CN109374877A - A kind of preparation method and applications with nano column array paper - Google Patents
A kind of preparation method and applications with nano column array paper Download PDFInfo
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- CN109374877A CN109374877A CN201811092182.4A CN201811092182A CN109374877A CN 109374877 A CN109374877 A CN 109374877A CN 201811092182 A CN201811092182 A CN 201811092182A CN 109374877 A CN109374877 A CN 109374877A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
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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
- A61B5/02—Detecting, measuring or recording pulse, heart rate, blood pressure or blood flow; Combined pulse/heart-rate/blood pressure determination; Evaluating a cardiovascular condition not otherwise provided for, e.g. using combinations of techniques provided for in this group with electrocardiography or electroauscultation; Heart catheters for measuring blood pressure
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/68—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient
- A61B5/6801—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be attached to or worn on the body surface
- A61B5/6802—Sensor mounted on worn items
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
- A61B2562/02—Details of sensors specially adapted for in-vivo measurements
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Abstract
The invention discloses a kind of preparation method and applications with nano column array paper, its preparation step is as follows: 1) selecting single-pass anodic oxidation aluminium formwork, after cleaning using acetone and ethyl alcohol to single-pass anodic oxidation aluminium formwork, Surface Treatment with Plasma is carried out to its surface；2) precursor liquid that nano column array paper is perfused into treated single-pass anodic oxidation aluminium formwork erodes single-pass anodic oxidation aluminium formwork, is obtained after cleaning with nano column array paper after precursor liquid drying and moulding.What this method was prepared there is nano column array paper to have close skin attachement, and the ability with multivariate analysis, the multivariate analysis to a variety of determinands may be implemented applied to field of fast detection, transducer sensitivity can be significantly improved applied to wearable sensor field, is had the advantages that at low cost, reusable, highly sensitive.
Description
Technical field
The present invention relates to a kind of preparation method and applications with nano column array paper, belong to function of paper field.
Background technique
With the development of modern society, people pay much attention to the acquisition of itself various health indicator, wearable sensing
Device is widely paid close attention to because it has to be attached at due to human body and real-time monitoring collect human body health signal the characteristics of.Wearable biography
Sensor has the characteristics that small in size, Highgrade integration, multifunction, high sensitivity, stability are strong.At present it is commercialized it is various can
It is various to dress sensor, including flexible sensor and wearable electronic product, but wearable sensors still have it is all
More problems, if substrate and human skin contact are poor, affect signal stablizes acquisition and transmission, thereby reduces the spirit of detection
Sensitivity.In addition, existing wearable sensor is concentrated mainly on personal body movement (the heart rate and step number) signal of tracking at present
Collection, human body biochemical indicator (pH, lactic acid, urea, ion etc.) cannot be detected.Wearable biology existing at present passes
Sensor have have a single function, the problem of Sensitivity Stability difference, limit its extensive use in daily life, thus urgent need
Accurately, delicately sensor detects index of correlation, and such sensor needs the conduct substrate of functionalization material.
Paper is a kind of indispensable material of today's society, has extremely wide application, is people's daily life, work
The necessity made and learnt.The main component of paper is cellulose, and cellulose is that reserves are most abundant in nature, it is also most wide to be distributed
Natural polymer, be a kind of degradable, renewable resource.In addition to this, paper is also equipped at low cost, nontoxic, bio-compatibility
Well, good mechanical properties, porosity are high, are easy to the features such as physics and chemical modification, can be used as a kind of outstanding functional material
With the important substrate of composite material.Therefore, the structure of modification of paper is particularly important to the purposes for expanding paper, simultaneously for realization
The sustainable development of society is also of great significance.
In view of the deficienciess of the prior art, the present invention provides a kind of single based on corrosion in conjunction with the structure of modification technology of paper
The mode of logical anodised aluminium (AAO) template makes the paper substrates for having nano column array, and the paper of preparation has preferable fitting
Property, significantly enhance the signal of pulse transducer；By carrying out the Imprint patterning paper that multichannel may be implemented in paper substrates
The production of chip.
