CN107028615B - A kind of nanometer of flexible blood glucose microsensor and preparation method thereof - Google Patents
A kind of nanometer of flexible blood glucose microsensor and preparation method thereof Download PDFInfo
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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
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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
- A61B5/14532—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
Abstract
The invention discloses a kind of nanometer of flexible blood glucose microsensors and preparation method thereof, comprising: flexible substrates, epoxy resin layer, electrode structure, glucose oxidase film layer.Flexible substrates have good thermal adaptability (- 10-300 DEG C); electrode structure electric conductivity is excellent and antiacid caustic corrosion; glucose oxidase loads micro- channel, and (channel length is less than 10mm; 10 μm -500 μm of width) it is that nano material texture forms; flexibility is good; high sensitivity; linear dependence is presented in concentration of glucose (0.5-30mmol/L) range; with good invertibity and repeatability, hydrophilic wear-resistance thin film has the function of good ion through characteristic, strong water absorption character and protection sensitive layer.The present invention is nontoxic, and comfortably allergy, overall structure are not no more than less than 1cm contact human skin2, the real-time measurement in situ and analysis of blood of human body blood glucose value (0.5-30mmol/L) can be realized by current-responsive.
Description
Technical field
The invention belongs to the preparation field of electrochemical sensor, more particularly, to a kind of nanometer of flexible blood glucose sensor and its
Preparation method for realizing the real-time detection in situ and analysis to blood sugar for human body, and ensures that sensor is suitble to human body long periods of wear
With steady operation, it is able to achieve noninvasive or minimally invasive blood sugar monitoring, and meets a wide range of blood sugar monitoring of diabetes.
Background technique
Blood glucose is closely bound up with human health, long term hyperglycemia can cause various complication (such as uremia, limb necrosis,
Blindness etc.), and hypoglycemia will cause the consequences such as syncope, nervous inability, therefore blood sugar test is to human health important in inhibiting.
But traditional blood sugar test equipment volume is huge, and time-consuming, can not achieve accurate detection in real time, limit popularization in the family and
It uses.Huge market demand promotes scientific research personnel to research and develop a kind of high efficiency low cost, accurate portable blood sugar test equipment.
Existing non-optical type blood glucose sensor research is concentrated mainly on material modification, surface modification, combination electrode etc.,
Lee etc. are in paper " Flexible chitosan/carbon nanotubes aerogel, a robust matrix forin-
Situ growth and non-enzymatic biosensing applications " in mention carbon nanotube changed
Property, carbon nanotube and chitosan are assembled together as by sensitive materials using ice template method and prepare blood glucose biography on a flexible substrate
Sensor, but test process needs reference electrode, and test environmental requirement is alkaline solution.It is designed in terms of flexible sensor array,
Wei Gao etc. is in paper " Fully integrated wearable sensor arrays for multiplexed in
Situperspiration analysis " in mention integrated flexible sensor array design, by glucose, sodium potassium ion, pH value
It senses microdevice to merge in same flexible substrate, design technology is complicated, is unfavorable for realizing product mass production.It is comprehensive
It closes and considers existing generally existing a series of problems of glucose sensor: 1, low using effectiveness, complex structural designs, volume is big, difficult
To realize portable wearable function；2, technique is cumbersome, and device cost is excessively high；3, detection accuracy is lower, it is difficult to realize real-time in-situ
Monitoring；4, test environmental requirement is high；5, blood glucose response range is narrow, it is difficult to meet the prison of a wide range of blood sugar concentration of diabetes patient
It surveys.
Summary of the invention
For the existing above problem in actual use, the present invention devises a kind of nanometer of flexible blood glucose sensor and its system
By sensing the combination of micro- channel structure and hydrophilic wearing layer micro-analysis and fast slowdown monitoring may be implemented, and can expire in Preparation Method
The highly integrated requirement of the high efficiency low cost and small size of sufficient sensor, while by selecting and body-sensing nontoxic to skin comfortably good
Material prepare sensor, avoid that active layer and skin contact bring human body be uncomfortable and material damage.It is simple to test environment,
Change of blood sugar, simple process and low cost are analyzed in real time by current-responsive.
