkage tube, so that the sensing electrode array layer of the sampling suction head forms a tubular interface, the tubular interface and liquid drops have larger contact area, the liquid utilization rate can be obviously improved, and on the other hand, the area of an electrocatalytic interface can be regulated by changing the sample quantity, the effective sensing area is enlarged, and the sensitivity and the concentration of a sample can be flexibly regulated. And the tubular interface is favorable for forming a closed detection environment to reduce liquid volatilization, is not easy to be interfered by external environment, and further improves the accuracy of detection data.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments or the description of the prior art 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 flow chart of a method of manufacturing a sampling tip according to an embodiment of the present application;
FIG. 2 is a flow chart of a printing screen design in a method of manufacturing a sampling tip according to an embodiment of the present application;
FIG. 3 is a flow chart of printing of a plurality of flexible sensing elements in a method of manufacturing a sampling tip according to an embodiment of the present application;
FIG. 4 is a flow chart of printing a single flexible sensor element in a method of manufacturing a sampling tip according to an embodiment of the present application;
FIG. 5 is a flow chart of the preparation of a sampling tip according to an embodiment of the present application;
FIG. 6 is a schematic perspective view of a sampling tip according to an embodiment of the present application;
FIG. 7 is a schematic view of a flexible sensing element of a sampling tip according to an embodiment of the present application;
fig. 8 is a schematic structural diagram of an electrochemical sensing device according to an embodiment of the present application.
Wherein, in the figure: 11-outer frame line printing holes; 12-electrode lead printing holes; 13-insulating layer printing holes; 14-working electrode and counter electrode printing holes; 15-reference electrode printing holes; 100-a flexible sensing element; 101-a lead connection point; 102-electrode lead; 103-working electrode; 104-a counter electrode; 105-a reference electrode; 106-a flexible substrate layer; 107-an insulating layer; 108-outer frame lines; 200-sampling elements; 201-a support; 202-a sampling part; 300-suction means; 400-miniature electrochemical workstation; 500-a signal processing device; 600-die; 700-heat shrinkage tube.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
It will be understood that when an element is referred to as being "mounted" or "disposed" on another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
It is to be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are merely for convenience in describing and simplifying the description based on the orientation or positional relationship shown in the drawings, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus are not to be construed as limiting the application.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The technical scheme of the application is described in detail below with reference to the accompanying drawings of the specification.
Example 1
Referring to fig. 1, the application provides a method for preparing a sampling suction head, which comprises the following steps:
step S1: the model of the flexible sensor element 100 is designed by modeling software and a printing screen is fabricated based on the model design.
In this step, specifically, further includes: and respectively manufacturing a frame wire mesh plate, an electrode lead wire mesh plate, an insulating layer mesh plate, a working electrode, a counter electrode mesh plate and a reference electrode mesh plate based on the flexible sensing element model. Wherein, be equipped with the printing hole of every flexible sensing element 100 frame line on the frame line otter board, be equipped with the printing hole of electrode lead wire and lead wire tie point on the electrode lead wire otter board, be equipped with the printing hole of insulating layer on the insulating layer otter board, be equipped with the printing hole of working electrode and counter electrode on working electrode and the counter electrode otter board, be equipped with the printing hole of reference electrode on the reference electrode otter board.
In some embodiments, each printing screen is provided with printing apertures that can print a plurality of flexible sensor elements 100. For example: the wire screen is provided with outer frame wire printing holes 11 for printing outer frame wires of the plurality of flexible sensor elements 100. The electrode lead screen is provided with electrode lead printing holes 12 for printing electrode leads and lead connection points of a plurality of flexible sensing elements 100, the insulating layer screen is provided with insulating layer printing holes 13 for printing insulating layers of the plurality of flexible sensing elements 100, the working electrode and the counter electrode screen are provided with working electrode and counter electrode printing holes 14 for printing working electrodes and counter electrodes of the plurality of flexible sensing elements 100, and the reference electrode screen is provided with reference electrode printing holes 15 for printing reference electrodes of the plurality of flexible sensing elements 100. The printed aperture structure for each flexible sensor element can be seen in fig. 2.
