CN107684416B - Glass micro-tube electrode based on liquid metal and preparation method thereof - Google Patents
Glass micro-tube electrode based on liquid metal and preparation method thereof Download PDFInfo
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- CN107684416B CN107684416B CN201610633088.XA CN201610633088A CN107684416B CN 107684416 B CN107684416 B CN 107684416B CN 201610633088 A CN201610633088 A CN 201610633088A CN 107684416 B CN107684416 B CN 107684416B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/24—Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/68—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient
- A61B5/6846—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be brought in contact with an internal body part, i.e. invasive
- A61B5/6847—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be brought in contact with an internal body part, i.e. invasive mounted on an invasive device
- A61B5/6852—Catheters
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
- A61N1/00—Electrotherapy; Circuits therefor
- A61N1/02—Details
- A61N1/04—Electrodes
- A61N1/05—Electrodes for implantation or insertion into the body, e.g. heart electrode
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
- A61B2562/02—Details of sensors specially adapted for in-vivo measurements
- A61B2562/0209—Special features of electrodes classified in A61B5/24, A61B5/25, A61B5/283, A61B5/291, A61B5/296, A61B5/053
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Abstract
The invention provides a glass micro-tube electrode based on liquid metal and a preparation method thereof, wherein the glass micro-tube electrode comprises an ultra-thin glass tube (1), liquid metal (2), packaging adhesive (3) and a connecting wire (4); the superfine glass tube (1) is conical, the inner diameter of the tip of the superfine glass tube is 1-5 microns, and the inner diameter of the other end of the superfine glass tube is 1-2 mm; liquid metal (2) is poured into the superfine glass tube (1); filling packaging glue (3) at the thicker end of the superfine glass tube (1); a connecting wire (4) is inserted into the packaging adhesive (3), one end of the connecting wire is contacted with the liquid metal, and the other end of the connecting wire extends out of the superfine glass tube and is connected with a detection instrument. Compared with the traditional glass micro-electrode, the glass micro-tube electrode provided by the invention has a smoother electrode surface and lower electrical impedance characteristic, and is stable in electrochemical property. The preparation process is simpler, the cost is lower, and the controllability is better. Furthermore, a plurality of capillary glass tubes can be combined into a micro-tube electrode array, so that physiological signal detection and electrical stimulation of a plurality of sites are realized.
Description
Technical Field
The invention relates to the field of medical materials, in particular to a glass micro-tube electrode based on liquid metal and a preparation method thereof.
Background
The microelectrode is a common medical sensing device and has wide application in the fields of bioelectrophysiology research, biomedical detection, biomedical electrical stimulation and the like. The micro-electrode has a micro-nano-scale fine structure and can measure the potential of a single cell or a deep tissue. The commonly used microelectrodes include metal microelectrodes and glass microelectrodes, which differ in their electrical properties and their manufacturing processes.
The metal microelectrode is generally a high-strength metal fine needle, the surface of the metal microelectrode is subjected to insulation treatment by using an organic material, but the geometric shape of the microelectrode is difficult to keep consistent with the insulation state, and the tip of the electrode plated with an insulation layer needs to be cut by a blade manually in the traditional manufacturing process, so that the surface of the electrode is not smooth, and the measurement result has errors. The glass microelectrode is drawn by a hard capillary tube, and when the glass microelectrode is used for measuring the resting potential and the action potential in cells, the tip of the glass microelectrode needs to be less than 0.5 mu m; when the probe is used for measuring the potential of the non-active point in the extracellular active area, the tip of the probe can be 1-5 μm. Usually, electrolyte is poured into the tip of the glass microelectrode to serve as an electrode material, but insulating paint or epoxy resin is needed to be used for sealing, and the leakage phenomenon of the epoxy resin in the solution can cause the occurrence of noise signals in the detection process, so that the detection sensitivity is greatly reduced. In some glass microelectrodes, superfine metal wires are inserted to replace electrolyte as electrode materials, but the processing technology of the superfine metal wires is high in requirement, irregular metal section shapes of electrode tips can also cause errors of measurement results, and the cost of noble metal electrode wires is high.