The present invention realizes above-mentioned technical purpose by following technological means.
A kind of preparation method of nanometer of flexible blood glucose sensor, which comprises the following steps:
Step 1: carbon nanotube film forming
Carbon nanotube is weighed according to 0.1-0.3mg/mL concentration, places it in the dense sulphur of volume ratio 3:1 mass fraction 95-98%
Acid removes supernatant, adjusts pH with 45-90min, centrifugation in the mixed acid of mass fraction 65-68% concentrated nitric acid, is stirred at 110 DEG C
To neutrality；Evaporating water at 30-60 DEG C of tiling, obtains carboxylic carbon nano-tube film；
Step 2: glucose sensing material preparation
It is made on film using magnetron sputtering in step 1 and prepares zinc oxide, target selects zinc oxide, and sputtering pressure is
1pa, target-substrate distance 5-10cm, sputtering power 50-300W use argon gas as protection gas, and substrate temperature is room temperature, sputters 20-
90min；Spraying 5-30 μ L glucose aoxidizes enzyme solutions on the material, and obtained sensing material is identical as micro- trench size；Portugal
Grape oxidase solution concentration is 1-40mg/mL；
Step 3: flexible substrate pretreatment
Flexible base material is handled in plasma reinforced chemical vapour deposition system: using hydrogen or oxygen reaction gas
20-120Pa, radio-frequency power 20-80W is pressed to handle flexible substrates at room temperature, locating it, less than 5 °, in advance with Liquid contact angle
It is coated on reason substrate with a thickness of 1-3 μm of epoxy resin；
Step 4: electrode and the micro- channel design of sensing
Electrode template is carried out by uv-exposure on flexible base material after treatment, between plating by electron beam evaporation plating
Every 1-10 μm of metal electrode, two end electrodes pass through pressure welding or elargol extraction electrode lead；Micro channel electrode layer is made, designs micro-
Ditch road length 1-6cm, 3-100 μm of width；
Step 5: the preparation of hydrophilic protective layer
It is 0.01-0.5 microns of vinylidene pvdf membrane in plasma reinforced chemical vapour deposition system by aperture
Reason: using hydrogen or oxygen reaction pressure 20-120Pa, radio-frequency power 20-80w handles at room temperature, contacts it with liquid
Angle selects hydrophilic protective layer less than 5 °, as ion, is mounted on above electrode and sensing material by epoxy resin, guard electrode
Material, sensing material guarantee that glucose molecule penetrates and precipitation simultaneously.
Further, it is controlled using the thicknesses of layers of magnetron sputtering or vapor deposition preparation in 100-250nm.
Further, electrode uses Ti/Au electrode, uv-exposure parameter: 110 DEG C of front baking 1-15min of AZ5214 glue, exposure
0.1-20s dries 1-5min after 120 DEG C, exposes 10-15s, and develop 0.1-5min；Electron beam evaporation plating parameter: vacuum degree 5 × 10- 6Mbar, Ti/Au thickness are respectively 10/100nm；
The preparation of glucose sensing material is with flexible substrate processing without sequencing.
Prepared blood glucose microsensor is used to be the linear response of 0.5-30mmol/L blood glucose to concentration.
A kind of nanometer of flexible blood glucose sensor and preparation method thereof, comprising: flexible substrates, epoxy resin layer, electrode structure,
Glucose oxidase loads micro- channel, ion penetrates hydrophilic wearing layer.Using bend resistance flexible polymer as substrate, using outstanding
Coating is coated with 1-3 μm of epoxy resin on polyimides (PI) substrate, the micro- channel structure of electrode is designed by template, by nanometer
Line textured material (carbon nanotube zinc oxide composite) and 1~40mg/mL glucolase are transferred in micro- channel as sensitivity
Layer realizes glucose quick adsorption with sensitive layer through hydrophilic wearing layer covering electrode with ion and avoids directly connecing with human body
Touching.
