CN107028615A - Flexible blood glucose microsensor of a kind of nanometer and preparation method thereof - Google Patents
Flexible blood glucose microsensor of a kind of nanometer and preparation method thereof Download PDFInfo
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- 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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Abstract
The invention discloses flexible blood glucose microsensor of a kind of nanometer and preparation method thereof, including：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- raceway groove, and (channel length is less than 10mm; 500 μm of width 10 μm) constituted for nano material texture; pliability is good; sensitivity is high; linear dependence is presented in concentration of glucose (0.5 30mmol/L) scope; with good invertibity and repeatability, hydrophilic wear-resistance thin film has good ion permeable characteristic, strong water absorption character and the effect of protection sensitive layer.The present invention is nontoxic, the comfortable not allergy of contact human body skin, and its general structure, which is no more than, is less than 1cm2, the original position measurement in real time 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 flexible blood glucose sensor of nanometer and its
Preparation method, for realizing original position detection in real time and analysis to blood sugar for human body, and ensures that sensor is adapted to human body long periods of wear
With steady operation, noninvasive or minimally invasive blood sugar monitoring can be realized, and meet a wide range of blood sugar monitoring of diabetes.
Background technology
Blood glucose is closely bound up with health, long term hyperglycemia can cause various complication (such as uremia, limb necrosis,
Blindness etc.), and hypoglycemia can cause the consequence such as powerless of fainting, have palpitation, therefore blood sugar test is to health important in inhibiting.
But traditional blood sugar test equipment volume is huge, and time-consuming, it is impossible to realize accurate detection in real time, limit popularization in the family and
Use.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 in terms of material modification, surface modification, combination electrode,
Lee etc. are in paper《Flexible chitosan/carbon nanotubes aerogel,a robust matrix forin-
situ growth and non-enzymatic biosensing applications》In mention CNT changed
Property, CNT and chitosan are assembled together as by sensitive materials using ice masterplate method and prepare blood glucose biography on a flexible substrate
Sensor, but test process needs reference electrode, and test environment requirement is alkaline solution.Designed in terms of flexible sensor array,
Wei Gao etc. are 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
Sense microdevice to merge in same flexible substrate, design technology is complicated, is unfavorable for realizing product mass production.It is comprehensive
Close and consider existing glucose sensor generally existing a series of problems：1, complex structural designs low using effectiveness, volume is big, difficult
To realize portable wearable function；2, technique is cumbersome, and device cost is too high；3, accuracy of detection is relatively low, it is difficult to realize real-time in-situ
Monitoring；4, test environment requires 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
Survey.
The content of the invention
The above mentioned problem existed during for actual use, the present invention devises a kind of flexible blood glucose sensor of nanometer and its system
Preparation Method, by the combination for sensing micro- channel structure and hydrophilic wearing layer, it is possible to achieve micro-analysis and fast slowdown monitoring, and can expire
The highly integrated requirement of the high efficiency low cost and small size of sufficient sensor, while by comfortably good from and body-sensing nontoxic to skin
Material prepare sensor, it is to avoid active layer contacts with skin that the human body brought is uncomfortable and material damage.Test environment is simple,
Change of blood sugar is analyzed by current-responsive in real time, technique is simple, with low cost.
The present invention realizes above-mentioned technical purpose by following technological means.
The preparation method of a kind of nanometer of flexible blood glucose sensor, it is characterised in that comprise the following steps：
Step one：CNT film forming
CNT is weighed according to 0.1-0.3mg/mL concentration, volume ratio 3 is placed on：The 1 dense sulphur of mass fraction 95-98%
Acid removes supernatant, regulation pH with the mixed acid of mass fraction 65-68% concentrated nitric acids, stirring 45-90min, centrifugation at 110 DEG C
To neutrality；Evaporating water at 30-60 DEG C of tiling, obtains carboxylic carbon nano-tube film；
Step 2：It is prepared by glucose sensing material
It is made using magnetron sputtering in step one on film and prepares zinc oxide, target selects zinc oxide, sputtering pressure is
1pa, target-substrate distance 5-10cm, sputtering power 50-300W, with argon gas as protection gas, substrate temperature is normal temperature, sputters 20-
90min；Spraying 5-30 μ L glucoses aoxidize enzyme solutions on the material, and obtained sensing material is identical with micro- trench size；Portugal
Grape oxidase solution concentration is 1-40mg/mL；
Step 3：Flexible substrate is pre-processed
Flexible base material is handled in plasma reinforced chemical vapour deposition system：Using hydrogen or oxygen reaction gas
20-120Pa is pressed, radio-frequency power is 20-80W, and flexible substrates are handled at room temperature, it is less than 5 ° with Liquid contact angle, locating in advance
It is 1-3 μm of epoxy resin that thickness is coated with reason substrate；
Step 4：Electrode and the micro- raceway groove design of sensing
Electrode template is carried out by uv-exposure on flexible base material after treatment, between being plated 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-
The long 1-6cm of raceway groove, 3-100 μm of width；
Step 5：The preparation of hydrophilic protective layer
Aperture is located for 0.01-0.5 microns of vinylidene pvdf membrane in plasma reinforced chemical vapour deposition system
Reason：Using hydrogen or oxygen reaction air pressure 20-120Pa, radio-frequency power is 20-80w, handles at room temperature, it is contacted with liquid
Angle is less than 5 °, and hydrophilic protective layer is selected as ion, and electrode and sensing material top, guard electrode are mounted on by epoxy resin
Material, sensing material ensure that glucose molecule is passed through and precipitation simultaneously.