It will be appreciated that a framing wire mesh sheet is used to print the framing wires 108 forming each flexible sensing element 100 on the flexible substrate layer 106. The electrode lead screen is used to print the electrode leads 102 and the lead connection points 101. The insulating layer screen is used for printing the insulating layer 107. The working electrode and the counter electrode screen are used to print the working electrode 103 and the counter electrode 104. The reference electrode screen is used to print the reference electrode 105.
Step S2: preparing a printed material of the flexible sensing element 100; wherein the printing material comprises a flexible substrate layer material and a printing paste.
In some embodiments, the flexible substrate layer 106 material comprises a polyimide film.
The flexible substrate layer 106 of the application adopts polyimide film, which can make the flexible degree of the flexible sensing element stronger, thereby improving the adhesion degree of the flexible sensing element and the heat shrinkage tube.
In some embodiments, the polyimide film has a thickness of 0.05 to 0.075mm. The polyimide film is too thin and is not easy to be in seamless joint with the heat shrinkage tube, and is not easy to be curled into a cylindrical structure if too thick, so the thickness of the polyimide film adopted by the application is 0.05-0.075 mm.
In some embodiments, the printing paste includes insulating ink, conductive silver paste, silver chloride paste, carbon paste ink, and carbon nanotube paste. The printing materials of the working electrode and the counter electrode are carbon paste ink and carbon nanotube paste (the mass percentage of the carbon nanotubes is 14 wt%) for printing, so that the electrochemical signals of the printed electrode are strong and the repeatability and stability of the printed electrode are excellent. The printing material of the reference electrode is silver chloride slurry.
Step S3: the plurality of flexible sensing elements 100 are formed by using a fully automatic screen printer to pattern the printed material and printing a plurality of sensing electrode array layers on the flexible substrate layer 106 using a printing screen.
Referring to fig. 2, 3 and 4, in step S3, the method specifically further includes:
step 1: printing insulating ink on the surface of the flexible substrate layer 106 by using a wire mesh plate to form outer frame wires 108 of each flexible sensing element 100;
step 2: printing conductive silver paste in the outer frame wire 108 of each flexible sensing element by using an electrode lead screen plate to form an electrode lead 102 and a lead connection point 101;
step 3: printing insulating ink over the electrode leads 102 of each flexible sensor element with an insulating layer screen to form an insulating layer 107;
step 4: printing carbon paste ink and carbon nanotube paste on exposed parts of the insulating layer 107 of each flexible sensing element by using a working electrode and a counter electrode screen plate to form a working electrode 103 and a counter electrode 104;
step 5: a reference electrode screen is used to print silver chloride paste on the exposed portion of the insulating layer 107 of each flexible sensor element to form a reference electrode 105.
And a plurality of sensing electrode array layers can be printed on the flexible substrate layer 106 in batches, the printing flow of each sensing electrode array layer is as shown in fig. 4, and the flexible sensing element 100 is cut along the outer frame line after printing, so that the manufacturing process is simple, and the mass production and manufacturing are easy.
In some embodiments, each layer is dried in an oven at 70-80 ℃ for 15-20 minutes after printing. The number of printing times per layer may be 2 to 3. The printing speed can be 180-230 mm/s, and in particular, the printing speed can be specifically adjusted according to the viscosity of the printing paste. The printing pressure can be 50N-70N, if the scraping pressure is too high, the screen plate is easy to damage, and if the pressure is too low, the printing effect is poor or the plate is stuck. Screen pitch: (-900 to-1300) mu m, the spacing is too small, the printing plate is easy to adhere or is blurred, and the screen plate is easy to print poorly and damage if the spacing is too large.
Step S4: cutting a single flexible sensing element 100, winding the cut flexible sensing element 100 into a cylindrical structure in a mode that a sensing electrode array layer is positioned on the inner side, sleeving a heat shrinkage tube 700 on the outer side of the flexible sensing element 100, and performing heating and heat shrinkage so that the flexible sensing element 100 is attached to the inner wall of the heat shrinkage tube 700 around the circumference of the heat shrinkage tube 700 to assemble the sampling suction head.
