CN110448305A - The production method of micro- needle electrode of glucose sensor and micro- needle electrode - Google Patents
The production method of micro- needle electrode of glucose sensor and micro- needle electrode Download PDFInfo
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- CN110448305A CN110448305A CN201910648843.5A CN201910648843A CN110448305A CN 110448305 A CN110448305 A CN 110448305A CN 201910648843 A CN201910648843 A CN 201910648843A CN 110448305 A CN110448305 A CN 110448305A
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/145—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue
- A61B5/14525—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue using microdialysis
- A61B5/14528—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue using microdialysis invasively
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- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/145—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue
- A61B5/14532—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue for measuring glucose, e.g. by tissue impedance measurement
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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
- A61B5/145—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue
- A61B5/1468—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue using chemical or electrochemical methods, e.g. by polarographic means
- A61B5/1473—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue using chemical or electrochemical methods, e.g. by polarographic means invasive, e.g. introduced into the body by a catheter
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Abstract
The production method of micro- needle electrode of glucose sensor and micro- needle electrode, the production method of micro- needle electrode of the glucose sensor include the following steps: to provide substrate；Current collector layers are formed by depositing operation on the substrate；Medium layer is formed by depositing operation in the current collector layers；Enzyme layer is formed in medium layer；The first permeable membrane is formed, in enzyme layer to form working electrode；Reference electrode is provided, or to electrode and reference electrode, by the reference electrode or described electrode and reference electrode is fixed on the working electrode.By the production method, the adhesive force between each layer can be preferably improved, improves sensitivity and stability.
Description
Technical field
The present invention relates to field of sensor production, the production side of micro- needle electrode of especially a kind of glucose sensor
Micro- needle electrode of method and the glucose sensor formed using this method.
Background technique
Glucose sensor is the core equipment in blood glucose monitoring system.According to detection mode, common glucose sensing
Device can be divided into three classes: refer to blood formula, non-invasive (including interstitial fluid glucose sensor and glucose optical sensor) and micro-
Pin type.Wherein the deep enough human body of micropin formula energy measures, and therefore, the result of measurement is more accurate.
It is that each active constituent is passed through into substep brushing, spin coating, dip-coating, spraying etc. in existing micropin formula production method
Mode is formed on substrate, after dry, completes preparation.Such mode step is more and rough, and due in drying process
Surface tension effects, the active material particle formed in this way is larger, does not have stronger interaction between substrate, easily leads into
It is unevenly distributed, sticking not enough between ingredient and substrate and between each ingredient, is easy to fall off from substrate.To influence
The controllable integration system of sensor is standby, sensing sensitivity and stability.
Summary of the invention
In view of this, the present invention provides the production method of micro- needle electrode of glucose sensor and using this method
Micro- needle electrode of the glucose sensor of formation can preferably be improved sticking between each layer by the production method
Power improves sensitivity and stability.
The present invention provides a kind of production method of micro- needle electrode of glucose sensor, this method includes following step
It is rapid:
Substrate is provided；
Current collector layers are formed by depositing operation on the substrate side；
Medium layer is formed by depositing operation in the current collector layers；
Enzyme layer is formed in medium layer；
The first permeable membrane is formed, in enzyme layer to form working electrode；
Reference electrode is provided, or to electrode and reference electrode, by the reference electrode or described to electrode and reference electrode
It is fixed on the other side that substrate and working electrode are supported or opposed.
Further, the depositing operation includes e-beam evaporation, magnetron sputtering method or thermal evaporation.
Further, the substrate is to be formed by inorganic non-metallic ceramics, silica glass or organic polymer material
Substrate.
Further, the organic polymer includes polytetrafluoroethylene (PTFE), polyethylene, polyvinyl chloride, acrylonitrile-butadiene-
One of styrol copolymer, polymethyl methacrylate, polycarbonate, polyimides or a variety of combinations.
Further, the substrate includes matrix part and the needle body part that is set on matrix part, and the current collector layers are simultaneously
It is formed in described matrix portion and needle body part, the medium layer is formed in the current collector layers of the needle body part, the enzyme layer shape
In the medium layer of needle body part described in Cheng Yu.
Further, the reference electrode is being prepared, or when to electrode and reference electrode, is first preparing electrode layer, then exist
The second permeable membrane is prepared on the electrode layer.
