CN106983517A - One kind is without flexible blood glucose microsensor of enzyme nanometer and preparation method thereof - Google Patents
One kind is without flexible blood glucose microsensor of enzyme nanometer and preparation method thereof Download PDFInfo
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- CN106983517A CN106983517A CN201710205521.4A CN201710205521A CN106983517A CN 106983517 A CN106983517 A CN 106983517A CN 201710205521 A CN201710205521 A CN 201710205521A CN 106983517 A CN106983517 A CN 106983517A
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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 one kind without flexible blood glucose microsensor of enzyme nanometer and preparation method thereof, including：Flexible substrates, electrode structure, sensing layer and the hydrophilic protective layer of ion selectivity.Flexible substrates have good thermal adaptability (10 300 DEG C); electrode structure electric conductivity is excellent and antiacid caustic corrosion; (channel length is less than 10mm to the micro- raceway groove of glucose detection; 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 (1 28mmol/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 sensing layer.Blood glucose sensor of the present invention is nontoxic, and the comfortable not allergy of contact human body skin, its general structure is no more than 1cm2, the original position measurement in real time and analysis of blood of human body blood glucose value (1 28mmol/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 realize blood sugar for human body original position in real time detection with analysis, and ensure sensor be adapted to human body long periods of wear with
Steady operation, and 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.
The blood glucose sensor research of existing non-optical type is concentrated mainly on the side such as material modification, surface modification, combination electrode
Face.The blood glucose sensor for being mostly based on resistance or potential response is required for grape oxidase enzyme to be converted to H+Ion is visited
Survey.Attract attention and pay attention in recent years without enzyme blood glucose sensor.Zhao etc. are in paper《3D nanoporous gold
scaffold supported on graphene paper:Freestanding and flexible electrode with
high loading of ultrafine PtCo alloy nanoparticles for electrochemical
glucose sensing》It is middle to load to 3D nanoporous noble metal supports in graphene paper, then by platinum cobalt Ultra-fine Grained particle group
Glucose sensor is prepared on support, preparation technology is complicated, with high costs, test needs to carry out under alkaline environment.
Shabnam etc. is in paper《Doped graphene/Cu nanocomposite:A high sensitivity non-
enzymatic glucose sensor for food》Copper nano particles are mixed system with nitrogen-doped graphene by middle use one kettle way
Standby Cu-NGr materials, detect glucose, and three-electrode method test is complex.But existing blood glucose sensor and sensing material are present
A series of problems below：1, low using effectiveness, complex structural designs, volume is big, it is difficult to realize portable wearable function；2, technique
Cumbersome, preparation cost is too high, and service life is short, use cost is high；3, accuracy of detection is relatively low, it is difficult to realize monitoring in real time in situ；
4, blood glucose response range is narrow, it is difficult to meet the monitoring of a wide range of blood sugar concentration of diabetes patient；5, no enzyme blood glucose sensor due to
Stability and precision problem, it is current temporarily without relevant market product.
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, the combination of micro- channel structure and hydrophilic protective layer is sensed by nano wire, it is possible to achieve micro-analysis and fast slowdown monitoring,
And the highly integrated requirement of the high efficiency low cost and small size of sensor can be met, while by from the various indispensabilities to skin-friendly
Material prepares sensor, it is to avoid active layer contacts with skin that the human body brought is uncomfortable and material damage.Test environment is simple, leads to
Change of blood sugar is analyzed in overcurrent response in real time, and technique is simple, with low cost.Sensor hoist sensor without enzyme uses the longevity
Life, reduces use cost.
The present invention realizes above-mentioned technical purpose by following technological means.
A kind of preparation method without the flexible blood glucose microsensor of enzyme nanometer, 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 is laid in, carboxylic carbon nano-tube film is obtained；
Step 2：It is prepared by glucose sensing material
With Ga2O3Powder is 1 according to mol ratio with carbon dust:3 mixing, grind 5min precursor powders derived above, with step one
Obtained film plates 5nm-30nm metal catalytic agent film as substrate；Precursor powder and substrate are put into plasma enhancing
Prepared in chemical meteorology deposition system PECVD：Precursor powder is 3 with film quality ratio:1-15:1, using N2And H2As
Reacting gas, air pressure 30-120Pa；500 DEG C -1200 DEG C of underlayer temperature；Radio-frequency power supply power 40-100W；N2And H2Gas mixing
Gas, N2And H2Gas flow rate is 10 centimetres3- 100 centimetres of/minute3/ minute, the reaction time is 45-120min；
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 substrate after reason；
Step 4：Electrode and the micro- raceway groove design of sensing
Electrode template is carried out by uv-exposure in flexible substrates after the pre-treatment, interval is plated by electron beam evaporation plating
1-10 μm of metal electrode, two end electrodes pass through pressure welding or elargol extraction electrode lead；Micro channel electrode layer is made, micro- ditch is designed
Road length is less than 1-6cm, and sensing material is imported micro- raceway groove by 3-100 μm of width；
Step 5：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, is pasted onto electrode and sensing material top, guard electrode material, sensing material
Material ensures that glucose molecule is passed through simultaneously.