The flexible substrates are adhered to using nontoxic, bend resistance polymer such as PI etc. by processing hydrophily and surface
Property is good.
For the flexible substrates with a thickness of 50-200 μm, entire area is less than 1cm2。
The carbon nanotube zinc oxide composite film of the nano wire texture sensitivity layer material selection carboxylated surface processing is negative
Carry glucose oxidase film.
The micro- channel structure of electrode by template make, micro- channel length be less than 5mm, 3-100 μm of width.
The ion is porous polymer film, good hydrophilic property, glucose molecule transmitance height through hydrophilic wearing layer.
A kind of nanometer of flexible glucose sensor and preparation method thereof, includes the following steps:
(1) selection and surface treatment of flexible substrates: flexible base material select including PI etc., have good mechanics and
Thermal adaptability, the adhesion properties such as surface treatment enhancing electrode, sense channel and hydrophilic film.Flexible substrates 1 are made.
(2) the micro- channel structure design and fabrication of electrode: design structure size can be required with integrated according to device detection, to protect
It demonstrate,proves electrode excellent conductive performance and saves cost, be antiacid caustic corrosion by most there is structure design, select the chemistry such as Au, Pt steady
Qualitative good metal material.The micro- channel 2 of electrode is made.
(3) it is handled by strong acid (concentrated sulfuric acid, concentrated nitric acid), carboxylic group is introduced in carbon nanotube, enhance carbon nanotube
Hydrophily (contact angle is less than 5 °), is made carbon nanotube zinc-oxide film using magnetron sputtering, in carbon nano-tube film zinc oxide
Appropriate (1-40mg/mL) glucose oxidase is sprayed on composite material to import in micro- channel as sensitive materials.
(4) ion is handled and is encapsulated through hydrophilic wear-resistant coating, and by treated, hydrophilic wearing layer carries out surface mount, whole
Bulk area is no more than substrate sizes, and electrode is completely covered by with sensitive layer and avoids rubbing, and guarantees that electrode layer and sensitive material are long
Phase, which is used for multiple times, not to be fallen off.
Step (1) the surface treatment means include oxygen plasma treatment.
The micro- channel structure design method of step (2) electrode includes by mask plate, uv-exposure or electron beam exposure etc.
One or more of means design electrode structure.
The micro- channel structure preparation method of step (2) electrode can be one in the PVD means such as magnetron sputtering, electron beam evaporation plating
Kind or several production electrode layers, thickness of electrode control guarantee to reduce cost while electric conductivity in 100-150nm.
Step (4) ion is porous hydrophilic thin polymer film through hydrophilic wearing layer, and processing mode is oxygen plasma
Body processing, at 0.1-1 μm, thickness is not more than 0.1mm in aperture.
Beneficial effects of the present invention:
(1) a kind of nanometer provided by the invention flexible glucose microsensor and preparation method thereof, is designed by template
Nanometer texture senses micro- channel and ion selects the combination of hydrophilic wear-resistant coating, realizes that the small size of device is highly integrated, and sufficiently
Device active layer is protected, prevents from occurring peeling off because of Reusability and failing.Based on the biggish surface energy of carbon nano-tube film, use
Sputtering zinc oxide, while the method for spraying glucose oxidase prepares sensing material, it is linearly sensitive to glucose.
(2) a kind of nanometer of the present invention flexible glucose microsensor and preparation method thereof, by ion through parent
The use of water wearing layer avoids sensitive material and electrode material from contacting with the direct of measured body, is being applied to wearable biological Portugal
On grape sugar microsensor, material can be eliminated and reacted with the allergy that direct body contact arrives with discomfort, while protecting sensitive layer
Injury-free long-term precise operation.