Further, the reference electrode is multiplexed with to electrode.
Further, the substrate includes needle body part, in the needle body part region, first permeable membrane, the enzyme layer,
The medium layer, the current collector layers are successively successively set to the side of the substrate, the electrode layer and second infiltration
Film layer is successively successively set to the other side of the substrate, and first permeable membrane and second permeable membrane are respectively the needle
The upper and lower surface in body portion.
Further, the substrate includes matrix part and the needle body part that is set in described matrix portion, in the needle body part
Region, the enzyme layer, the medium layer, the current collector layers are successively successively set on the substrate, first permeable membrane
It is coated on outside the enzyme layer, the medium layer and the current collector layers, it is described to electrode and reference electrode winding in a spiral form
In on the working electrode, second permeable membrane is coated on outside the electrode layer.
The present invention also provides a kind of micro- needle electrode of glucose sensor, the micropin formulas of the glucose sensor
Electrode is made using the production method of micro- needle electrode of above-mentioned glucose sensor.
In conclusion in the present invention, make that current collector layers are formed on substrate by depositing operation and medium layer passes through
Depositing operation is formed in current collector layers, and being uniformly distributed for current collector layers and medium layer may be implemented in this aspect；On the other hand
The interaction between each working lining can be increased, realize that the high intensity between each working lining is sticked, be conducive to electron-transport
It carries out, to improve the sensitivity and stability of sensor；In another aspect, passing through the current collector layers and medium of depositing operation formation
Layer, can no longer be dried and etc., the molding time is shortened, it can be after forming current collector layers and medium layer quickly
Carry out the processing procedure of other film layers.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And it can be implemented in accordance with the contents of the specification, and in order to allow above and other objects, features and advantages of the invention can
It is clearer and more comprehensible, it is special below to lift preferred embodiment, and cooperate attached drawing, detailed description are as follows.
Detailed description of the invention
Fig. 1 show the production method of micro- needle electrode of the glucose sensor of first embodiment of the invention offer
Flow diagram.
Fig. 2 show the production side of micro- needle electrode of the glucose sensor provided using first embodiment of the invention
The structural schematic diagram of micro- needle electrode of glucose sensor made of method production.
Fig. 3 show the structural schematic diagram of each layer of micropin formula electrode needle body part in Fig. 2.
Fig. 4 show the structural representation of micro- needle electrode of the glucose sensor of second embodiment of the invention offer
Figure.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing and preferred embodiment, detailed description are as follows.
The present invention provides the production method of micro- needle electrode of glucose sensor and the Portugals formed using this method
Micro- needle electrode of grape sugar sensor can preferably improve the adhesive force between each layer by the production method, improve spirit
Sensitivity and stability.
Fig. 1 show the production method of micro- needle electrode of the glucose sensor of first embodiment of the invention offer
Flow diagram, Fig. 2 show the system of micro- needle electrode of the glucose sensor provided using first embodiment of the invention
It is used as the structural schematic diagram of the micro- needle electrode for the glucose sensor that method is made, Fig. 3 show micropin formula electricity in Fig. 2
The structural schematic diagram of each layer of pole needle body part.As shown in Figure 1 to Figure 3, the glucose sensor that first embodiment of the invention provides is used
The production method of micro- needle electrode include the following steps:
S1: a substrate 10 is provided.
In the present embodiment, described basic 10 be sheet, and the material of substrate 10 can be by inorganic non-metallic ceramics, silica
The materials such as glass or organic polymer are formed.Organic polymer may include polytetrafluoroethylene (PTFE) (Poly tetra
Fluoroethylene, PTFE), polyethylene (polyethylene, PE), polyvinyl chloride (Polyvinyl chloride,
PVC), acrylonitrile-butadiene-styrene copolymer (Acrylonitrile butadiene Styrene copolymers,
ABS), polymethyl methacrylate (poly (methyl methacrylate, PMMA), polycarbonate (Polycarbonate,
PC), one of polyimides (Polyimide, PI) etc. or a variety of combinations.
