CN109115282A - A kind of preparation method of Bionic flexible stress/strain sensor - Google Patents
A kind of preparation method of Bionic flexible stress/strain sensor Download PDFInfo
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- CN109115282A CN109115282A CN201811249855.2A CN201811249855A CN109115282A CN 109115282 A CN109115282 A CN 109115282A CN 201811249855 A CN201811249855 A CN 201811249855A CN 109115282 A CN109115282 A CN 109115282A
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
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- G01D21/02—Measuring two or more variables by means not covered by a single other subclass
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Abstract
The characteristics of the invention discloses a kind of preparation methods of Bionic flexible stress/strain sensor, are related to sensor field, can have both highly sensitive, big range of stretch, quick response and stability, has excellent comprehensive performance.The present invention includes: to use the patterning PDMS film for preparing using the animal skin with suitable micro-structure as template as base material, as sensing material, the two combines and flexibility stress/strain transducer is prepared the CNTs of the metal nanoparticle modification prepared using technique for atomic layer deposition.Present invention process is simple, it is at low cost, it is environmentally protective, the base material prepared replicates the micro-structure in animal skin well, sensing material has good electric conductivity and range of stretch, make the flexibility stress/strain transducer prepared that there is excellent comprehensive performance, including high sensitivity, big range of stretch, fast response time and good cyclical stability.
Description
Technical field
The present invention relates to sensor field more particularly to a kind of preparation methods of Bionic flexible stress/strain sensor.
Background technique
Flexibility stress/strain transducer is because it is in wearable device, electronic skin, human motion detection, human-computer interaction, strong
Health monitoring etc. great potential and be concerned.Traditional strain transducer is narrow (< 5%) due to its rigidity, induction range
With muting sensitivity (~2) and be unable to satisfy these application requirement.There is high sensitivity in most of stress/strain sensors
Contradictory relation between high range of stretch.Specifically, flexibility stress/strain transducer is with highly sensitive but rather low
Stretchable range, or it is opposite.Therefore, obtain have excellent comprehensive performance (as high sensitivity, big range of stretch, fastly
Response time and good stability) flexibility stress/strain transducer be an arduous challenge.
Therefore, lack a kind of flexibility stress/strain transducer in the prior art, can have both highly sensitive, big range of stretch,
The characteristics of quick response and stability, has excellent comprehensive performance.
Summary of the invention
The present invention provides a kind of preparation method of Bionic flexible stress/strain sensor, can prepare with it is highly sensitive,
The strong Bionic flexible stress/strain sensor of high stretch, quick response, stability.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of Bionic flexible stress/strain sensor, comprising:
S1, it is sticked on glass slide after the fresh animal skin with suitable micro-structure is cut clean dry as biology
Template.Animal cuticle has microstructure abundant, extremely sensitive to outside stimulus, using dynamic with suitable microstructure features
Object skin is as biological template, complex process flow needed for can be avoided production micro-structure, and preparation flow is simple, at low cost
It is honest and clean.
S2, PDMS (polydimethylsiloxane dimethyl silicone polymer) is entirely poured in animal skin surfaces,
It tears after room temperature curing, obtains patterned PDMS film.PDMS film has outstanding elasticity and excellent bio-compatible
Property.Also, compared with flat PDMS film, the patterning PDMS film with micro-structure makes electronic device have higher spirit
Sensitivity and faster response time.
S3, grow discrete distribution in CNTs (Carbon Nanotube carbon nanotube) using Atomic layer deposition method can
The metal nanoparticle of control, obtains metal NPs@CNTs composite material, and the diameter of metal nanoparticle is 5-20nm.
CNT material has fabulous toughness and electric conductivity, is able to bear higher strain, but sensitivity is not good enough, it is sluggish compared with
Greatly.However, metal nanoparticle has quite high sensitivity, but range of stretch is smaller, and stability is insufficient.