In some embodiments, referring specifically to fig. 5, fig. 5 shows a flowchart of preparation of a sampling tip in an electrochemical sensing device according to an embodiment of the present application; the preparation process of the sampling suction head further comprises the following steps:
step (1): winding the flexible sensing element 100 with the sensing electrode array layer positioned on the inner wall of the flexible sensing element 100;
step (2): the mold 600 is nested inside the flexible sensor element 100.
Step (3): heat shrink tubing 700 is nested outside of flexible sensing element 100.
Step (4): heating and shrinking; and the lower end of the heat shrinkage tube stretches into a cone shape by means of stress.
In the step, the thermal shrinkage temperature is 110-120 ℃, and the thermal shrinkage time is 40-80 s. If the temperature is too low, the heat shrinkage tube is not easy to be completely attached to the flexible sensing element, and if the temperature is too high, the heat shrinkage tube cannot be matched with the aperture of the suction device.
Step (5): the inner mold 600 is removed, thereby forming a sampling tip.
In some embodiments, the heat shrinkage tube 700 is heat shrunk to form the sampling element 200, where the sampling element 200 includes a supporting portion 201 at an upper end and a sampling portion 202 at a lower end, the supporting portion 201 is cylindrical, the sampling portion 202 is conical, the sampling element 200 is a portion for sampling a sample liquid to be tested, and the sample to be tested is sucked through the sampling portion 202 and allowed to enter and contact with a sensing electrode array of the flexible sensing element inside.
In another embodiment of the present application, the aperture of the supporting portion 201 is 5mm to 6mm, and the small mouth end of the sampling portion 202 is provided with a suction port, and the aperture of the suction port is 2mm to 3mm. The proper aperture can enable the sampling suction head to be tightly connected with the suction device of the electrochemical sensing device and the flexible sensing element 100 to form a closed system, so that volatilization of liquid is reduced, interference from external environment is not easy to occur, and accuracy of detection data is improved.
Example 2
Referring to fig. 6, fig. 6 is a schematic perspective view of a sampling tip according to an embodiment of the present application, and as shown in fig. 6, the sampling tip according to the present application is prepared by the preparation method described in embodiment 1.
The sampling tip comprises a sampling element 200 and a flexible sensing element 100. The flexible sensing element 100 is wound into a cylindrical structure, a sensing electrode array layer is printed on the inner wall of the flexible sensing element 100 with the cylindrical structure, the sampling element 200 is sleeved on the outer side of the flexible sensing element 100, and the flexible sensing element 100 is attached to the inner wall of the sampling element 200 around the circumference of the sampling element 200.
It will be appreciated that the term "outside of the flexible sensor element 100" as used herein refers to the side of the flexible sensor element that is remote from the sensor electrode array layer, and may also be understood as: the outer wall side of the flexible sensor element of the cylindrical structure. The term "attached" refers to that the outer side surface of the cylindrical structure of the flexible sensing element is attached to the inner wall of the sampling element.
The sampling suction head has a simple structure, is convenient to operate and is easy to produce and manufacture on a large scale. According to the sampling suction head, the flexible sensing element is wound to be in a cylindrical structure and is attached to the inner wall of the sampling element, so that a sensing electrode array layer formed by printing the inner wall of the flexible sensing element forms a tubular interface, a larger contact area is formed between the tubular interface and liquid drops, the liquid utilization rate can be remarkably improved, and on the other hand, the area of an electrocatalytic interface can be regulated by changing the sample quantity, the effective sensing area is enlarged, and the sensitivity and concentration of a sample can be flexibly regulated. And the tubular interface is favorable for forming a closed detection environment to reduce liquid volatilization, and is not easy to be interfered by external environment.