As shown in Fig. 2, substrate 10 can be divided into matrix part 11 and the needle body part being connected with matrix part 111 112, using
When, needle body part 112 is for being inserted into the skin of human body, and in subsequent processing procedure, each layer of micro- needle electrode is all set in needle body
In portion 112, so that membrane layer can be pierced into human skin when in use.Matrix part 111 is equipped with the working electrode, to electricity
Pole, the corresponding pin of reference electrode, each electrode pass through the corresponding pin of conducting wire and are electrically connected.
More specifically, the width of needle body part 12 is no more than 0.3mm, of length no more than 6mm.
S2: current collector layers 20 are formed by depositing operation on the side of substrate 10；
Current collector layers 20 are formed by the metal materials such as gold, silver or conducting polymer, are preferably formed by golden material, thickness
For 50-300nm.Current collector layers 20 are laid in simultaneously on needle body part 12 and matrix part 11.
In the present embodiment, current collector layers 20 can be heavy by e-beam evaporation, magnetron sputtering method or thermal evaporation etc.
Product process deposits are on substrate 10.
Due in the present embodiment, introducing microelectronic processing technique, current collector layers 20 are formed by way of deposition
In on substrate 11.By taking e-beam evaporation as an example, under the cooperation of electromagnetic field, e-beam evaporation can accurately utilize high energy
Electron bombardment target, such as gold make target melt and then deposit on the substrate 11 with atomic form.Electron beam evaporation plating can plate out height
Being uniformly distributed for active material gold may be implemented in purity, high-precision gold thin film, this aspect；On the other hand can increase gold with
Interaction between substrate 11 realizes that high intensity between the two is sticked, and is conducive to the progress of electron-transport, to improve biography
The sensitivity and stability of sensor；In another aspect, the current collector layers 12 formed by depositing operation, can no longer be dried
Step shortens the molding time, can be carried out the production of other functional layers after the formation of current collector layers 12.
S3: medium layer 13 is formed by depositing operation in current collector layers 12.
Medium layer 13 is formed by the metals such as gold, silver, platinum or Prussian blue similar object, and preferably platinum product matter is formed, thickness
For 50-300nm.Medium layer 13 can be only formed in the current collector layers 12 of needle body part 112.
Identically as current collector layers 12, medium layer 13 again may be by e-beam evaporation, magnetron sputtering method or heat steaming
The modes such as hair method are deposited on substrate 11.
Similarly, after forming medium layer 13 by depositing operation, medium layer 13 can be distributed evenly in current collector layers 12
On, and tenaciously adhere in current collector layers 12.At the same time, medium layer 13 upon formation, equally no longer needs drying
Step can carry out the production of other functional layers directly over.
S4: enzyme layer 14 is formed in medium layer 13；
In the present embodiment, enzyme layer 14 can be by glucose oxidase or the nonwoven fabric from filaments of glucose dehydrogenase by solidification work
Skill is formed, it is preferable that enzyme layer 14 can be formed by the glucose oxidase layer 14 by crosslinking by curing process.
Due in the present embodiment, being therefore the current collector layers 12 and medium layer 13 formed by depositing operation are being formed
After medium layer 13, drying steps can be no longer waiting for, the solidification of enzyme layer 14 is carried out directly in medium layer 13.
S5: forming the first permeable membrane 15 in enzyme layer 14, to form working electrode 10；
In the present embodiment, other interfering substances and enzyme other than glucose can be isolated in human body in the first permeable membrane 15
Layer 14 contacts, and the first permeable membrane 15 can be for by polyvinyl acetate (polyvinyl acetate, PVA), polyethylene glycol
(Polyethylene glycol, PEG), polyacrylamide (polyacrylamide, PAM), acetate (acetate), polyoxy
Change ethylene (homopolymer, PEO), polyvinylpyrrolidone (polyvinyl pyrrolidone, PVP) and polytetrafluoroethylene (PTFE)
With made of one or more materials in perfluor -3,6- diepoxy -4- methyl -7- decene-sulfuric acid copolymer (Nafion)
One permeable membrane 15, preferably polytetrafluoroethylene (PTFE) and perfluor -3,6- diepoxy -4- methyl -7- decene-sulfuric acid copolymer
(Nafion)。
It further, can be by modes such as brushing, spin coating, dip-coating and sprayings, by when forming the first permeable membrane 15
One permeable membrane 15 is formed in enzyme layer 14.