Summary of the invention
Technical problem: in view of the deficienciess of the prior art, the object of the present invention is to provide one kind to have nano column array
The preparation method and applications of paper, preparation method of the present invention is simple, can mass production, the nano column array paper tool being prepared
Have the characteristics that skin attachement, for detecting when it is strong with high sensitivity, signal, have good use value.
Technical solution: for the purpose for realizing foregoing invention, the present invention provides a kind of preparations with nano column array paper
Method, method includes the following steps:
1) single-pass anodised aluminium (AAO) template is selected, single-pass anodic oxidation aluminium formwork is carried out using acetone and ethyl alcohol
After cleaning, Surface Treatment with Plasma is carried out to its surface；
2) precursor liquid of nano column array paper is perfused into treated single-pass anodic oxidation aluminium formwork, to precursor liquid 50
After~80 DEG C of drying and mouldings, single-pass anodic oxidation aluminium formwork is eroded, is obtained after cleaning with nano column array paper.
Wherein:
The single-pass anodic oxidation aluminium formwork have cellular pore structure, and the range of aperture size in hole be 20nm~
400nm, pitch of holes 60nm~450nm, hole depth be 150nm~120 μm.
The progress Surface Treatment with Plasma of surface described in step 1) refers to be handled under conditions of power is 150W~300W
For 60~300s.
The precursor liquid of nano column array paper described in step 2) is nitrocellulose (NC) precursor liquid, dimethyl silicone polymer
(PDMS) before precursor liquid, polystyrene (PS) precursor liquid, polymethyl methacrylate (PMMA) precursor liquid or polyurethane (PU)
Drive liquid.
During eroding single-pass anodic oxidation aluminium formwork described in step 2), used corrosion reagent be hydrofluoric acid,
Phosphoric acid or sodium hydroxide.
The present invention also provides what a kind of preparation method with nano column array paper was prepared to have nano column array
The application of paper, described there is nano column array paper to be applied to quickly detection or wearable sensor field.
Wherein:
It is as follows applied to the method quickly detected:
Step 1 will have nano column array paper to carry out Surface Treatment with Plasma；
Step 2, template imprint by way of, using with figuratum seal nano column array paper have nano-pillar
Produce microfluidic channel in the side of array；
Step 3, the fixed inspection reagent in microfluidic channel, to detect determinand.
There to be nano column array paper to carry out Surface Treatment with Plasma described in step 1 and refer to that in power be 150W~300W
Under conditions of processing be 60~300s.
It is adjusted according to demand described in step 2 with the pattern on figuratum seal；The template moulding process
Middle pressure limit is 0.1~1MPa；The width of the microfluidic channel is between 30~2000 μm, quantity >=1；Institute
The material with figuratum seal stated is that perhaps its processing method of organic glass is photoetching or laser cutting to stainless steel.
The multivariate analysis of determinand is realized in type >=a kind of testing reagent described in step 3.
The testing reagent is pH, lactic acid or urea testing reagent, and the object of analysis is human sweat.
Method applied to wearable sensor field is as follows:
1., by wearable sensor step is fixed on the side without nanometer rod structure with nano column array paper；
2., by the side with nanometer rod structure with nano column array paper step fits in position to be detected, carry out
Detection.
1. the wearable sensor is piezoelectric transducer, capacitance sensing for human health signal detection to step
Device or electric resistance sensor.
Step is 1. described to be fixed on wearable sensor one without nanometer rod structure with nano column array paper
Side, fixed form are to be fixed with double faced adhesive tape, and the material of adhesive tape is polyethylene terephthalate (PET), poly- diformazan
Radical siloxane (PDMS), polymethyl methacrylate (PMMA) or polyurethane (PU).
Step 2. the laminating type for fitting in position to be detected be use with a thickness of 1~10 μm double faced adhesive tape into
Row fitting, and the material of adhesive tape is polyethylene terephthalate (PET), dimethyl silicone polymer (PDMS), poly- methyl-prop
E pioic acid methyl ester (PMMA) or polyurethane (PU).
Sensor is fitted in on nano column array paper and being affixed on skin and can significantly improve the sensitivity of sensor spirit.