Further, the thicknesses of layers prepared using magnetron sputtering or evaporation is controlled in 100-250nm.
Further, electrode uses Ti/Au electrodes, uv-exposure parameter：110 DEG C of front baking 1-15min of AZ5214 glue, exposure
0.1-20s, 1-5min is dried after 120 DEG C, exposes 10-15s, and develop 0.1-5min；Electron beam evaporation plating parameter：Vacuum 5 × 10- 6Mbar, Ti/Au thickness are respectively 10/100nm；
Glucose sensing material is prepared with flexible substrate processing without sequencing.
Prepared blood glucose microsensor is used to be 0.5-30mmol/L blood glucose linear responses to concentration.
Flexible blood glucose sensor of a kind of nanometer and preparation method thereof, including：Flexible substrates, epoxy resin layer, electrode structure,
Glucose oxidase loads micro- raceway groove, the hydrophilic wearing layer of ion permeable.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 (CNT zinc oxide composite) is transferred in micro- raceway groove as sensitivity with 1~40mg/mL glucolases
Layer, realizes glucose quick adsorption with sensitive layer with the hydrophilic wearing layer covering electrode of ion permeable and avoids directly connecing with human body
Touch.
The flexible substrates are using nontoxic, bend resistance polymer such as PI etc., by handling hydrophily and surface attachment
Property is good.
The flexible substrates thickness is 50-200 μm, and entire area is less than 1cm2。
The CNT zinc oxide composite film of the sensitive layer material selection carboxylated surface processing of the nano wire texture is born
Carry glucose oxidase film.
The micro- channel structure of electrode is made by template, and micro- channel length is less than 5mm, 3-100 μm of width.
The hydrophilic wearing layer of ion permeable is porous polymer film, and good hydrophilic property, glucose molecule transmitance is high.
Flexible glucose sensor of a kind of nanometer and preparation method thereof, comprises the following steps：
(1) selection and surface treatment of flexible substrates：Flexible base material selection includes PI etc., with good mechanics and
Thermal adaptability, surface treatment strengthens the adhesion properties such as electrode, sense channel and hydrophilic film.Flexible substrates 1 are made.
(2) the micro- channel structure design and fabrication of electrode：Can according to device detection with it is integrated require design structure size, for protect
Electrode excellent conductive performance is demonstrate,proved with saving cost, is antiacid caustic corrosion by most there is structure design, it is steady from the chemistry such as Au, Pt
Qualitative good metal material.The micro- raceway groove 2 of electrode is made.
(3) handled by strong acid (concentrated sulfuric acid, concentrated nitric acid), carboxylic group is introduced in CNT, strengthen CNT
Hydrophily (contact angle is less than 5 °), is made CNT zinc-oxide film, in carbon nano-tube film zinc oxide using magnetron sputtering
Appropriate (1-40mg/mL) glucose oxidase is sprayed on composite to import in micro- raceway groove as sensitive materials.
(4) the hydrophilic wear-resistant coating processing of ion permeable and encapsulation, surface mount is carried out by the hydrophilic wearing layer after processing, whole
Bulk area is no more than substrate sizes, and electrode and sensitive layer be completely covered by avoid friction, it is ensured 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 processing.
The micro- channel structure design method of step (2) electrode is included by mask plate, uv-exposure or electron beam exposure etc.
One or more of design electrode structures in means.
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
Plant or several making electrode layers, thickness of electrode is controlled in 100-150nm, it is ensured that cost is reduced while electric conductivity.
The hydrophilic wearing layer of step (4) ion permeable is porous hydrophilic thin polymer film, and processing mode is oxygen plasma
Body processing, aperture is at 0.1-1 μm, and thickness is not more than 0.1mm.