At work, the glucose in blood passes through the first permeable membrane 15 and contacts with enzyme layer 14, in the catalysis of medium layer 13
Under, glucose reflects with enzyme layer 14, and the electric current of generation can draw needle body part by current collector layers, it is transferred in analytical unit,
For analyzing.
S6: another opposite with working electrode 10 of substrate 11 is fixed on by reference electrode 20, or to electrode and reference electrode 20
On side, to form micro- needle electrode of glucose sensor.
In this step, electrode layer 21 is first prepared, prepares the second permeable membrane 22, on electrode layer 21 then to form reference
Electrode 20, or to electrode and reference electrode 20.
It can be by the metal electrodes such as platinum, gold, silver, the materials shape such as graphite electrode or glass-carbon electrode to the electrode layer 21 of electrode
At.The electrode layer 21 of reference electrode 20 can be formed by silver/silver chloride electrode, calomel electrode etc..Electrode layer 21 is laid in simultaneously
In needle body part 112 and matrix part 111.
It more specifically, in the present embodiment, can be with when the micropin formula glucose detector is two electrode work system
Only reference electrode 20 is fixed on working electrode 10；When the micropin formula glucose detector is three electrode work system, need
Electrode and reference electrode 20 will be fixed on working electrode 10 simultaneously.Preferably, above-mentioned reference electrode 20 can be multiplexed
For to electrode, that is, being combined into one to electrode and reference electrode 20.
The material and preparation method of second permeable membrane 22 can be identical with the first permeable membrane 15, and details are not described herein.Second
Permeable membrane 22 is only arranged on the electrode layer 21 of needle body part 112.
Referring to figure 2. and Fig. 3, in the present embodiment, each functional layer is stacked, at this point, in S6 step, to electrode and
Electrode layer 21 in reference electrode 20 is fixed on the side on substrate 11 far from current collector layers 12, and the second permeable membrane 22 is arranged
In side of the electrode layer 21 far from substrate 11.At this point, first permeable membrane 15 and second seeps in 112 region of needle body part of substrate 11
Permeable membrane 22 is covered in each film layer from the outermost of each film layer respectively.
That is, 112 region of needle body part of substrate 11 is substantially in cuboid-type, in 112 region of needle body part of substrate 11 from
One permeable membrane, 15 to the second permeable membrane, 22 direction, the first permeable membrane 15, enzyme layer 14, medium layer 13, current collector layers 12, substrate 11,
Electrode layer 21 and the second permeable membrane 22 are set gradually.In 111 region of matrix part of substrate 11, current collector layers 12, substrate 11 and electricity
Pole layer 21 is set gradually.First permeable membrane 15, enzyme layer 14, medium layer 13 and current collector layers 12 are successively successively set to substrate 11
Side, electrode layer 21 and the second permeable membrane 22 are successively successively set to the other side of substrate 11.First permeable membrane 15 and second seeps
Upper and lower surface of the permeable membrane 22 respectively as needle body part 112.
In 112 region of needle body part of substrate 11, the width of micro- needle electrode of glucose sensor is no more than 0.3mm,
Of length no more than 6mm, thickness are no more than 0.2mm.
Compared to taper or cylindrical micro- needle electrode, micro- needle electrode of the glucose sensor being successively arranged can be with
What is be arranged is more small, is easier to penetrate skin, and combines between each layer stronger.Further improve glucose sensor use
Micro- needle electrode sensitivity and stability, while can also reduce pain/sense of discomfort and infection occur probability, reduce life
Object rejection.
Fig. 4 show the structural representation of micro- needle electrode of the glucose sensor of second embodiment of the invention offer
Figure, as shown in figure 4, the production method and structure of the micro- needle electrode for the glucose sensor that second embodiment of the invention provides
It is essentially identical with first embodiment, the difference is that, in the present embodiment, multiplexing can be with to electrode and reference electrode 20
It is wound in the form of screw electrode on working electrode 10 in 112 region of needle body part of substrate 11.
Under such configuration, in S5 step, the first permeable membrane 15 is not only needed to form in outside enzyme layer 14, also needs to coat
In outside each film layer of enzyme layer 14, medium layer 13 and the entire working electrode 10 of Streaming Media.At the same time, the second permeable membrane 22 is also required to
It is coated in the upper and lower surface of electrode layer 21.