Atomic layer deposition method is a kind of with from restricted and self-saturation reaction mechanism novel thin film deposition technique,
Have the characteristics that excellent three-dimensional stickiness, the uniformity of large area and simple accurate subband structures film thickness monitoring.Atomic layer deposition
Product method prepares the controllable metal nanoparticle of discrete distribution in such a way that island is grown, and has obtained metal NPs@CNTs composite wood
Material.
Therefore, metal NPs@CNTs composite material CNT material and the respective deficiency of metal nanoparticle have been supplied into, had both
The advantages of Large strain and sensitivity.
S4, it disperses metal NPs@CNTs composite material in ethyl alcohol with the concentration of 0.5-4.5mg/mL, ultrasonic 1h is obtained
The alcohol dispersion liquid of metal NPs@CNTs.
S5, the alcohol dispersion liquid of metal NPs@CNTs is equably applied to patterned PDMS film surface, obtains metal
NPs@CNTs-PDMS film, by metal NPs@CNTs-PDMS film heating.
S6, copper foil is sticked to metal NPs@CNTs-PDMS film both ends using conductive silver glue, curing conductive elargol, and
Metal NPs@CNTs-PDMS film surface wraps up one layer of PDMS film as protective layer, obtains Bionic flexible stress/strain sensing
Device.
Further, biological template uses animal skin, including die Schwimmhaut, pigskin.
Further, PDMS is made by matrix and crosslinking agent mixing, and mixing mass ratio is matrix: crosslinking agent=10:1.
Further, in S3, CNTs is hydroxylated CNTs.
Further, in S3, metal nanoparticle includes Ir NPs, Pt NPs, W NPs.
The beneficial effects of the present invention are:
The patterning PDMS film that the present invention uses the animal skin with suitable micro-structure to prepare for template is as substrate
Material, as sensing material, the two is combined and is prepared into the CNTs of the metal nanoparticle modification prepared using technique for atomic layer deposition
To flexibility stress/strain transducer.Present invention process is simple, at low cost, environmentally protective, and the base material prepared is multiple well
The micro-structure in animal skin is made, sensing material has good electric conductivity and range of stretch, has both the toughness of PDMS film
By force, the Large strain power and stability of highly sensitive, quick response feature and CNT material, make the flexibility stress/strain prepared
Sensor has excellent comprehensive performance, steady including high sensitivity, big range of stretch, fast response time and good circulation
It is qualitative.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is flexibility stress prepared by the present invention/strain transducer preparation process schematic diagram;
Fig. 2 is the SEM figure of patterning PDMS film prepared by the present invention;
Fig. 3 is that the TEM of Ir NPs@CNTs composite material prepared by the present invention schemes;
Fig. 4 is that the XPS of Ir NPs@CNTs composite material prepared by the present invention schemes;
Fig. 5 is the dynamic response curve of flexibility stress/strain transducer prepared by the present invention;
Fig. 6 is the sensitivity curve of flexibility stress/strain transducer prepared by the present invention;
Fig. 7 is the response time curve of flexibility stress/strain transducer prepared by the present invention;
Fig. 8 is the stable circulation linearity curve of flexibility stress/strain transducer prepared by the present invention.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, With reference to embodiment to this
Invention is described in further detail.