(3) test philosophy of the present invention be based on resistance variations caused by current-responsive, test environmental requirement it is low, sensor for
It is 0.5-30mmol/L blood glucose linear response to concentration (human normal blood sugar concentration is 3.61-6.11mmol/L).
Detailed description of the invention
Fig. 1 is that (1 is flexible substrates to sensor structure figure, and 2 be electrode layer, and 3 be interdigital electrode position, that is, sensing material position
It sets, 4 be protective layer)
Fig. 2 is 3 enlarged diagrams in sensor structure figure, and mask plate makes the micro- channel structure schematic diagram of electrode
One response curve of Fig. 3 embodiment
Two response curve of Fig. 4 embodiment
Fig. 5 bend test influences sensitivities
Specific embodiment
Embodiment 1
It (1) is the pure concentrated nitric acid of analysis (mass fraction 68%) of 3:1 and the pure concentrated sulfuric acid (mass fraction of analysis with volume ratio
98%) mixed liquor introduces carboxylic group in single-walled carbon nanotube, 90min is stirred at 110 DEG C, in height as acidification liquid
It is centrifuged in fast centrifuge 9500rad/min, filters off supernatant, adjust carbon pipe pH to neutrality, evaporating water at 50 DEG C of tiling obtains
Single wall carboxyl-functional carbon pipe film.Using zinc oxide as target, sputtering pressure 1pa, target-substrate distance 7cm, sputtering power
Carbon nanotube zinc oxide composite is made, under room temperature with a thickness of 200nm in 50W, argon flow 40sccm.In the material
10 μ L (concentration 35mg/mL) glucose oxidases of upper spraying are used as sensing material, sensing material used and micro- trench size phase
Together；
It (2) will be with a thickness of 100 μm of flexibility PI substrates in oxygen plasma treatment, design parameter: vacuum degree 0.1Pa, work
Air pressure 20Pa, working gas O2, flow 20sccm, radio-frequency power 60w, room temperature handle 5min, contact flexible substrates with liquid
Angle is coated with 1 μm of epoxy resin of thickness less than 5 ° in pre-processed substrate；Then it is cut into 1 × 1cm2Flexibility base is made in square piece
Bottom imports made sensing material in 1.
(3) design such as Fig. 1 Lithographic template, carries out electrode template by uv-exposure on PI piece of processing, passes through electricity
Beamlet plate interval 3 μm of Ti/Au electrodes, uv-exposure parameter: 110 DEG C of front baking 3min of AZ5214 glue, expose 1s, 120 DEG C
After dry 2min, expose 20s, develop 1min.Electron beam evaporation plating parameter: vacuum degree 5 × 10-6Mbar, Ti/Au thickness are respectively 10/
100nm.Electrode thickness 50nm, two end electrodes pass through pressure welding or elargol extraction electrode lead.Designing micro- channel length is 1cm, wide
Micro channel electrode layer, thick 100nm is made in 10 μm of degree.The sensing material of steps for importing (1) preparation in channels.
(4) by 100 μm of thickness, the PVDF micropore wearing layer in 0.47 μm of aperture carries out surface oxygen plasma treatment and increases parent
It is aqueous, design parameter: vacuum degree 0.1Pa, operating air pressure 20Pa, working gas O2, flow 20sccm, radio-frequency power 60W, room temperature
Handle 5min.Then it is cut into 1 × 1cm2Piece is mounted on above electrode and sensing material, and ion is made through hydrophilic wear-resisting
Layer, makes it with Liquid contact angle less than 5 °；
(5) PI flexible substrate uses at being used in temperature lower than 300 DEG C, and senser element is sensitive to glucose solution, response
Curve is the glucose solution of 3mmol/L, 4mmol/L, 5mmol/L, 6mmol/L close to 3 μ L concentration linearly, are respectively taken respectively, is surveyed
Try its sensitive property.Test data is shown in Fig. 3, and the response time is less than 0.1s, and tests device recovery, and response rate is greater than 90%.