Typical metallic materials tend to have very high melting points, while some metallic materials, such as mercury, remain in liquid form at ambient temperatures. Similar to mercury, some gallium-based alloys, indium-based alloys, and bismuth-based alloys have lower melting points and wider liquid temperature ranges, and are chemically stable. In recent years, research on gallium-indium alloy is widely carried out, and related experiments show that metal gallium cannot be dissolved in water, is not easy to be absorbed through skin, and has low cytotoxicity to cells. Liquid metal has the electrical conductivity, thermal conductivity and radiation imaging capabilities of metal as well as the fluidity and compliance of liquids. These characteristics make liquid metal as electrode material for preparing glass micro tube electrode.
Disclosure of Invention
The invention aims to provide a glass micro-tube electrode based on liquid metal and a preparation method thereof.
The invention also aims to provide a glass microtube electrode array prepared from the glass microtube electrode.
In order to realize the purpose of the invention, the glass micro-tube electrode based on the liquid metal comprises an ultra-thin glass tube 1, the liquid metal 2, packaging glue 3 and a connecting wire 4; the superfine glass tube 1 is conical, the inner diameter of the tip end of the superfine glass tube is 1-5 microns, and the inner diameter of the other end of the superfine glass tube is 1-2 mm; liquid metal 2 is poured into the superfine glass tube 1; filling a packaging adhesive 3 at the thicker end of the superfine glass tube 1; a connecting wire 4 is inserted into the packaging adhesive 3, one end of the connecting wire is contacted with the liquid metal, and the other end of the connecting wire extends out of the superfine glass tube and is used for being connected with a detection instrument.
The liquid metal is a metal or alloy material which keeps liquid state at normal temperature, and comprises gallium-based alloy, indium-based alloy, bismuth-based alloy and the like; or the liquid metal is an alloy material with a modified metal surface, and the modification comprises oxidation or electroplating treatment.
Liquid metal alloys with different melting points and conductive properties, such as gallium-indium alloy, gallium-indium-tin alloy or bismuth-indium-tin alloy, can be obtained by different content ratios.
Preferably, the liquid metal is formed from gallium and indium in a ratio of 75.5: 24.5, and the melting point of the gallium-indium alloy is 10.35 ℃.
The packaging adhesive used in the present invention includes epoxy resin or silicone rubber, etc.
The invention also provides a preparation method of the glass micro-tube electrode, which comprises the following steps:
1) taking a capillary glass tube with the inner diameter of 1-2mm, and injecting liquid metal into the capillary glass tube;
2) inserting two connecting wires into two ends of the capillary glass tube respectively, contacting with liquid metal in the tube, and then coating packaging glue on the two ends of the capillary glass tube to seal the capillary glass tube;
3) drawing the packaged capillary glass tube into an ultra-fine glass tube with the middle part of the tube with the inner diameter of 1-5 microns by a heating melting method;
4) cutting the ultra-thin glass tube drawn in the step 3) from the middle to obtain the ultra-thin glass tube.
Preferably, step 3) draws the packaged capillary glass tube with a micro tube drawing machine at 750 ℃.
Ultra-fine glass tubes made by other methods are also within the scope of the present invention.
The invention further provides a glass micro-tube electrode array prepared from the glass micro-tube electrode.
The glass micro-tube electrode array comprises glass micro-tube electrodes 5, electrode connecting circuits 6 and a substrate 7 with a concave hole array, wherein the glass micro-tube electrodes 5 are fixed in the concave holes on the substrate, the electrode connecting circuits 6 are formed by depositing metal leads corresponding to the concave holes on the substrate 7 through the surfaces, one end of each metal lead and a connecting lead extending out from the glass micro-tube electrodes 5 are welded at the bottoms of the concave holes together, and the other end of each metal lead extends to the edge of the substrate to form a metal connecting sheet for connecting with a detection instrument.
Preferably, the substrate 7 is a silicon plate with a thickness of 1-2 mm.
The thicker end of the glass micro-tube electrode 5, which is not an electrode end, can be fixed in each concave hole on the substrate by using epoxy resin or silicon rubber, and the inner diameter of each concave hole is 1-2 mm.
