CN109975365A - A kind of wearable liquid sensor and preparation method thereof - Google Patents
A kind of wearable liquid sensor and preparation method thereof Download PDFInfo
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- CN109975365A CN109975365A CN201910182638.4A CN201910182638A CN109975365A CN 109975365 A CN109975365 A CN 109975365A CN 201910182638 A CN201910182638 A CN 201910182638A CN 109975365 A CN109975365 A CN 109975365A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/06—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a liquid
Abstract
The invention belongs to technical field of electronic materials, specially a kind of wearable liquid flexible sensor and preparation method thereof.The liquid flexible sensor includes flexible base layer and induction conducing composite material layer, and flexible base layer includes cellulosic fabric, and induction conducing composite material layer is mainly homemade carbon black ink.The preparation of liquid flexible sensor is realized by the dip-coating method being simple and efficient.The liquid flexible sensor has universality, and most cellulose based fabrics are all suitable for, and has the characteristics that quick large scale preparation, low in cost, high sensitivity, operation are direct, environmentally friendly.The liquid flexible sensor all has wide application prospects in environmental monitoring and wearable field.
Description
Technical field
The invention belongs to technical field of electronic materials, and in particular to a kind of wearable liquid sensor and preparation method thereof.
Background technique
The fast development of wearable flexible electronic industry makes more and more flexible sensors, such as pressure sensor, wet
Spend sensor, temperature sensor, the extensive concern by researcher such as liquid sensor.Softness of the flexible sensor because of its own
Property can be integrated well into textile, as a kind of novel communication platform, to environmental change, human health and movement
Body-building etc. plays the function of real-time monitoring.In order to which the variation of the mechanical signal or electric signal made to environmental stimuli has
Effect monitoring, researcher develop a large amount of inductive material, such as metal oxide, silicon nanowires, water soluble polymer, carbon material etc.
Deng (X. Wang, S. H. Wang, Y. Yang and Z. L. Wang, ACS Nano, 2015,9,4553-
4562.).Wherein, carbon material, as graphene, graphene oxide, carbon nanotube etc. is mechanical because it is with unique electric property
Flexible and chemical stability is by large-scale application.Although a large number of studies show that carbon nanotube has excellent table in sensor field
It is existing, but expensive cost, the complexity of preparation process and the pollution generated during the preparation process all limit its development.Cause
This, needs to replace carbon nanotube to reduce cost with material inexpensively.In addition, traditional sensor is fixed on hard base more
On bottom, although silicon substrate or plastic-substrates also have certain flexibility, wearable comfortable, grade of breathing freely can not be met well
It is required that.And fabric has comparable flexibility, the feature of environmental protection, lower-price characteristic, and is widely used, and is optimal wearable flexibility
The substrate of sensor.In recent years, it was also taken seriously increasingly to the research of fabric sensor.Currently, researcher is to liquid sensor
Research it is less, but it is of wide application general, such as can detect water leakage situation under water-less environment, judge opposed polarity solution
In water content etc..Such a liquid flexible sensor following medical treatment and in terms of there is important application prospect,
The research and development of flexible sensor function need further to develop with integrated optimization design simultaneously, it is also noted that the sensitivities of device
Can, energy-saving consumption-reducing, process flow, cost control, environment influence etc..
Summary of the invention
Object of the present invention is to propose a kind of simple process, low-cost wearable liquid flexible sensor and its preparation side
Method.
A kind of wearable liquid flexible sensor proposed by the present invention, the liquid flexible sensor by flexible base layer and
Incude conducing composite material layer composition, the induction conducing composite material layer is coated on outside flexible base layer, and induction is conductive compound
Liquid flexible sensor is arrived by conductive silver glue connection and extraction wire in material layer both ends；Wherein:
The flexible base layer is natural cellulosic fabrics and/or regenerated cellulose fabric；
The induction conducing composite material layer material ingredient is mainly carbon black ink；In the carbon black ink, solute it is main at
It is divided into graphite, sulfuric acid, oxalic acid and glycerine；Solvent is deionized water；Wherein: the quality of graphite, sulfuric acid, oxalic acid and glycerine
Than for 5:(1-2): (1-3): (1-3)；The mass ratio of solute and solvent is 1:(5-20).
In the present invention, the natural cellulosic fabrics are cotton fabric or sodolin, and the regenerated cellulose fabric is not
Dai Er fabric or Lycoell fabrics.