The order of step 2 and step 3 can be exchanged successively.
Further, magnetron sputtering and evaporation, thicknesses of layers are 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.
The flexible blood glucose microsensor of prepared nanometer is used to be 1-28mmol/L blood glucose linear responses to concentration.
It is a kind of without flexible blood glucose sensor of enzyme nanometer and preparation method thereof, including：Flexible substrates, electrode structure, glucose
Detect the hydrophilic protective layer of micro- raceway groove, ion permeable.Using bend resistance flexible polymer as substrate, electrode is designed by template
Micro- channel structure, nano wire textured material is transferred in micro- raceway groove as sensitive layer, is covered with the hydrophilic wearing layer of ion permeable
Electrode is realized glucose quick adsorption and avoided and direct body contact with sensitive layer.
The flexible substrates are using nontoxic, bend resistance polymer such as polyimides (PI) etc., at plasma
Reason enhancing hydrophily (5 ° of contact angle ＜).
The flexible substrates thickness is 50-200 μm, and entire area is less than 1cm2。
The sensitive layer material selects that growth is had into gallium nitride nanometer using micro-nano technology in the micro- raceway groove of texture nano wire
The carboxyl function carbon nano tube texture of line imports micro- raceway groove as the induction zone material in situ of glucose molecule.
The micro- channel structure of electrode is made by template, and micro- channel length is less than 5mm, 3-100 μm of width.
One kind comprises the following steps without flexible blood glucose microsensor of enzyme nanometer and preparation method thereof：
(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 using photoetching process.
(3) nanometer texture glucose-sensitive layer makes.The carboxylated carbon nanometer for having gallium nitride nano-wire is grown by PECVD
Pipe texture imports micro- raceway groove as the induction zone material in situ of glucose molecule, prepares glucose molecule sensitive layer 3.
(4) the hydrophilic protective layer processing of ion permeable and encapsulation, surface mount is carried out by the hydrophilic wearing layer after processing, overall
Area is 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 more for a long time
Secondary use does not fall off.The hydrophilic wearing layer of ion permeable is porous hydrophilic thin polymer film, and processing mode is oxygen plasma processing,
Aperture is at 0.1-1 μm, and thickness is not more than 0.1mm.
Beneficial effects of the present invention：
(1) what the present invention was provided is a kind of without flexible glucose sensor of enzyme nanometer and preparation method thereof, is set by template
The combination that nano wire texture senses micro- raceway groove and the hydrophilic wear-resistant coating of ion selection is counted, realizes that the small size of device is highly integrated, and
Adequately protect device active layer, prevents because peeling off occurs in Reusability and fails.GaN and carboxylation carbon pipe film formation hetero-junctions,
Electric current linear response is produced to glucose molecule,
(2) it is of the present invention a kind of without flexible glucose sensor of enzyme nanometer and preparation method thereof, pass through ion permeable
The use of hydrophilic wearing layer, it is to avoid sensitive material and electrode material are contacted with the direct of measured body, are applied to wearable biological Portugal
On grape sugar sensor, material can be eliminated and the allergy of direct body contact's arrival is reacted with uncomfortable, while protecting sensitive layer not
It is damaged long-term precise operation.Be free of glucose oxidase in whole material simultaneously, it is to avoid enzyme influenceed by temperature, acid-base property etc. and
Change the test error caused by activity.
(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 1-28mmol/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
Fig. 3 is that carbon pipe film grows GaN nano wire
Fig. 4 is the response curve of embodiment 1
Fig. 5 is the response curve of embodiment 2
Fig. 6 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；With Ga2O3(mol ratio is 1 to powder with carbon dust:3) mix, grinding 5min obtains front axle shell
Body：In carboxylated carbon pipe film as substrate, plating 10nm Au is used as catalyst film；By precursor powder and substrate be put into etc. from
Prepared in son enhancing chemical meteorology deposition system：Precursor powder is 10 with film quality ratio:1, using N2And H2Mixed gas
For reacting gas, air pressure 90Pa；700 DEG C of underlayer temperature；Radio-frequency power supply power 80W；N280 centimetres of gas flow rate3/ minute, H2Gas
50 centimetres of rate of flow of fluid3/ minute, react 65min.Sensing material is made, its size is identical with micro- raceway groove.