In another embodiment of the present application, referring to FIG. 7, a flexible sensing element 100 includes a flexible substrate layer 106 and a sensing electrode array layer, wherein the sensing electrode array layer is printed on one of the sides of the flexible substrate layer 106.
It will be appreciated that the sensing electrode array layer is formed by printing on one of the sides of the flexible substrate layer 106. One of the sides of the flexible substrate layer 106 described herein refers to one of the surfaces of the flexible substrate layer.
The sensing electrode array layer is printed on one side surface of the flexible substrate layer, so that the whole flexible sensing element has flexibility and is convenient to roll to form a cylindrical structure.
In another embodiment of the present application, referring to fig. 7, the sensing electrode array layer includes electrode leads 102, lead connection points 101, an insulating layer 107, and electrode units. The electrode lead 102 and the lead connection point 101 are printed on the surface of the flexible base layer 106, one end of the electrode lead 102 is connected to the lead connection point 101, the other end of the electrode lead 102 is connected to the electrode unit, and the insulating layer 107 covers the electrode lead 102.
In the sensing electrode array layer according to the embodiment of the application, the lead connection points 101 are in one-to-one correspondence with the electrode units, the lead connection points 101 are connected with the electrode units through the electrode leads 102, the lead connection points 101 are used for connecting conductive connection wires such as wires or conductive adhesive tapes, the insulating layer 107 covers the electrode leads, and the lead connection points 101 and the electrode units are exposed to the outside.
In another embodiment of the application, the electrode unit comprises a working electrode 103, a reference electrode 105 and a counter electrode 104, wherein the working electrode 103 comprises three and the three working electrodes 103 are arranged side by side. Because the inside of the sensing electrode array layer is printed with a plurality of working electrodes 103, the sensing electrode array layer can be used for simultaneous monitoring of a plurality of substances, namely, one-time sample solution is inhaled, and the simultaneous output of a plurality of index electrochemical signals can be realized, for example, the sensing electrode array layer can be used for simultaneous monitoring of a plurality of indexes of liver/kidney functions, simultaneous monitoring of antibiotic blood concentration and prognosis biochemical indexes and the like in the biomedical field.
In some embodiments, the electrode unit of the present application comprises three working electrodes 103, one reference electrode 105, and one counter electrode 104.
The printing materials of the working electrode and the counter electrode can be carbon paste and carbon nano tube paste, and the printing materials of the reference electrode can be silver chloride paste.
In another embodiment of the present application, the flexible substrate layer 106 is a polyimide film.
In another embodiment of the application, the flexible substrate layer 106 may be transparent.
In another embodiment of the present application, the flexible substrate layer 106 has a thickness of 0.05 to 0.075mm.
The thickness of the flexible substrate layer 106 in the embodiment of the application is 0.05-0.075 mm, so that the flexible sensing element 100 is easy to be closely attached to the sampling element 200, and meanwhile, the flexible sensing element 100 is easy to be wound into a cylindrical structure. While a flexible substrate layer 106 that is too thin is not easily seamlessly attached to the sampling element 200, too thick is not easily curled into a cylindrical configuration.
In another embodiment of the present application, referring to fig. 6, the sampling element 200 includes a supporting portion 201 and a sampling portion 202, wherein the supporting portion 201 is cylindrical, the sampling portion 202 is conical, a large opening end of the sampling portion 202 is connected to the supporting portion 201, a small opening end of the sampling portion 202 extends away from the supporting portion 201, and the flexible sensing element 100 is attached to an inner wall of the supporting portion 201 around a circumferential direction of the supporting portion.
The sampling element 200 is a portion for sampling a sample liquid to be measured, and sucks the sample to be measured through the sampling portion 202, and allows the sample liquid to enter and come into contact with an electrode unit of an internal flexible sensor element.
In another embodiment of the present application, the sampling element 200 is formed by heat shrinking a transparent heat shrink tube.
In another embodiment of the present application, the aperture of the supporting portion 201 is 5mm to 6mm, and the small mouth end of the sampling portion 202 is provided with a suction port, and the aperture of the suction port is 2mm to 3mm.