Beneficial effects of the present invention：
(1) flexible glucose microsensor of a kind of nanometer that the present invention is provided and preparation method thereof, is designed by template
Nanometer texture senses micro- raceway groove and ion selects the combination of hydrophilic wear-resistant coating, realizes that the small size of device is highly integrated, and fully
Protection device active layer, is prevented because peeling off occurs in Reusability and fails.Based on the surface energy that carbon nano-tube film is larger, use
Sputtering zinc oxide, while the method for spraying glucose oxidase prepares sensing material, to the linear sensitivity of glucose.
(2) flexible glucose microsensor of a kind of nanometer of the present invention and preparation method thereof, passes through ion permeable parent
The use of water wearing layer, it is to avoid sensitive material and electrode material are contacted with the direct of measured body, are being applied to wearable biological Portugal
On grape sugar microsensor, material can be eliminated and the allergy of direct body contact's arrival is reacted with uncomfortable, while protecting sensitive layer
Injury-free long-term precise operation.
(3) current-responsive that test philosophy of the present invention is caused based on resistance variations, test environment require 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).
Brief description of the drawings
Fig. 1 is that (1 is flexible substrates to sensor structure figure, and 2 be electrode layer, and 3 be that interdigital electrode position is sensing material position
Put, 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
The response curve of Fig. 3 embodiments one
The response curve of Fig. 4 embodiments two
Fig. 5 bend tests influence on sensitivities
Embodiment
Embodiment 1
(1) using volume ratio as 3：The 1 pure concentrated nitric acid of analysis (mass fraction 68%) and the pure concentrated sulfuric acid (mass fraction of analysis
98%) mixed liquor introduces carboxylic group in single-walled carbon nanotube, 90min is stirred at 110 DEG C, in height as acidifying liquid
Centrifuged in fast centrifuge 9500rad/min, filter off supernatant, regulation carbon pipe pH to neutrality, evaporating water at 50 DEG C of tiling is obtained
Single wall carboxyl-functional carbon pipe film.Using zinc oxide as target, sputtering pressure is 1pa, target-substrate distance 7cm, sputtering power
CNT zinc oxide composite is made under 50W, argon flow amount 40sccm, room temperature condition, thickness is 200nm.In the material
10 μ L (concentration 35mg/mL) glucose oxidases of upper spraying, as sensing material, sensing material used and micro- trench size phase
Together；
(2) it is that 100 μm of flexibility PI substrates are handled in oxygen plasma by thickness, design parameter：Vacuum 0.1Pa, work
Air pressure 20Pa, working gas O2, flow 20sccm, radio-frequency power 60w, room temperature treatment 5min make flexible substrates be contacted with liquid
Angle is less than 5 °, and 1 μm of epoxy resin of thickness is coated with pre-processed substrate；Then it is cut into 1 × 1cm2Square piece, is made flexibility base
Bottom, imports made sensing material in 1.
(3) design such as Fig. 1 Lithographic templates, carry out electrode template by uv-exposure on the PI slice, thin pieces of processing, pass through electricity
Beamlet plates the 3 μm of Ti/Au electrodes in interval, 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 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.Micro- channel length is designed for 1cm, it is wide
10 μm of degree, is made micro channel electrode layer, thick 100nm.The sensing material that in channels prepared by steps for importing (1).
(4) by 100 μm of thickness, the PVDF micropores wearing layer in 0.47 μm of aperture carries out Surface Oxygen corona treatment increase parent
It is aqueous, design parameter：Vacuum 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 × 1cm2Slice, thin piece, is mounted on electrode with above sensing material, ion permeable being made hydrophilic wear-resisting
Layer, makes it be less than 5 ° with Liquid contact angle；
(5) PI flexible substrates are used at being used in temperature less than 300 DEG C, and senser element is sensitive to glucose solution, response
Curve respectively takes the glucose solution that 3 μ L concentration are 3mmol/L, 4mmol/L, 5mmol/L, 6mmol/L respectively close to linear, surveys
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 more than 90%.
Embodiment 2
(1) using volume ratio as 3：The 1 pure concentrated nitric acid of analysis (mass fraction 68%) and the pure concentrated sulfuric acid (mass fraction of analysis
98%) mixed liquor stirs 60min as acidifying liquid at 110 DEG C, is centrifuged in supercentrifuge 9500rad/min, filters off
Supernatant, regulation carbon pipe pH to neutrality, evaporating water at 50 DEG C of tiling obtains single wall carboxyl-functional carbon pipe film.Target is selected
With zinc oxide, sputtering pressure is 1pa, target-substrate distance 5cm, sputtering power 80W, argon flow amount 30sccm, and substrate temperature temperature is room
Temperature, sputters 80min, CNT zinc oxide composite is made, thickness is 100nm, and 20 μ L (concentration are sprayed on the material
25mg/mL) glucose oxidase, as sensing material, is made sensing material identical with micro- trench size；
(2) it is that 100 μm of flexibility PI substrates are handled in oxygen plasma by thickness, design parameter：Vacuum 0.1Pa, work
Air pressure 20Pa, working gas O2, flow 20sccm, radio-frequency power 60w, room temperature treatment 5min.Flexible substrates are made to be contacted with liquid
Angle is less than 5 °, and 1 μm of epoxy resin of thickness is coated with pre-processed substrate；Then it is cut into 1 × 1cm2Square piece, is made flexibility base
Bottom.