Embodiment one:
The preparation process schematic diagram of the present embodiment as shown in Figure 1,
1) fresh die Schwimmhaut is cut, is successively cleaned with ethyl alcohol and deionized water, with being dried with nitrogen, is adhesive in two-sided
Biological template is used as on glass slide;
2) by PDMS (polydimethylsiloxane dimethyl silicone polymer) matrix and crosslinking agent with the quality of 10:1
Than being uniformly mixed, magnetic agitation 30min is placed in deflation 30min in vacuum environment and is then entirely poured in die Schwimmhaut with eliminating bubble
It tears after room temperature curing 48h, and is cut into 15 × 5 × 0.5mm in surface3Size;
3) Ir is grown on the CNTs (Carbon Nanotube carbon nanotube) that hydroxylating is handled with technique for atomic layer deposition
NPs, atomic layer deposition growth conditions are as follows: growth temperature is 300 DEG C;Presoma is respectively acetylacetone,2,4-pentanedione iridium (Ir (C5H7O2)3, source
200 DEG C of temperature) and oxygen (O2, room temperature);Deposition pulse circulation are as follows: 8s Ir (C5H7O2)3Pulse, 20s clean pulse, 8s O2Arteries and veins
Punching, 20s clean pulse;Carrier gas and purge gas are high pure nitrogen (N2, 99.999%);The partial pressure and flow of oxygen be respectively
1.1hPa and 50sccm;Growing recurring number is 200 circulations;
4) it disperses Ir NPs@CNTs composite material in ethyl alcohol with the concentration of 1.5mg/mL, ultrasonic 1h obtains Ir NPs@
The alcohol dispersion liquid of CNTs;
5) dispersant liquid drop is applied to above-mentioned patterned PDMS film surface, then heats 10min at 75 DEG C, to guarantee
The uniformity of drop coating, the step is in triplicate;
6) copper foil is sticked to above-mentioned Ir NPs@CNTs-PDMS film both ends using conductive silver glue, is heated at 75 DEG C
30min solidifies conductive silver glue, and wraps up one layer of PDMS again as protective layer on surface, that is, prepares highly sensitive high stretching model
Enclose Bionic flexible stress/strain sensor.
Embodiment two:
1) fresh die Schwimmhaut is cut, is successively cleaned with ethyl alcohol and deionized water, with being dried with nitrogen, is adhesive in two-sided
Biological template is used as on glass slide;
2) PDMS matrix and crosslinking agent are uniformly mixed with the mass ratio of 10:1, magnetic agitation 30min is placed in vacuum environment
Then middle deflation 30min is entirely poured in die Schwimmhaut surface, is torn after room temperature curing 48h to eliminate bubble, and it is cut into 15 ×
5×0.5mm3Size;
3) Pt NPs, growth conditions are as follows: growth temperature are grown on the CNTs that hydroxylating is handled with technique for atomic layer deposition
It is 300 DEG C;Presoma is respectively methyl cyclopentadienyl trimethyl platinum (PtMeCpMe3, 80 DEG C of source temperature) and oxygen (O2, room temperature);
Deposition pulse circulation are as follows: 8s PtMeCpMe3Pulse, 20s clean pulse, 8s O2Pulse, 20s clean pulse;Carrier gas and purgative gas
Body is high pure nitrogen (N2, 99.999%);The partial pressure and flow of oxygen are respectively 24.5hPa and 864sccm;Growing recurring number is
200 circulations;
4) it disperses Pt NPs@CNTs composite material in ethyl alcohol with the concentration of 2.5mg/mL, ultrasonic 1h obtains Pt NPs@
The alcohol dispersion liquid of CNTs;
5) dispersant liquid drop is applied to above-mentioned patterned PDMS film surface, then heats 10min at 75 DEG C, to guarantee
The uniformity of drop coating, the step is in triplicate;
6) copper foil is sticked to above-mentioned Pt NPs@CNTs-PDMS film both ends using conductive silver glue, is heated at 75 DEG C
30min solidifies conductive silver glue, and wraps up one layer of PDMS film again as protective layer on surface, that is, prepares highly sensitive high drawing
Stretch range Bionic flexible stress/strain sensor.