According to the embodiment of the application, the aperture of the supporting part of the sampling element can be tightly connected with the suction device and the sensing sampling element to form a closed system, so that the tightness is enhanced, the volatilization of liquid can be reduced, the interference of external environment is avoided, and the accuracy of detection data is improved.
Example 3
Referring to fig. 8, the present application further provides an electrochemical sensing apparatus, which includes a suction apparatus 300, a micro electrochemical workstation 400, a signal processing device 500, and the sampling tip described in the above embodiments 1 and 2. Wherein, sampling suction head detachable sets up in the lower extreme of suction device 300, and sampling suction head is connected with miniature electrochemical workstation 400 through electrically conductive connecting wire, and miniature electrochemical workstation 400 detachable sets up in the middle part of suction device 300, miniature electrochemical workstation 400 and signal processing device 500 communication connection. The conductive connecting wire can be a wire and a conductive adhesive tape and is used for realizing the electric connection between the electrode lead of the sampling suction head and external equipment.
The sampling tip comprises a sampling element 200 and a flexible sensing element 100. The flexible sensing element 100 is wound into a cylindrical structure, a sensing electrode array layer is printed on the inner wall of the flexible sensing element 100 with the cylindrical structure, the sampling element 200 is sleeved on the outer side of the flexible sensing element 100, and the flexible sensing element 100 is attached to the inner wall of the sampling element 200 around the circumference of the sampling element 200. The upper end of the sampling member 200 is detachably connected to the lower end of the suction device 300 and forms a sealed connection. One end of a conductive connection line, such as a conductive adhesive strip, is connected to the lead connection point 101 of the sensing electrode array layer, and the other end is connected to the micro electrochemical workstation 400.
In some embodiments, the aspiration device 300 may be a pipette or syringe. The signal processing device 500 may be a notebook computer, a tablet computer, or a smart phone. The communication connection may be a wired connection or a wireless connection. The wireless connection may be a bluetooth connection, an infrared connection, a cellular (cell phone) wireless connection, a wifi connection, or the like.
The complete electrochemical sensing device is assembled by assembling the suction device 300, the sampling tip, the micro electrochemical workstation 400, and the signal processing apparatus 500. The electrochemical sensing device can be a handheld integrated device, is simple in structure and convenient to operate, and can realize semi-automatic one-hand operation.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.
Claims (10)
1. A method for preparing a sampling tip, comprising the steps of:
designing a model of the flexible sensing element through modeling software, and manufacturing a printing screen based on the model design;
preparing a printing material of the flexible sensing element; wherein the printing material comprises a flexible substrate layer material and a printing paste;
using a full-automatic screen printer to design the printing material according to a model and printing a plurality of sensing electrode array layers on a flexible substrate layer by using the printing screen to form a plurality of flexible sensing elements;
cutting a single flexible sensing element, winding the cut flexible sensing element into a cylindrical structure in a mode that a sensing electrode array layer is located on the inner side, sleeving a heat shrinkage sleeve on the outer side of the flexible sensing element for heating and heat shrinkage, enabling the flexible sensing element to be attached to the inner wall of the heat shrinkage tube around the circumference of the heat shrinkage tube, and assembling the sampling suction head.
2. The method of manufacturing according to claim 1, wherein the step of designing a model of the flexible sensor element by modeling software and creating the printing screen based on the model design further comprises:
the model based on the flexible sensing element is used for respectively manufacturing a frame wire screen plate, an electrode lead screen plate, an insulating layer screen plate, a working electrode screen plate, a counter electrode screen plate and a reference electrode screen plate,
the electrode lead screen plate is provided with printing holes for connecting electrode leads and lead wires, the insulating layer screen plate is provided with printing holes for insulating layers, the working electrode screen plate and the counter electrode screen plate are provided with printing holes for working electrodes and counter electrodes, and the reference electrode screen plate is provided with printing holes for reference electrodes.
3. The method of claim 2, wherein the flexible substrate layer material comprises a polyimide film, and the printing paste comprises insulating ink, conductive silver paste, silver chloride paste, carbon paste ink, and carbon nanotube paste.