The invention provides a design scheme of a glass micro-tube electrode based on liquid metal for the first time, which is characterized in that the liquid metal is poured into a capillary glass tube by utilizing the liquidity and the conductivity of the liquid metal, then the capillary glass tube is drawn into an ultra-fine glass tube, and the liquid metal in the tube is used as an electrode material. Compared with the traditional glass micro-electrode, the glass micro-tube electrode provided by the invention has a smoother electrode surface and lower electrical impedance characteristic, and is stable in electrochemical property. The preparation process is simpler, the cost is lower, and the controllability is better. Furthermore, a plurality of capillary glass tubes can be combined into a micro-tube electrode array, so that physiological signal detection and electrical stimulation of a plurality of sites are realized.
Drawings
Fig. 1 shows a glass microtube electrode based on liquid metal prepared in example 1 of the present invention.
Fig. 2 is a process flow chart of the preparation of the glass microtube electrode in example 1 of the present invention.
Fig. 3 shows an array of liquid metal based glass micro tube electrodes prepared in example 2 of the present invention.
In the figure, 1: an ultra-fine glass tube; 2: a liquid metal; 3: packaging glue; 4: connecting a lead; 5: a glass microtube electrode; 6: an electrode connection circuit; 7: a substrate; 3 a: a capillary glass tube; 3 b: a liquid metal; 3 c: connecting a lead; 3 d: packaging glue; 3 e: drawing an ultra-fine glass tube.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are commercially available products.
The liquid metal used in the following examples was prepared from gallium and indium at 75.5: 24.5, the melting point of the gallium indium alloy is 10.35 ℃. Experiments show that the gallium-indium alloy can not be dissolved in water, is not easy to be absorbed by skin and is safe to use. The packaging adhesive comprises epoxy resin or silicon rubber.
In the description of the present invention, unless otherwise specified, the terms "upper", "lower", and the like, indicate orientations or state relationships only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Example 1 liquid metal based glass microtube electrode and method for making same
The glass micro-tube electrode (fig. 1) provided by the embodiment comprises a superfine glass tube 1, liquid metal 2, packaging adhesive 3 and a connecting wire 4; the superfine glass tube 1 is conical, the inner diameter of the tip end of the superfine glass tube is 1-5 microns, and the inner diameter of the other end of the superfine glass tube is 1-2 mm; liquid metal 2 is poured into the superfine glass tube 1; filling packaging glue 3 at the thicker end (non-electrode end) of the superfine glass tube 1; a connecting wire 4 is inserted into the packaging adhesive 3, one end of the connecting wire is contacted with the liquid metal, and the other end of the connecting wire extends out of the superfine glass tube and is used for being connected with a detection instrument.
The preparation method comprises the following steps:
1) taking a capillary glass tube 3a with the inner diameter of 1-2mm, and injecting liquid metal 3b into the capillary glass tube 3 a;
2) inserting two connecting wires 3c into two ends of a capillary glass tube 3a respectively, contacting with liquid metal 3b in the tube, and then coating packaging glue 3d on two ends of the capillary glass tube 3a to seal the capillary glass tube;
3) drawing the packaged capillary glass tube 3a into an ultra-fine glass tube 3e with the middle part having an inner diameter of 1-5 microns by a micro-tube drawing instrument at 750 ℃ by adopting a heating melting method;
4) cutting off the superfine glass tube 3e drawn in the step 3) from the middle to obtain the glass micro-tube electrode.
The schematic processing process of the liquid metal glass micropipe electrode is shown in fig. 2.
Through detection, compared with the traditional glass micro-electrode, the glass micro-tube electrode prepared in the embodiment has a smoother electrode surface and lower electrical impedance characteristic, the electrochemical property is stable, and the variation amplitude is controlled within 5%.
Example 2 liquid metal based glass microtube electrode array
The glass micro-tube electrode array (fig. 3) based on liquid metal provided in this embodiment includes the glass micro-tube electrode 5 prepared in embodiment 1, an electrode connection circuit 6, and a substrate 7 with a concave hole array, where the glass micro-tube electrode 5 is fixed in each concave hole on the substrate, the electrode connection circuit 6 is formed by depositing a metal wire corresponding to each concave hole on the substrate 7 through a surface, one end of each metal wire and a connection wire extending from the glass micro-tube electrode 5 are welded together at the bottom of the concave hole, and the other end of the metal wire extends to the edge of the substrate to form a metal connection sheet for connecting with a detection instrument.