Embodiment three:
1) fresh pigskin is cut, is successively cleaned with ethyl alcohol and deionized water, with being dried with nitrogen, is adhesive in two-sided
Biological template is used as on glass slide;
2) PDMS matrix and crosslinking agent are uniformly mixed with the mass ratio of 10:1, magnetic agitation 30min is placed in vacuum environment
Then middle deflation 30min is entirely poured in pig skin surfaces, is torn after room temperature curing 48h to eliminate bubble, and it is cut into 15 ×
5×0.5mm3Size;
3) Ir NPs, growth conditions are as follows: growth temperature are grown on the CNTs that hydroxylating is handled with technique for atomic layer deposition
It is 300 DEG C;Presoma is respectively acetylacetone,2,4-pentanedione iridium (Ir (C5H7O2)3, 200 DEG C of source temperature) and oxygen (O2, room temperature);Deposition pulse is followed
Ring are as follows: 8s Ir (C5H7O2)3Pulse, 20s clean pulse, 8s O2Pulse, 20s clean pulse;Carrier gas and purge gas are high-purity
Nitrogen (N2, 99.999%);The partial pressure and flow of oxygen are respectively 1.1hPa and 50sccm;Growing recurring number is 200 circulations;
4) it disperses Ir NPs@CNTs composite material in ethyl alcohol with the concentration of 1.5mg/mL, ultrasonic 1h obtains Ir NPs@
The alcohol dispersion liquid of CNTs;
5) dispersant liquid drop is applied to above-mentioned patterned PDMS film surface, then heats 10min at 75 DEG C, to guarantee
The uniformity of drop coating, the step is in triplicate;
6) copper foil is sticked to above-mentioned Ir NPs@CNTs-PDMS film both ends using conductive silver glue, is heated at 75 DEG C
30min solidifies conductive silver glue, and wraps up one layer of PDMS film again as protective layer on surface, that is, prepares highly sensitive high drawing
Stretch range Bionic flexible stress/strain sensor.
The Bionic flexible stress/strain sensor that embodiment one is prepared is tested for the property below:
(1) pattern of base material is characterized with SEM, as shown in Fig. 2, (a) is shown with die Schwimmhaut as biological template duplicating
PDMS film on dermatoglyph;(b) structure subtleer in dermatoglyph is shown with higher amplification factor, such as is permitted
More ridge, groove and protrusions, their size range is from several hundred nanometers to several microns.(c) and (d) is respectively different amplification
Under be covered with CNTs patterning PDMS film SEM image, it is thin that image shows that CNTs is evenly distributed in patterned PDMS
The surface of film, including in groove, the top and side of ridge and protrusion.
(2) pattern of sensing material is characterized with TEM, as shown in figure 3, (a) and (b) is respectively in 200 ALD
The TEM image for the CNTs that IrNPs is modified after (Atomic layer deposition atomic layer deposition) growth circulation.On CNTs
Hydroxyl becomes the active site of Ir NPs nucleation core and island growth, and spherical Ir NPs fairly evenly divides along the outer wall of CNTs
Cloth, for the diameter of Ir NPs in the range of 5nm to 20nm, the diameter of CNTs is about 10~25nm.(c) IrNPs@CNTs's in
High-resolution TEM image shows that the lattice fringe from Ir NPs, average interplanar spacing d are 0.229nm.(d) it shows
The polycrystalline diffraction ring for the IrNPs@CNTs that selective electron diffraction (SAED) is formed, diffraction ring are corresponded respectively to from Irfcc phase
(111), (200), (220) and (311) crystal face and (002) crystal face from CNTs.
(3) it is characterized with XPS (X-ray photoelectron spectroscopy, X-ray photoelectron spectroscopic analysis)
The ingredient of sensing material come from CNTs positioned at the peak extremely strong C 1s of 284.6eV as shown in figure 4, in (a), (b) in,
Weaker bimodal peak value corresponds to Ir 4f 7/2 and 4f 5/2 at 61.5eV and 64.5eV, and spin orbit splitting can be
3.0eV。
(4) using the dynamic response curve of electrochemical workstation test sensor, as shown in figure 5, with the strain of application
Increase to 30% from 0, relative resistance change also correspondingly increases to above 600% from 0, and relative resistance change is for strain
Response is immediately, rapidly;The sensitivity of sensor is tested, as shown in fig. 6, relative resistance change-strain curve has exponent relation, with
The increase of strain, the sensitivity of the sensor constantly increases, and sensitivity is about 5.63 under the strain of 0-15%, in 15-
Sensitivity is about 35.38 under 30% strain, shows that the sensor has high sensitivity;The response time of sensor is tested,
As shown in fig. 7, the sensor has quickish response time, respectively 150ms and 100ms when applying or removing strain;
The cyclical stability of sensor is tested, as shown in figure 8, after stretching-recovery cycles more than 10000 times, the electricity of the sensor
Stream offset is only about 4.8%, and the table sensor is with good stability.