4. The method according to claim 3, wherein the polyimide film has a thickness of 0.05 to 0.075mm.
5. The method of manufacturing according to claim 4, wherein the step of using a fully automatic screen printer to print the printed material in a pattern and print a plurality of the sensor electrode array layers on the flexible substrate layer using the printing screen to form a plurality of flexible sensor elements further comprises:
printing insulating ink on the surface of the flexible substrate layer by utilizing the frame wire mesh plate to form the frame wire of each flexible sensing element;
printing conductive silver paste in the outer frame line of each flexible sensing element by utilizing the electrode lead screen plate so as to form electrode leads and lead connection points;
printing insulating ink above the electrode lead of each flexible sensing element by utilizing the insulating layer screen plate to form an insulating layer;
printing carbon paste ink and carbon nano tube paste on the insulating layer of each flexible sensing element by utilizing the working electrode and the counter electrode screen plate to form a working electrode and a counter electrode;
silver chloride paste is printed on the insulating layer of each flexible sensing element by using the reference electrode screen plate to form a reference electrode.
6. The method of manufacturing according to claim 5, wherein the step of using a fully automatic screen printer to print the printed material in a pattern and print a plurality of the sensor electrode array layers on the flexible substrate layer using the printing screen to form a plurality of flexible sensor elements further comprises:
and after each layer of printing is finished, putting the printing layers into an oven, and drying the printing layers for 15 to 20 minutes at the temperature of between 70 and 80 ℃.
7. The method according to claim 6, wherein the step of cutting the single flexible sensor element, winding the cut flexible sensor element in a cylindrical structure in such a manner that the sensor electrode array layer is located at the inner side, sleeving a heat shrink tube on the outer side of the flexible sensor element, and performing heat shrink so that the flexible sensor element is attached to the inner wall of the heat shrink tube around the circumference of the heat shrink tube, and assembling the sampling tip further comprises:
winding the flexible sensing element; and positioning a sensing electrode array layer on the inner wall of the flexible sensing element;
nesting a mold inside the flexible sensing element;
nesting a heat shrink tube outside the flexible sensing element;
heating and shrinking; stretching the lower end of the heat shrinkage tube into a cone shape by means of stress;
the inner mold is removed.
8. The method according to claim 7, wherein the heat shrinkage temperature is 110 to 120 ℃ and the heat shrinkage time is 40 to 80s when the heat shrinkage is performed.
9. A sampling suction head is prepared by the preparation method of any one of the claims 1 to 8, and comprises a sampling element and a flexible sensing element, wherein the flexible sensing element is wound into a cylindrical structure, a sensing electrode array layer is printed on the inner wall of the flexible sensing element of the cylindrical structure, the sampling element is sleeved on the outer side of the flexible sensing element, the flexible sensing element is attached to the inner wall of the sampling element around the circumference of the sampling element,
the flexible sensing element comprises a flexible substrate layer and a sensing electrode array layer, wherein the sensing electrode array layer is printed on one side of the flexible substrate layer.
10. The sampling tip of claim 9, wherein the sensing electrode array layer comprises an electrode lead, a lead connection point, an insulating layer and an electrode unit, wherein the electrode lead and the lead connection point are printed on the surface of the flexible substrate layer, one end of the electrode lead is connected to the lead connection point, the other end of the electrode lead is connected to the electrode unit, and the insulating layer covers the electrode lead; the electrode unit includes three working electrodes, a reference electrode and a counter electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310934351.9A CN117074471A (en) | 2023-07-27 | 2023-07-27 | Sampling suction head and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310934351.9A CN117074471A (en) | 2023-07-27 | 2023-07-27 | Sampling suction head and preparation method thereof |
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| CN117074471A true CN117074471A (en) | 2023-11-17 |
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| CN202310934351.9A Pending CN117074471A (en) | 2023-07-27 | 2023-07-27 | Sampling suction head and preparation method thereof |
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