A kind of preparation method of liquid flexible sensor proposed by the present invention, the specific steps are as follows:
(1) solute graphite, sulfuric acid, oxalic acid and glycerine are uniformly mixed, obtains mixture；
(2) solvent deionized water dissolution is poured into the mixture of step (1), magnetic agitation obtains uniform carbon black ink, cold
It hides spare；
(3) flexible base layer is cleaned by ultrasonic, is then immersed in the carbon black ink that step (2) obtains, then in an oven,
Drying；
(4) step (3) are repeated several times, the induction conduction for obtaining being coated on the outer different carbon black ink depositions of flexible base layer is multiple
Condensation material layer；
(5) it is arrived in the induction conducing composite material layer both ends that step (4) obtains by conductive silver glue connection and extraction wire
Liquid flexible sensor.
In the present invention, graphite, sulfuric acid, oxalic acid and glycerine mass ratio be 5:(1-2): (1-3): (1-3)；Solute with it is molten
The mass ratio of agent is 1:(5-20).
In the present invention, in step (2), the speed for controlling magnetic agitation is 1000-1500 revs/min, is carried out at room temperature；
Refrigerated condition is 2-4 DEG C, and cold preservation time is 24-48 hours.
In the present invention, in step (3), flexible base layer is cleaned by ultrasonic 2-3 times, and being immersed in the time in carbon black ink is 3-10
Minute, oven temperature is 100 DEG C -150 DEG C, and criteria thus the drying time is 5-10 minutes.
In the present invention, in step (4), repeating step (3) number is 1-7 times.
A kind of purposes of wearable liquid flexible sensor proposed by the present invention, liquid flexible sensor is for monitoring in real time
Fluid seepage situation judges solution concentration or real-time monitoring sweat discharge situation.
Flexible sensor of the invention, has the function of liquid sensor.
Above-mentioned flexible sensor is tested as liquid sensor, and method is: testing liquid flexible sensor respectively in drying
Under state and it is immersed in aqueous solution, the resistance variations in the simulation human sweat of water/alcohol mixed solution and different pH, and not
With under water temperature to the influence of resistance variations.Calculation of Sensitivity formula are as follows:R rel =△R/R 0 × 100%, whereinR rel It is opposite
Increased resistance value, i.e. sensitivity, △RFor the changing value of resistance,R 0 For initial resistivity value.
Wherein, the length-width ratio of liquid flexible sensor is (5-10): 1, water/alcohol mixed solution volume ratio is 1:(0-
100) pH value for, simulating human sweat is respectively 4.7,7.0 and 8.8, and water temperature is respectively 10 DEG C, 30 DEG C, 50 DEG C and 70 DEG C.In water
In solution, relative resistance change value is obviously increased, and when being restored to drying regime, relative resistance change value goes to zero, therefore can be with
To water-less environment carry out real time monitoring and it is reusable.In water/alcohol mixed solution of different volumes ratio, as ethyl alcohol contains
The increase of amount, relative resistance change value reduce, and when being restored to drying regime, relative resistance change value goes to zero, therefore can be used for
Detect concentration of alcohol.In the simulation human sweat of different pH, relative resistance change value significantly decreases, dry when being restored to
Dry state, relative resistance change value almost go to zero, therefore can be used for detecting sweat discharge situation.Under different water temperatures, with
The raising of temperature, relative resistance change value reduces, therefore can be used for measuring different liquids temperature.
The beneficial effects of the present invention are:
(1) the liquid flexible sensor has universality, and most cellulosic fabrics are all suitable for.
(2) the liquid flexible sensor has that quick large scale preparation, low in cost, sensitivity is high, operation is direct, environmentally friendly
The features such as.
(3) the liquid flexible sensor all has wide application prospects in environmental monitoring, human motion and wearable field.
Detailed description of the invention
Fig. 1 is the preparation flow figure of liquid flexible sensor.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is explained in further detail.Solute uses the mass ratio of graphite, sulfuric acid, oxalic acid and glycerine for 5:(1-2): (1-3): (1-
3)；The mass ratio of solute and solvent is 1:(5-20)；
Embodiment 1
(1) graphite, sulfuric acid, oxalic acid and glycerine are mixed with mass ratio for the ratio uniform of 5:1:1:1, obtains mixture；
(2) will be mixed through the mixture that step (1) obtains with solvent deionized water with mass ratio 1:5, and at room temperature with
1000 revs/min of rate after mixing evenly, obtains carbon black ink, is placed in 2 DEG C of refrigerator and refrigerates 24 hours.