The utility model has the advantages that compared with prior art, present invention has the advantage that
1, the present invention is based on the modes of corrosion AAO template to make the paper substrates for having nano column array, preparation method is simple,
Can mass production, gained have nano column array paper have preferable stickiness；
2, the present invention realizes multichannel by carrying out Imprint patterning on nano column array paper in having of being prepared
The production of paper chip, the diversification for object to be detected detect, and have the characteristics that high sensitivity, signal are strong；
3, what the present invention was prepared has nano column array paper with skin attachement, by by itself and wearable device
It is used in combination, solves the disadvantages of wearable device medium sensitivity is low, interference is big, there is good use value；
4, the present invention be prepared with nano column array paper in quick detection or wearable sensor field
It is at low cost, reusable, highly sensitive using having the advantages that.
Detailed description of the invention
Fig. 1 is the preparation method flow diagram provided by the invention with nano column array paper；
Fig. 2 is the patterning method schematic diagram provided by the invention with nano column array paper；
Fig. 3 is to utilize the patterned fluorescence intensity figure that fluorescence detection lactic acid concn is used for nano column array paper；
Fig. 4 is to utilize the patterned fluorescence intensity figure that fluorescence detection urea concentration is used for nano column array paper；
Fig. 5 is the effect of signals comparison diagram with nano column array paper and structureless paper to piezoelectricity pulse transducer.
Specific embodiment
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, and the present embodiment is with technical solution of the present invention
Premised under implemented, it should be understood that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.
Embodiment 1:
A kind of preparation method (as shown in Figure 1) with nano column array paper, method includes the following steps:
1) selecting aperture in 20nm, pitch of holes 60nm, hole depth is 500nm single-pass anodised aluminium (AAO) template, is utilized
After acetone and ethyl alcohol clean single-pass anodic oxidation aluminium formwork, Surface Treatment with Plasma, treatment conditions are carried out to its surface
Are as follows: power 100W, time 300s；
2) precursor liquid of nano column array paper, i.e. nitrocellulose are perfused into treated single-pass anodic oxidation aluminium formwork
(NC) precursor liquid (7.5%, w/v, acetone), and in 50 DEG C of drying and mouldings；
3) corrode AAO template using 4% hydrofluoric acid, spontaneously dry and obtain with nano column array at room temperature after cleaning
NC paper.
A kind of application with nano column array paper, there is nano column array paper to be applied to quickly detection for this, and method is such as
Under:
Step 1 handles the above-mentioned NC paper being prepared using Plasma plasma processor, is 100W's in power
Under the conditions of handle 300s；
Step 2, layout as needed are made using the mode of photoetching with figuratum stainless steel imprinting seal；
Seal is carried out imprinted pattern under 0.1MPa pressure condition using the mode that template imprints by step 3 on paper
Change to make microfluidic channel, the width of microfluidic channel obtains having a plurality of microfluidic channel between 30~2000 μm
NC nano column array paper (as shown in Figure 2)；
Lactate detection object and urea detectable substance is added dropwise in the end of different microfluidic channels in step 4 respectively, uses after dry
5% bovine serum albumin(BSA) (BSA) solution closed channel, it is spare；
The mixture of determinand lactic acid and urea is added dropwise in the sample introduction end of microfluidic channel step 5, and determinand passes through micro-
Fluid channel flows to detection zone and sufficiently reacts generation fluorescent molecule with detectable substance, detects fluorescence signal using fluorescence detector,
The result shows that detecting lactic acid (Fig. 3) and urea (Fig. 4) using the NC paper with nano column array has good linear relationship.
Embodiment 2:
A kind of preparation method with nano column array paper, method includes the following steps:
1) selecting aperture in 100nm, pitch of holes 150nm, film thickness is 500nm single-pass anodised aluminium (AAO) template, is utilized
After acetone and ethyl alcohol clean single-pass anodic oxidation aluminium formwork, Surface Treatment with Plasma is carried out to its surface, power is
150W, processing time are 200s；
2) forerunner of nano column array paper, i.e. polymethylacrylic acid are perfused into treated single-pass anodic oxidation aluminium formwork
Methyl esters (PDMS, 10:1, w/w), and in 60 DEG C of drying and mouldings；
3) the phosphoric acid corrosion AAO template for using 4%, spontaneously dries at room temperature after cleaning and obtains having nano column array
NC paper.