(2) by 100 μm of flexibility PI substrates in oxygen plasma processing, design parameter：Vacuum 0.1Pa, operating air pressure
20Pa, working gas O2, flow 20sccm, radio-frequency power 60w, room temperature treatment 5min makes flexible substrates be less than with Liquid contact angle
5 °, 1 μm of epoxy resin is coated with pre-processed substrate；Then it is cut into 1 × 1cm2Slice, thin piece, is made flexible substrates.
(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.Two end electrodes pass through pressure welding or elargol extraction electrode lead.Micro- channel length is designed for 1cm, 10 μm of width is made
Micro channel electrode layer, electrode thickness 150nm.Sensing material made from step (1) is imported into raceway groove.
(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 400 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 3mmol/L, 4mmol/L, 5mmol/L, 6mmol/L respectively, tests its sensitive property.
Test data is shown in Fig. 4, and the response time is less than 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 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；With Ga2O3(mol ratio is 1 to powder with carbon dust：3) mix, grinding 4min obtains front axle shell
Body：In carboxylated carbon pipe film as substrate, plating 20nm Au is used as catalyst film；By precursor powder and substrate be put into etc. from
Prepared in son enhancing chemical meteorology deposition system：Precursor powder is 5 with film quality ratio:1, using N2And H2It is used as reaction
Gas, air pressure 60Pa；500 DEG C of underlayer temperature；Radio-frequency power supply power 80W；N260 centimetres of gas flow rate3/ minute, H2Gas flow rate
50 centimetres3/ minute, the reaction time is 75min.Sensing material is made, its size is identical with micro- raceway groove.
(2) by 100 μm of flexibility PI substrates in oxygen plasma processing, design parameter：Vacuum 0.1Pa, operating air pressure
20Pa, working gas O2, flow 20sccm, radio-frequency power 60w, room temperature treatment 5min makes flexible substrates be less than with Liquid contact angle
5 °, 1 μm of epoxy resin is coated with pre-processed substrate；Then it is cut into 1 × 1cm2Square piece, is made flexible substrates.
(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.Two end electrodes pass through pressure welding or elargol extraction electrode lead.Micro channel electrode layer is made, electrode thickness 200nm is long
Spend for 2cm, 10 μm of width.Sensing material made from step (1) is imported into raceway groove.
(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 400 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. 5, and the response time is less than 1s, and tests device recovery, and response rate is more than 90%.
Claims (5)
1. a kind of preparation method without the flexible blood glucose microsensor of enzyme nanometer, 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 is laid in, carboxylic carbon nano-tube film is obtained；
Step 2：It is prepared by glucose sensing material
With Ga2O3Powder is 1 according to mol ratio with carbon dust:3 mixing, grind 5min precursor powders derived above, are obtained with step one
Film be used as substrate, plate 5nm-30nm metal catalytic agent film；Precursor powder and substrate are put into plasma-reinforced chemical
Prepared in vapor phase deposition system PECVD：Precursor powder is 3 with film quality ratio:1-15:1, using N2And H2It is used as reaction
Gas, air pressure 30-120Pa；500 DEG C -1200 DEG C of underlayer temperature；Radio-frequency power supply power 40-100W；N2And H2Gas mixing gas,
N2And H2Gas flow rate is 10 centimetres3- 100 centimetres of/minute3/ minute, the reaction time is 45-120min；
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 afterwards；
Step 4：Electrode and the micro- raceway groove design of sensing
Electrode template is carried out by uv-exposure in flexible substrates after the pre-treatment, interval 1-10 is plated by electron beam evaporation plating
μm metal electrode, two end electrodes pass through pressure welding or elargol extraction electrode lead；Micro channel electrode layer is made, micro- raceway groove is designed long
Degree is less than 1-6cm, and sensing material is imported micro- raceway groove by 3-100 μm of width；
Step 5：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, electrode is pasted onto and above sensing material, guard electrode material, sensing material is simultaneously
Ensure that glucose molecule is passed through.
2. preparation method according to claim 1, magnetron sputtering or evaporation, thicknesses of layers are controlled in 100-250nm.
3. the order of preparation method according to claim 1, step 2 and step 3 can be exchanged successively.
4. 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.
5. the flexible blood glucose microsensor of nanometer prepared by any one of the claim 1-4 preparation methods is used to be 1- to concentration
28mmol/L blood glucose linear responses.
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