In conclusion in the present invention, it is formed in current collector layers 12 on substrate 11 by depositing operation and medium layer
13 are formed in current collector layers 12 by depositing operation, and uniform point of current collector layers 12 and medium layer 13 may be implemented in this aspect
Cloth；On the other hand it can increase the interaction between each working lining, realize that the high intensity between each working lining is sticked, be conducive to
The progress of electron-transport, to improve the sensitivity and stability of sensor；In another aspect, the afflux formed by depositing operation
Body layer 12 and medium layer 13, can no longer be dried and etc., the molding time is shortened, current collector layers 12 can formed
And the processing procedure of other film layers is carried out after medium layer 13 quickly.
The present invention also provides a kind of micro- needle electrode of glucose sensor, the micropin formulas of the glucose sensor
Electrode is made using the production method of micro- needle electrode of above-mentioned glucose sensor, about the glucose sensor
Other technical characteristics of micro- needle electrode, refer to the prior art, details are not described herein.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
It is right according to the technical essence of the invention for the equivalent embodiment of equivalent variations, but without departing from the technical solutions of the present invention
Any simple modification, equivalent change and modification made by above embodiments, all of which are still within the scope of the technical scheme of the invention.
Claims (10)
1. a kind of production method of micro- needle electrode of glucose sensor, it is characterised in that: this method comprises the following steps:
Substrate is provided；
Current collector layers are formed by depositing operation on the substrate side；
Medium layer is formed by depositing operation in the current collector layers；
Enzyme layer is formed in medium layer；
The first permeable membrane is formed, in enzyme layer to form working electrode；
Reference electrode is provided, or to electrode and reference electrode, by the reference electrode or described electrode and reference electrode is fixed
In the other side that substrate and working electrode are supported or opposed.
2. the production method of micro- needle electrode of glucose sensor according to claim 1, it is characterised in that: described
Depositing operation includes e-beam evaporation, magnetron sputtering method or thermal evaporation.
3. the production method of micro- needle electrode of glucose sensor according to claim 1, it is characterised in that: described
Substrate is the substrate formed by inorganic non-metallic ceramics, silica glass or organic polymer material.
4. the production method of micro- needle electrode of glucose sensor according to claim 3, it is characterised in that: described
Organic polymer includes polytetrafluoroethylene (PTFE), polyethylene, polyvinyl chloride, acrylonitrile-butadiene-styrene copolymer, poly- methyl-prop
One of e pioic acid methyl ester, polycarbonate, polyimides or a variety of combinations.
5. the production method of micro- needle electrode of glucose sensor according to claim 2, it is characterised in that: described
Substrate includes matrix part and the needle body part that is set on matrix part, and the current collector layers are formed simultaneously in described matrix portion and needle body
In portion, the medium layer is formed in the current collector layers of the needle body part, and the enzyme layer is formed in the medium layer of the needle body part
On.
6. the production method of micro- needle electrode of glucose sensor according to claim 1, it is characterised in that: making
The standby reference electrode, or when to electrode and reference electrode, electrode layer is first prepared, then preparation second is seeped on the electrode layer
Permeable membrane.
7. the production method of the micro- needle electrode for the glucose sensor stated according to claim 6, it is characterised in that: the ginseng
It is multiplexed with than electrode to electrode.
8. the production method of the micro- needle electrode for the glucose sensor stated according to claim 7, it is characterised in that: the base
Plate includes needle body part, in the needle body part region, first permeable membrane, the enzyme layer, the medium layer, the current collector layers
It is successively successively set to the side of the substrate, the electrode layer and second osmotic membrane layer are successively successively set to the base
The other side of plate, first permeable membrane and second permeable membrane are respectively the upper and lower surface of the needle body part.
9. the production method of the micro- needle electrode for the glucose sensor stated according to claim 7, it is characterised in that: the base
Plate includes matrix part and the needle body part that is set in described matrix portion, in the needle body part region, the enzyme layer, the medium
Layer, the current collector layers are successively successively set on the substrate, and first permeable membrane is coated on the enzyme layer, the medium
It is described that electrode and reference electrode are set around in a spiral form on the working electrode outside layer and the current collector layers, described the
Two permeable membranes are coated on outside the electrode layer.
10. a kind of micro- needle electrode of glucose sensor, it is characterised in that: using any one of claim 1 to 9 institute
The production method of the micro- needle electrode for the glucose sensor stated is made.
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