(3) design such as Fig. 1 Lithographic templates, carry out electrode template by uv-exposure on the PI slice, thin pieces of processing, pass through electricity
Beamlet plates the 6 μm of Ti/Au electrodes in interval, 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 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.Micro- channel length is designed for 2cm, it is wide
80 μm of degree, is made micro channel electrode layer.The sensing material that in channels prepared by steps for importing (1).
(4) by 100 μm of thickness, the PVDF micropores wearing layer in 0.47 μm of aperture carries out Surface Oxygen corona treatment increase parent
It is aqueous, design parameter：Vacuum 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 × 1cm2Slice, thin piece, is mounted on electrode with above sensing material, ion permeable being made hydrophilic wear-resisting
Layer, makes it be less than 5 ° with Liquid contact angle；
(5) PI substrates can be used below at 300 DEG C, and senser element is sensitive to glucose solution, and response curve is close linear,
The glucose solution for respectively taking 3 μ L concentration to be 2mmol/L, 4mmol/L, 6mmol/L, 8mmol/L respectively, 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 more than 90%.
Claims (5)
1. the preparation method of a kind of nanometer of flexible blood glucose microsensor, it is characterised in that comprise the following steps：
Step one：CNT film forming
CNT is weighed according to 0.1-0.3mg/mL concentration, volume ratio 3 is placed on：The 1 mass fraction 95-98% concentrated sulfuric acids with
In the mixed acid of mass fraction 65-68% concentrated nitric acids, 45-90min is stirred at 110 DEG C, centrifugation removes supernatant, regulation pH into
Property；Evaporating water at 30-60 DEG C of tiling, obtains carboxylic carbon nano-tube film；
Step 2：It is prepared by glucose sensing material
It is made using magnetron sputtering in step one on film and prepares zinc oxide, target selects zinc oxide, sputtering pressure is 1pa, target
Cardinal distance 5-10cm, sputtering power 50-300W, with argon gas as protection gas, substrate temperature is normal temperature, sputters 20-90min；At this
5-30 μ L glucoses oxidation enzyme solutions are sprayed on material, obtained sensing material is identical with micro- trench size；Glucose oxidase
Solution concentration is 1-40mg/mL；
Step 3：Flexible substrate is pre-processed
Flexible base material is handled in plasma reinforced chemical vapour deposition system：Using hydrogen or oxygen reaction air pressure
20-120Pa, radio-frequency power is 20-80W, and flexible substrates are handled at room temperature, it is less than 5 ° with Liquid contact angle, in pretreatment
It is 1-3 μm of epoxy resin that thickness is coated with substrate；
Step 4：Electrode and the micro- raceway groove 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, micro- raceway groove is designed
Long 1-6cm, 3-100 μm of width；
Step 5：The preparation of hydrophilic protective layer
Aperture is handled for 0.01-0.5 microns of vinylidene pvdf membrane in plasma reinforced chemical vapour deposition system：Adopt
With hydrogen or oxygen reaction air pressure 20-120Pa, radio-frequency power is 20-80w, handles at room temperature, it is less than with Liquid contact angle
5 °, hydrophilic protective layer is selected as ion, is mounted on by epoxy resin above electrode and sensing material, guard electrode material,
Sensing material ensures that glucose molecule is passed through and precipitation simultaneously.
2. preparation method according to claim 1, it is characterised in that the thicknesses of layers prepared using magnetron sputtering or evaporation
Control is in 100-250nm.
3. preparation method according to claim 1, it is characterised in that electrode uses Ti/Au electrodes, uv-exposure parameter：
110 DEG C of front baking 1-15min of AZ5214 glue, expose and 1-5min are dried after 0.1-20s, 120 DEG C, expose 10-15s, and develop 0.1-5min；
Electron beam evaporation plating parameter：Vacuum 5 × 10-6Mbar, Ti/Au thickness are respectively 10/100nm.
4. preparation method according to claim 1, it is characterised in that
The order of step 2 and step 3 can be exchanged successively.
5. the blood glucose microsensor prepared by preparation method of the application as described in claim any one of 1-4 is used for
0.5-30mmol/L blood glucose linear responses.
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| 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 |
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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 |
| CN110975952A (en) * | 2019-12-10 | 2020-04-10 | 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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| 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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