(3) it will be immersed in the carbon black ink in step (2) after five minutes with ultrasonic cleaning 3 times cotton fabrics, taking-up is placed in
In 120 DEG C of baking oven, drying 10 minutes；
(4) step (3) are repeated 5 times, carbon black ink is coated on cotton fabric, finally obtaining carbon black ink deposition is 4.58
mg·cm-2Induction conducing composite material layer；
(5) liquid flexibility is obtained by conductive silver glue connection and extraction wire at obtained induction conducing composite material layer both ends
Sensor；
The liquid sensing capabilities for the flexible sensor being prepared are tested, it is found that the sensitivity for liquid water is 4800%, it is different
The sensitivity of water temperature is 4000%-4800%, and water/alcohol mixeding liquid body sensitivity of different volumes ratio is 900%-4800%, no
Sensitivity with the simulation human sweat of pH value is -90%-(-91%), and the liquid flexible sensor has very high repeat
Property.
Embodiment 2
(1) graphite, sulfuric acid, oxalic acid and glycerine are mixed with mass ratio for the ratio uniform of 5:2:2:2, obtains mixture；
(2) will be mixed through the mixture that step (1) obtains with solvent deionized water with mass ratio 1:10, and at room temperature with
1000 revs/min of rate after mixing evenly, obtains carbon black ink, is placed in 2 DEG C of refrigerator and refrigerates 24 hours.
(3) it will be immersed in the carbon black ink in step (2) after five minutes with ultrasonic cleaning 3 times cotton fabrics, taking-up is placed in
In 120 DEG C of baking oven, drying 5 minutes；
(4) step (3) are repeated 3 times, carbon black ink is coated on cotton fabric, finally obtaining carbon black ink deposition is 2.67
mg·cm-2Induction conducing composite material layer；
(5) liquid flexibility is obtained by conductive silver glue connection and extraction wire at obtained induction conducing composite material layer both ends
Sensor；
The liquid sensing capabilities for the flexible sensor being prepared are tested, it is found that the sensitivity for liquid water is 4500%, it is different
The sensitivity of water temperature is 3800%-4500%, and water/alcohol mixeding liquid body sensitivity of different volumes ratio is 600%-4500%, no
Sensitivity with the simulation human sweat of pH value is -82%-(-90%), and the liquid flexible sensor has very high repeat
Property.
Embodiment 3
(1) graphite, sulfuric acid, oxalic acid and glycerine are mixed with mass ratio for the ratio uniform of 5:2:3:3, obtains mixture；
(2) will be mixed through the mixture that step (1) obtains with solvent deionized water with mass ratio 1:15, and at room temperature with
1000 revs/min of rate after mixing evenly, obtains carbon black ink, is placed in 4 DEG C of refrigerator and refrigerates 48 hours.
(3) it will be immersed in the carbon black ink in step (2) after five minutes, taken out with ultrasonic cleaning 2 times modal fabrics
It is placed in drying 5 minutes in 130 DEG C of baking oven；
(4) step (3) are repeated 1 times, carbon black ink is coated on cotton fabric, finally obtaining carbon black ink deposition is 1.07
mg·cm-2Induction conductive material layer；
(5) liquid flexible sensor is obtained by conductive silver glue connection and extraction wire at obtained induction conductive layer both ends；
The liquid sensing capabilities for the flexible sensor being prepared are tested, it is found that the sensitivity for liquid water is 2500%, it is different
The sensitivity of water temperature is 1800%-2500%, and water/alcohol mixeding liquid body sensitivity of different volumes ratio is 700%-2500%, no
Sensitivity with the simulation human sweat of pH value is -69%-(-84%), and the liquid flexible sensor has very high repeat
Property.
Embodiment 4
(1) graphite, sulfuric acid, oxalic acid and glycerine are mixed with mass ratio for the ratio uniform of 5:2:2:3, obtains mixture；
(2) will be mixed through the mixture that step (1) obtains with solvent deionized water with mass ratio 1:15, and at room temperature with
1500 revs/min of rate after mixing evenly, obtains carbon black ink, is placed in 4 DEG C of refrigerator and refrigerates 48 hours.