Embodiment 2
It (1) is the pure concentrated nitric acid of analysis (mass fraction 68%) of 3:1 and the pure concentrated sulfuric acid (mass fraction of analysis with volume ratio
98%) mixed liquor stirs 60min at 110 DEG C, is centrifuged in supercentrifuge 9500rad/min as acidification liquid, filters off
Supernatant adjusts carbon pipe pH to neutrality, and evaporating water at 50 DEG C of tiling obtains single wall carboxyl-functional carbon pipe film.Target choosing
With zinc oxide, sputtering pressure 1pa, target-substrate distance 5cm, sputtering power 80W, argon flow 30sccm, substrate temperature temperature is room
Temperature sputters 80min, and carbon nanotube zinc oxide composite is made with a thickness of 100nm and sprays 20 μ L (concentration on the material
25mg/mL) glucose oxidase is used as sensing material, and it is identical as micro- trench size that sensing material is made；
It (2) will be with a thickness of 100 μm of flexibility PI substrates in oxygen plasma treatment, design parameter: vacuum degree 0.1Pa, work
Air pressure 20Pa, working gas O2, flow 20sccm, radio-frequency power 60w, room temperature processing 5min.Contact flexible substrates with liquid
Angle is coated with 1 μm of epoxy resin of thickness less than 5 ° in pre-processed substrate；Then it is cut into 1 × 1cm2Flexibility base is made in square piece
Bottom.
(3) design such as Fig. 1 Lithographic template, carries out electrode template by uv-exposure on PI piece of processing, passes through electricity
Beamlet plate interval 6 μm of Ti/Au electrodes, uv-exposure parameter: 110 DEG C of front baking 5min of AZ5214 glue, expose 1s, 120 DEG C
After dry 2min, expose 20s, develop 1min.Electron beam evaporation plating parameter: vacuum degree 5 × 10-6Mbar, Ti/Au thickness are respectively 10/
100nm.Electrode thickness 150nm, two end electrodes pass through pressure welding or elargol extraction electrode lead.Designing micro- channel length is 2cm, wide
Micro channel electrode layer is made in 80 μm of degree.The sensing material of steps for importing (1) preparation in channels.
(4) by 100 μm of thickness, the PVDF micropore wearing layer in 0.47 μm of aperture carries out surface oxygen plasma treatment and increases parent
It is aqueous, design parameter: vacuum degree 0.1Pa, operating air pressure 20Pa, working gas O2, flow 20sccm, radio-frequency power 60W, room temperature
Handle 5min.Then it is cut into 1 × 1cm2Piece is mounted on above electrode and sensing material, and ion is made through hydrophilic wear-resisting
Layer, makes it with Liquid contact angle less than 5 °；
(5) PI substrate can be used below at 300 DEG C, and senser element is sensitive to glucose solution, and response curve is close linear,
Respectively taking 3 μ L concentration respectively is the glucose solution of 2mmol/L, 4mmol/L, 6mmol/L, 8mmol/L, tests its sensitive property.
Test data is shown in Fig. 4, and the response time is less than 0.1s, and tests device recovery, and response rate is greater than 90%.