A kind of application with nano column array paper, there is nano column array paper to be applied to wearable sensor, side for this
Method is as follows:
The PET double-sided adhesive of 1 μ m-thick of the PVDF piezoelectric transducer for being used for human health signal detection is fixed on by step 1
The side without nanometer rod structure with nano column array paper；
The PET double-sided adhesive of 1 μ m-thick of the side with nanometer rod structure with nano column array paper is bonded by step 2
On the inside of wrist, it to be used for pulse detection；
Step 3 selects the NC paper without any micro-structure as control.
The result shows that 4 times of signal enhancing (Fig. 5) can be made using NC nano column array paper detection wrist portion pulse
Embodiment 3:
A kind of preparation method with nano column array paper, method includes the following steps:
1) selecting aperture in 200nm, pitch of holes 300nm, film thickness is 50 μm of single-pass anodised aluminium (AAO) templates, is utilized
After acetone and ethyl alcohol clean single-pass anodic oxidation aluminium formwork, Surface Treatment with Plasma is carried out to its surface, power is
200W, processing time are 100s；
2) precursor liquid of nano column array paper, i.e. polymethyl are perfused into treated single-pass anodic oxidation aluminium formwork
Sour methyl esters (PMMA) precursor liquid (10%, w/v, chloroform), and in 70 DEG C of drying and mouldings；
3) corrode AAO template using 4% sodium hydroxide, spontaneously dry and obtain with nano-pillar battle array at room temperature after cleaning
The NC paper of column.
A kind of application with nano column array paper, there is nano column array paper to be applied to quickly detection for this, and method is such as
Under:
Step 1 handles the above-mentioned NC paper being prepared using Plasma plasma processor, is 150W's in power
Under the conditions of handle 200s；
Step 2, layout as needed are made using the mode of laser cutting and imprint print with figuratum organic glass
Chapter；
Step 3 carries out seal Imprint patterning using the mode that template imprints under 1MPa pressure condition on paper
Microfluidic channel is made, the width of microfluidic channel obtains having a plurality of microfluidic channel between 30~2000 μm
NC nano column array paper；
Lactate detection object and urea detectable substance is added dropwise in the end of different microfluidic channels in step 4 respectively, uses after dry
5% bovine serum albumin(BSA) (BSA) solution closed channel, it is spare；
The mixture of determinand lactic acid and urea is added dropwise in the sample introduction end of microfluidic channel step 5, and determinand passes through micro-
Fluid channel flows to detection zone and sufficiently reacts generation fluorescent molecule with detectable substance, and fluorescence detector is used to detect fluorescence signal.
Embodiment 4:
A kind of preparation method with nano column array paper, method includes the following steps:
1) selecting aperture in 400nm, pitch of holes 450nm, film thickness is 120 μm of single-pass anodised aluminium (AAO) templates, is utilized
After acetone and ethyl alcohol clean single-pass anodic oxidation aluminium formwork, Surface Treatment with Plasma is carried out to its surface, power is
300W, processing time are 60s；
2) precursor liquid of nano column array paper, i.e. nitrocellulose are perfused into treated single-pass anodic oxidation aluminium formwork
(NC) precursor liquid (7.5%, w/v, acetone), and in 50 DEG C of drying and mouldings, and in 80 DEG C of drying and mouldings；
3) corrode AAO template using 4% hydrofluoric acid, spontaneously dry and obtain with nano column array at room temperature after cleaning
NC paper.
A kind of application with nano column array paper, there is nano column array paper to be applied to wearable sensor, side for this
Method is as follows:
Step 1 fixes the PET double-sided adhesive of 10 μ m-thicks of the graphene electric resistance sensor for being used for human health signal detection
In the side without nanometer rod structure with nano column array paper；
The PET double-sided adhesive of 10 μ m-thicks of the side with nanometer rod structure with nano column array paper is bonded by step 2
At heart, it to be used for heartbeat detection；
Step 3 selects the NC paper without any micro-structure as control, and verifying NC nano column array paper is for heartbeat detection
Signal enhancing.