(3) it will be immersed in the carbon black ink in step (2) after 7 minutes with ultrasonic cleaning 3 times sodolins, taking-up is set
In 150 DEG C of baking oven, drying 10 minutes；
(4) step (3) are repeated 7 times, carbon black ink is coated on cotton fabric, finally obtaining carbon black ink deposition is 8.36
mg·cm-2Induction conductive material layer；
(5) liquid flexible sensor is obtained by conductive silver glue connection and extraction wire at obtained induction conductive layer both ends；
The liquid sensing capabilities for the flexible sensor being prepared are tested, it is found that the sensitivity for liquid water is 3700%, it is different
The sensitivity of water temperature is 3200%-3700%, and water/alcohol mixeding liquid body sensitivity of different volumes ratio is 800%-3700%, no
Sensitivity with the simulation human sweat of pH value is -80%-(-87%), and the liquid flexible sensor has very high repeat
Property.
Embodiment 5
(1) graphite, sulfuric acid, oxalic acid and glycerine are mixed with mass ratio for the ratio uniform of 5:2:3:2, obtains mixture；
(2) it will be mixed through the mixture that step (1) obtains with deionized water with mass ratio 1:20, and at room temperature with 1200
Rev/min rate after mixing evenly, obtain carbon black ink, be placed in 4 DEG C of refrigerator and refrigerate 48 hours.
(3) it will be taken out after ten minutes in the carbon black ink being immersed in step (2) with ultrasonic cleaning 2 times Lycoell fabrics
It is placed in drying 5 minutes in 120 DEG C of baking oven；
(4) step (3) are repeated 4 times, carbon black ink is coated on cotton fabric, finally obtaining carbon black ink deposition is 3.69
mg·cm-2Induction conducing composite material layer；
(5) liquid flexibility is obtained by conductive silver glue connection and extraction wire at obtained induction conducing composite material layer both ends
Sensor；
The liquid sensing capabilities for the flexible sensor being prepared are tested, it is found that the sensitivity for liquid water is 4000%, it is different
The sensitivity of water temperature is 3200%-4000%, and water/alcohol mixeding liquid body sensitivity of different volumes ratio is 1000%-4000%, no
Sensitivity with the simulation human sweat of pH value is -76%-(-85%), and the liquid flexible sensor has very high repeat
Property.
Embodiment 6
(1) graphite, sulfuric acid, oxalic acid and glycerine are mixed with mass ratio for the ratio uniform of 5:2:3:2, obtains mixture；
(2) it will be mixed through the mixture that step (1) obtains with deionized water with mass ratio 1:20, and at room temperature with 1400
Rev/min rate after mixing evenly, obtain carbon black ink, be placed in 3 DEG C of refrigerator and refrigerate 36 hours.
(3) it will be immersed in the carbon black ink in step (2) after ten minutes, taken with ultrasonic cleaning 2 times polylactic acid fabrics
It is placed in 120 DEG C of baking oven out, drying 5 minutes；
(4) step (3) are repeated 5 times, carbon black ink is coated on cotton fabric, finally obtaining carbon black ink deposition is 0.72
mg·cm-2Induction conductive material layer；
(5) liquid flexible sensor is obtained by conductive silver glue connection and extraction wire at obtained induction conductive layer both ends；
The liquid sensing capabilities for the flexible sensor being prepared are tested, it is found that the sensitivity for liquid water is 1.5%, it is different
The sensitivity of water temperature is 1.2%-1.5%, and water/alcohol mixeding liquid body sensitivity of different volumes ratio is 0.9%-1.5%, different pH
The sensitivity of the simulation human sweat of value is -1%-(-2%), and the repeatability of the liquid flexible sensor is poor.
Embodiment 7
(1) graphite, sulfuric acid, oxalic acid and glycerine are mixed with mass ratio for the ratio uniform of 5:4:4:2, obtains mixture；
(2) will the mixture that obtained through step (1) mixed with solvent deionized water with mass ratio 1:10 and at room temperature with
1300 revs/min of rate after mixing evenly, obtains carbon black ink, is placed in 3 DEG C of refrigerator and refrigerates 36 hours.
(3) it will be taken after ten minutes in the carbon black ink being immersed in step (2) with ultrasonic cleaning 2 times glass fabrics
It is placed in drying 5 minutes in 120 DEG C of baking oven out；
(4) step (3) are repeated 7 times, carbon black ink is coated on cotton fabric, finally obtaining carbon black ink deposition is 0.42mg
cm-2Induction conductive material layer；
(5) liquid flexible sensor is obtained by conductive silver glue connection and extraction wire at obtained induction conductive layer both ends；
The liquid sensing capabilities for the flexible sensor being prepared are tested, it is found that the sensitivity for liquid water is 0.9%, it is different
The sensitivity of water temperature is 0.8%-0.9%, and water/alcohol mixeding liquid body sensitivity of different volumes ratio is 0.1%-0.9%, different pH
The sensitivity of the simulation human sweat of value is -0.5%-(-0.7%), and the repeatability of the liquid flexible sensor is poor.