Generally, a silicon plate is used as a substrate, the length is 2cm, the width is 2cm, the thickness is about 1mm, and a 4 × 5 concave hole array is distributed on the surface of the silicon plate. The inner diameter of the concave hole is 1-2mm, which is equivalent to the inner diameter of the thicker end (non-electrode end) of the glass micro-tube electrode 5, and the array interval is 2 mm. In this embodiment, the electrode connection circuit 6 is composed of 20 metal wires, and the metal connection pieces are uniformly distributed on the edge of the silicon plate. Fixing the non-electrode end of the glass micro-tube electrode 5 in each concave hole on the substrate by using epoxy resin or silicon rubber,
although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (1)
1. The glass micro-tube electrode array is characterized by comprising glass micro-tube electrodes (5), an electrode connecting circuit (6) and a substrate (7) with a concave hole array, wherein the glass micro-tube electrodes (5) are fixed in the concave holes on the substrate, the electrode connecting circuit (6) is formed by depositing metal leads corresponding to the concave holes on the substrate (7) through the surface, one end of each metal lead and a connecting lead extending out of the glass micro-tube electrodes (5) are welded at the bottoms of the concave holes together, and the other end of each metal lead extends to the edge of the substrate to form a metal connecting sheet for connecting with a detection instrument;
the glass micro-tube electrode comprises a super-fine glass tube (1), liquid metal (2), packaging glue (3) and a connecting wire (4); the superfine glass tube (1) is conical, the inner diameter of the tip of the superfine glass tube is 1-5 microns, and the inner diameter of the other end of the superfine glass tube is 1-2 mm; liquid metal (2) is poured into the superfine glass tube (1); filling a packaging adhesive (3) at the thicker end of the superfine glass tube (1); a connecting wire (4) is inserted into the packaging adhesive (3), one end of the connecting wire is contacted with the liquid metal, and the other end of the connecting wire extends out of the superfine glass tube and is used for being connected with a detection instrument;
the liquid metal is prepared from gallium and indium according to the weight ratio of 75.5: 24.5, wherein the melting point of the gallium-indium alloy is 10.35 ℃;
the packaging adhesive comprises epoxy resin or silicon rubber;
the substrate (7) is a silicon plate with the thickness of 1-2 mm;
and the thicker end of the glass micro-tube electrode (5) is fixed in each concave hole on the substrate by using epoxy resin or silicon rubber, and the inner diameter of each concave hole is 1-2 mm.
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| EP3527254B1 (en) * | 2018-02-14 | 2020-08-05 | Dyconex AG | Implantable multielectrode array |
| CN108896633B (en) * | 2018-04-20 | 2020-06-30 | 中国科学院生态环境研究中心 | High-precision pH microelectrode and manufacturing method thereof |
| CN110010403A (en) * | 2019-04-10 | 2019-07-12 | 常州大学 | A kind of glass tilt switch and preparation method based on gallium base liquid metal |
| CN111661814B (en) * | 2020-05-26 | 2022-09-23 | 上海交通大学 | Multifunctional integrated ultramicro/nano electrode and preparation method thereof |
| CN111849768B (en) * | 2020-07-14 | 2022-07-19 | 苏州大学 | Egg cell multi-efficiency accurate electrical stimulation device and method |
| CN112034741B (en) * | 2020-08-26 | 2021-08-10 | 中国科学院重庆绿色智能技术研究院 | Liquid-phase micro-nano processing method and equipment |
| CN113267649B (en) * | 2021-04-29 | 2023-03-17 | 大连海事大学 | Preparation method of long-arm probe of atomic force microscope |
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| CN105709331A (en) * | 2016-01-19 | 2016-06-29 | 云南科威液态金属谷研发有限公司 | Medical electrode for physical therapy |
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| CN201369392Y (en) * | 2009-01-24 | 2009-12-23 | 番禺得意精密电子工业有限公司 | Conductive component and electric connector with same |
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