To sum up, above experimental result indicates, flexibility stress/strain transducer prepared by the present invention can have both it is highly sensitive,
The characteristics of big range of stretch, quick response and stability, there is excellent comprehensive performance.
The beneficial effects of the present invention are:
The patterning PDMS film that the present invention uses the animal skin with suitable micro-structure to prepare for template is as substrate
Material, as sensing material, the two is combined and is prepared into the CNTs of the metal nanoparticle modification prepared using technique for atomic layer deposition
To flexibility stress/strain transducer.Present invention process is simple, at low cost, environmentally protective, and the base material prepared is multiple well
The micro-structure in animal skin is made, sensing material has good electric conductivity and range of stretch, has both the toughness of PDMS film
By force, the Large strain power and stability of highly sensitive, quick response feature and CNT material, make the flexibility stress/strain prepared
Sensor has excellent comprehensive performance, steady including high sensitivity, big range of stretch, fast response time and good circulation
It is qualitative.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by those familiar with the art, all answers
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be subject to the protection scope in claims.
Claims (5)
1. a kind of preparation method of Bionic flexible stress/strain sensor characterized by comprising
S1, it is sticked on glass slide after the fresh animal skin with suitable micro-structure is cut clean dry as biological mould
Plate;
S2, PDMS (polydimethylsiloxane dimethyl silicone polymer) is entirely poured in animal skin surfaces, in room
It tears after temperature solidification, obtains patterned PDMS film;
S3, discrete be distributed controllably is grown in CNTs (Carbon Nanotube carbon nanotube) using Atomic layer deposition method
Metal nanoparticle, obtains metal NPs@CNTs composite material, and the diameter of metal nanoparticle is 5-20nm;
S4, it disperses metal NPs@CNTs composite material in ethyl alcohol with the concentration of 0.5-4.5mg/mL, obtains metal after ultrasound
The alcohol dispersion liquid of NPs@CNTs;
S5, by the alcohol dispersion liquid of metal NPs@CNTs, equably drop coating obtains metal in patterned PDMS film surface
Metal NPs@CNTs-PDMS film heating is made metal NPs@CNTs be firmly adhered to PDMS by NPs@CNTs-PDMS film
On;
S6, copper foil is sticked to metal NPs@CNTs-PDMS film both ends using conductive silver glue, curing conductive elargol, and in metal
NPs@CNTs-PDMS film surface wraps up one layer of PDMS film as protective layer, obtains Bionic flexible stress/strain sensor.
2. the method according to claim 1, wherein the biological template includes animal skin die Schwimmhaut, pigskin.
3. the method according to claim 1, wherein the PDMS is matched by matrix and crosslinking agent mixing in S2
At mixing mass ratio is matrix: crosslinking agent=10:1.
4. the method according to claim 1, wherein the CNTs is hydroxylated CNTs in S3.
5. the method according to claim 1, wherein the metal nanoparticle includes Ir NPs, Pt in S3
NPs,W NPs。
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CN110361119A (en) * | 2019-07-11 | 2019-10-22 | 南京大学 | A kind of flexibility stress sensor of composite microstructure and preparation method thereof |
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CN113831565B (en) * | 2021-10-21 | 2023-09-29 | 杭州师范大学 | High-transparency recyclable flexible multifunctional electronic skin and preparation method and application thereof |
CN115290223A (en) * | 2021-12-29 | 2022-11-04 | 太原工业学院 | Flexible force-sensitive sensing test method based on RC oscillation frequency detection |
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