Claims (10)
1. a kind of preparation method with nano column array paper, it is characterised in that: method includes the following steps:
1) single-pass anodic oxidation aluminium formwork is selected, it is right after being cleaned using acetone and ethyl alcohol to single-pass anodic oxidation aluminium formwork
Its surface carries out Surface Treatment with Plasma；
2) precursor liquid of nano column array paper is perfused into treated single-pass anodic oxidation aluminium formwork, to precursor liquid 50~80
After DEG C drying and moulding, single-pass anodic oxidation aluminium formwork is eroded, is obtained after cleaning with nano column array paper.
2. a kind of preparation method with nano column array paper as described in claim 1, it is characterised in that: the single-pass sun
Pole alumina formwork have cellular pore structure, and the range of aperture size in hole be 20nm~400nm, pitch of holes 60nm~
450nm, hole depth are 150nm~120 μm.
3. a kind of preparation method with nano column array paper as described in claim 1, it is characterised in that: described in step 2)
The precursor liquid of nano column array paper is nitrocellulose precursor liquid, dimethyl silicone polymer precursor liquid, polystyrene precursor liquid, gathers
Methyl methacrylate precursor liquid or polyurethane precursor liquid.
4. a kind of preparation method with nano column array paper as described in claim 1, it is characterised in that: described in step 2)
During eroding single-pass anodic oxidation aluminium formwork, used corrosion reagent is hydrofluoric acid, phosphoric acid or sodium hydroxide.
5. the nano column array paper that the preparation method with nano column array paper is prepared a kind of as described in claim 1
Using, it is characterised in that: described there is nano column array paper to be applied to quickly detection or wearable sensor field.
6. a kind of application with nano column array paper as claimed in claim 5, it is characterised in that: described to be applied to quickly inspection
The method of survey is as follows:
Step 1 will have nano column array paper to carry out Surface Treatment with Plasma；
Step 2, template imprint by way of, using with figuratum seal nano column array paper have nano column array
Side produce microfluidic channel；
Step 3, the fixed inspection reagent in microfluidic channel, to detect determinand.
7. a kind of application with nano column array paper as claimed in claim 6, it is characterised in that: had described in step 2
Pattern on the seal of pattern is adjusted according to demand；Pressure limit is 0.1~1MPa in the template moulding process；Institute
The width for the microfluidic channel stated is between 30~2000 μm, quantity >=1.
8. a kind of application with nano column array paper as claimed in claim 6, it is characterised in that: inspection described in step 3
The multivariate analysis of determinand is realized in type >=a kind of reagent.
9. a kind of application with nano column array paper as claimed in claim 6, it is characterised in that: described is applied to wearing
The method of formula sensor field is as follows:
1., by wearable sensor step is fixed on the side without nanometer rod structure with nano column array paper；
2., by the side with nanometer rod structure with nano column array paper step fits in position to be detected, detected.
10. a kind of application with nano column array paper as claimed in claim 9, it is characterised in that: step is 1. described can
Wearable sensor is the piezoelectric transducer, capacitance sensor or electric resistance sensor for human health signal detection；Step
2. the laminating type for fitting in position to be detected be that use is bonded with a thickness of 1~10 μm of double faced adhesive tape, and double
The material of face adhesive tape is polyethylene terephthalate, dimethyl silicone polymer, polymethyl methacrylate or polyurethane.
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| CN111554670A (en) * | 2020-05-18 | 2020-08-18 | 济南大学 | Flexible intelligent piezoelectric sensor based on coupling of pentacene organic field effect transistor and PVDF (polyvinylidene fluoride) nano-column |
| US11996435B2 (en) | 2020-10-30 | 2024-05-28 | Taiwan Semiconductor Manufacturing Company, Ltd. | Polydimethylsiloxane antireflective layer for an image sensor |
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