Embodiment 8
(1) graphite, sulfuric acid, oxalic acid and glycerine are mixed with mass ratio for the ratio uniform of 0:3:3:5, obtains mixture；
(2) it will be mixed through the mixture that step 1) obtains with solvent deionized water with mass ratio 1:5, and at room temperature with 1000
Rev/min rate after mixing evenly, obtain ink, be placed in 2 DEG C of refrigerator and refrigerate 24 hours.
(3) it will be immersed in the carbon black ink in step (2) after five minutes with ultrasonic cleaning 3 times cotton fabrics, taking-up is placed in
In 120 DEG C of baking oven, drying 10 minutes；
(4) step (3) are repeated 5 times, carbon black ink is coated on cotton fabric, finally obtaining carbon black ink deposition is 1.39
mg·cm-2Induction conductive material layer；
(5) liquid flexible sensor is obtained by conductive silver glue connection and extraction wire at obtained induction conductive layer both ends；
The liquid sensing capabilities for the flexible sensor being prepared are tested, it is found that the sensitivity for liquid water is 0.1%, it is different
The sensitivity of water temperature is 0.09%-0.1%, and water/alcohol mixeding liquid body sensitivity of different volumes ratio is 0.01%-0.1%, different
The sensitivity of the simulation human sweat of pH value is -0.01%-(-0.08%).
Claims (8)
1. a kind of wearable liquid flexible sensor, which is characterized in that the liquid flexible sensor is by flexible base layer and sense
Conducing composite material layer is answered to form, the induction conducing composite material layer is coated on outside flexible base layer, incudes conductive composite wood
Liquid flexible sensor is arrived by conductive silver glue connection and extraction wire in bed of material both ends；Wherein:
The flexible base layer is natural cellulosic fabrics and/or regenerated cellulose fabric；
The induction conducing composite material layer material ingredient is mainly carbon black ink；In the carbon black ink, solute it is main at
It is divided into graphite, sulfuric acid, oxalic acid and glycerine；Solvent is deionized water；Wherein, the mass ratio of graphite, sulfuric acid, oxalic acid and glycerine
For 5:(1-2): (1-3): (1-3)；The mass ratio of solute and solvent is 1:(5-20).
2. wearable liquid flexible sensor according to claim 1, which is characterized in that the natural cellulosic fabrics are
Cotton fabric or sodolin, the regenerated cellulose fabric are modal fabric or Lycoell fabrics.
3. a kind of preparation method of liquid flexible sensor as described in claim 1, which is characterized in that specific step is as follows:
(1) solute graphite, sulfuric acid, oxalic acid and glycerine are uniformly mixed, obtains mixture；
(2) solvent deionized water dissolution is poured into the mixture of step (1), magnetic agitation obtains uniform carbon black ink, cold
It hides spare；
(3) flexible base layer is cleaned by ultrasonic, is then immersed in the carbon black ink that step (2) obtains, then in an oven, dried
It is dry；
(4) step (3) are repeated several times, the induction conduction for obtaining being coated on the outer different carbon black ink depositions of flexible base layer is multiple
Condensation material layer；
(5) it is arrived in the induction conducing composite material layer both ends that step (4) obtains by conductive silver glue connection and extraction wire
Liquid flexible sensor.
4. preparation method according to claim 3, which is characterized in that graphite, sulfuric acid, oxalic acid and glycerine mass ratio be
5:(1-2): (1-3): (1-3)；The mass ratio of solute and solvent is 1:(5-20).
5. preparation method according to claim 3, which is characterized in that in step (2), the speed for controlling magnetic agitation is
It 1000-1500 revs/min, carries out at room temperature；Refrigerated condition is 2-4 DEG C, and cold preservation time is 24-48 hours.
6. preparation method according to claim 3, which is characterized in that in step (3), flexible base layer is cleaned by ultrasonic 2-3
Secondary, being immersed in the time in carbon black ink is 3-10 minutes, and oven temperature is 100 DEG C -150 DEG C, and criteria thus the drying time is 5-10 minutes.
7. preparation method according to claim 3, which is characterized in that in step (4), repeating step (3) number is 1-7
It is secondary.
8. a kind of purposes of wearable liquid flexible sensor as described in claim 1, which is characterized in that liquid flexible sensing
Device judges solution concentration or real-time monitoring sweat discharge situation for monitoring fluid seepage situation in real time.
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Application publication date: 20190705 |