Claims (5)
1. the preparation method of a kind of nanometer of flexible blood glucose microsensor, which comprises the following steps:
Step 1: carbon nanotube film forming
Weigh carbon nanotube according to 0.1-0.3mg/mL concentration, place it in the volume ratio 3:1 mass fraction 95-98% concentrated sulfuric acid with
In the mixed acid of mass fraction 65-68% concentrated nitric acid, 45-90min is stirred at 110 DEG C, centrifugation removes supernatant, adjusts pH into
Property；Evaporating water at 30-60 DEG C of tiling, obtains carboxylic carbon nano-tube film；
Step 2: glucose sensing material preparation
It is made on film using magnetron sputtering in step 1 and prepares zinc oxide, target selects zinc oxide, sputtering pressure 1pa, target
Cardinal distance 5-10cm, sputtering power 50-300W use argon gas as protection gas, and substrate temperature is room temperature, sputters 20-90min；At this
5-30 μ L glucose is sprayed on material and aoxidizes enzyme solutions, and obtained sensing material is identical as micro- trench size；Glucose oxidase
Solution concentration is 1-40mg/mL；
Step 3: flexible substrate pretreatment
Flexible base material is handled in plasma reinforced chemical vapour deposition system: using hydrogen or oxygen reaction pressure
20-120Pa, radio-frequency power 20-80W, handles flexible substrates at room temperature, is pre-processing it less than 5 °, with Liquid contact angle
It is coated on substrate with a thickness of 1-3 μm of epoxy resin；
Step 4: electrode and the micro- channel design of sensing
Electrode template is carried out by uv-exposure on flexible base material after treatment, interval 1- is plated by electron beam evaporation plating
10 μm of metal electrodes, two end electrodes pass through pressure welding or elargol extraction electrode lead；Micro channel electrode layer is made, designs micro- channel
Long 1-6cm, 3-100 μm of width；
Step 5: the preparation of hydrophilic protective layer
The vinylidene pvdf membrane that aperture is 0.01-0.5 microns is handled in plasma reinforced chemical vapour deposition system: being adopted
With hydrogen or oxygen reaction pressure 20-120Pa, radio-frequency power 20-80w handles at room temperature, is less than it with Liquid contact angle
5 °, hydrophilic protective layer is selected as ion, is mounted on above electrode and sensing material by epoxy resin, guard electrode material,
Sensing material guarantees that glucose molecule penetrates and precipitation simultaneously.
2. preparation method according to claim 1, which is characterized in that using magnetron sputtering or the thicknesses of layers of vapor deposition preparation
Control is in 100-250nm.
3. preparation method according to claim 1, which is characterized in that electrode uses Ti/Au electrode, uv-exposure parameter:
110 DEG C of front baking 1-15min of AZ5214 glue expose 0.1-20s, 1-5min are dried after 120 DEG C, expose 20s, and develop 0.1-5min；Electricity
Beamlet evaporation plating parameter: vacuum degree 5 × 10-6Mbar, Ti/Au thickness are respectively 10/100nm.
4. preparation method according to claim 1, which is characterized in that
The sequence of step 2 and step 3 can be exchanged successively.
5. preparation method according to claim 1-4, using blood glucose microsensor prepared by the preparation method
The blood glucose linear response for being 2-8mol/L to concentration.
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| CN110006978A (en) * | 2018-01-05 | 2019-07-12 | 张家港万众一芯生物科技有限公司 | A kind of arrays of interdigitated electrodes sensor applied to chlorine residue in quantitative detection water |
| CN109730695A (en) * | 2018-12-28 | 2019-05-10 | 浙江清华柔性电子技术研究院 | Tissue fluid detection device |
| CN109730696A (en) * | 2018-12-28 | 2019-05-10 | 浙江清华柔性电子技术研究院 | Tissue fluid detection device |
| CN110975952B (en) * | 2019-12-10 | 2020-11-17 | 华中科技大学 | Paper-based microfluid chip and preparation method and application thereof |
| CN114280113A (en) * | 2021-11-24 | 2022-04-05 | 郑州大学 | Multiple electrochemistry biological detection micro-fluidic chip based on electrode array |
| CN114280114A (en) * | 2021-11-24 | 2022-04-05 | 郑州大学 | Electrochemical biological detection micro-fluidic chip based on three-dimensional electrode |
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| CN102156156A (en) * | 2011-05-17 | 2011-08-17 | 天津大学 | Three-dimensional copper oxide nanometer flower-based chip enzyme-free glucose sensor electrode as well as preparation method and application thereof |
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