CN108801513A - A kind of flexibility stress sensor and preparation method thereof fettering conduction liquid film based on nano wire - Google Patents
A kind of flexibility stress sensor and preparation method thereof fettering conduction liquid film based on nano wire Download PDFInfo
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- CN108801513A CN108801513A CN201710312772.2A CN201710312772A CN108801513A CN 108801513 A CN108801513 A CN 108801513A CN 201710312772 A CN201710312772 A CN 201710312772A CN 108801513 A CN108801513 A CN 108801513A
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- liquid film
- stress sensor
- nano wire
- fettering
- nano
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
Abstract
The invention discloses a kind of flexibility stress sensors and preparation method thereof fettering conduction liquid film based on nano wire, the flexibility stress sensor includes the silicone rubber substrate that surface has cluster nano thread structure, and ionic liquid is fettered in cluster nano thread structure as conductive liquid film;The length of nano wire is 300nm-6 μm in the cluster nano thread structure, a diameter of 30-400nm.The flexibility stress sensor of the present invention has the following advantages:Due to ionic liquid in drawing process without abrasion, there is superelevation fatigue performance:By repeatedly stretching experiment of more than 22500 stretch ratios from 0% to 100%, sensor remains to keep superperformance;Big range of stretch, maximum can detect 200% deformation;Minimum minimum stretch detects deformation quantity, and minimum can detect 0.3% deformation;Preparation flow is simple, at low cost.
Description
Technical field
The present invention relates to flexibility stress sensor preparation processes, and in particular to a kind of to fetter conduction liquid film based on nano wire
Flexibility stress sensor and preparation method thereof.
Background technology
With the fast development of artificial intelligence technology, requirement of the mankind to man-machine communication increasingly improves, and there is apery class to touch
The artificial flexible electronic device of the perceptional functions such as feel, smell, the sense of hearing, vision occupies extremely important position in this revolution
It sets.It is widely answered since flexibility stress sensor makes it have in medical treatment & health field in the advantage of detection pulse, heartbeat etc.
With foreground, become the core composition of artificial flexible electronic device.Currently, the main way of manufacture pulling force sensor is to stretch
The deformation of sensor is converted in journey the variation of resistance value.One of which method is to fill conductive materials in the polymer, example
Such as Ag nano wires, carbon dust and metallic particles, to obtain conductive elastomer.Another method is that face is embedding on a flexible substrate
Enter or the structure of stacked conductive, for example, the single-walled carbon nanotube of proper alignment, conducting polymer and carbon nanotube compound and
Metal film etc., and then obtain pulling force sensor with multi-layer structure.However there are two types of sensors with auxiliary electrode has in use
Distinct disadvantage:Fatigue durability is poor, electric signal is unstable, this has become the huge problem for restricting sensors with auxiliary electrode industrialization.It grinds
Study carefully and shows to generate both disadvantage reasons and be respectively:Solid conducting layer stretches, continuous in contraction cyclic process, and cracking is
It is expendable;Solid conduction substance can constantly be worn during rubs mutually.
Invention content
Present invention aims at:A kind of flexibility stress sensor and its preparation being fettered conduction liquid film based on nano wire is provided
Method, the sensor have superelevation fatigue performance, and this method preparation process is simple, and it is resistance to tired to be obviously improved flexibility stress sensor
Lao Xing.
In order to achieve the above objectives, present invention employs the following technical solutions:
The present invention is by the way that ionic liquid to be strapped in cluster nano thread structure, using the ionic liquid of liquid as conduction
Substance improves the fatigue performance of sensor.
The specific technical solution of the present invention is as follows:
A kind of flexibility stress sensor fettering conduction liquid film based on nano wire, the flexibility stress sensor includes surface
Silicone rubber substrate with cluster nano thread structure fetters ionic liquid as conductive liquid film in cluster nano thread structure;Institute
The length for stating nano wire in cluster nano thread structure is 300nm-6 μm, a diameter of 30-400nm.
It is described the present invention also provides a kind of preparation method for the flexibility stress sensor fettering conduction liquid film based on nano wire
Preparation method includes the following steps:
1) liquid prepolymer mixed liquor is prepared:Silicone oligomer, crosslinking agent and modifying agent are mixed;
2) silicone rubber substrate with cluster nano thread structure is prepared:Liquid prepolymer mixed liquor obtained by step 1) is added dropwise
Onto the template with nano-pore, polymerization crosslinking curing reaction is carried out, 2-20 in 70-90 DEG C of corrosive liquid is then immersed in
Hour is to remove removing template;
3) ionic liquid hybrid solution is configured:By ion liquid dissolving at low boiling point volatile organic solvent (such as ethyl alcohol)
In;
4) homogeneous conductive liquid film is prepared:In the step 3) that determined volume is added dropwise in the silicone rubber substrate surface that step 2) obtains
The ionic liquid hybrid solution of configuration;
5) the flexibility stress sensor that conduction liquid film is fettered based on nano wire is formed:The surface obtained in step 4) is added dropwise
The silicone rubber substrate of ionic liquid hybrid solution, which is stored at room temperature, makes low boiling point volatile organic solvent volatilize.
Preferably, the silicone oligomer is the dimethyl silicone polymer for the end-vinyl that the degree of polymerization is 10-200;Institute
State the dimethyl silicone polymer that crosslinking agent is terminal methyl;The modifying agent is the ethyoxyl polyethyleneimine of a concentration of 35~40wt%
Amine aqueous solution.
Preferably, the silicone oligomer:Crosslinking agent:The ratio of modifying agent is (5-10g):(0.5-1g):(10-40μ
L)。
Preferably, the template with nano-pore is in anodic oxidation aluminium formwork, porous silicon template and PET plastic template
One kind, the depth of the nano-pore is 300nm-6 μm, aperture 30-400nm.
Preferably, a concentration of 0.001mg/mL-0.1mg/mL of the ionic liquid hybrid solution;The ionic liquid is
Hydrophobic ionic liquid.
Preferably, the hydrophobic ionic liquid be 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, 1- oneself
Base -3- methyl imidazolium tetrafluoroborates, two (trimethyl fluoride sulfonyl) inferior amine salt of 1- octyl -3- methylimidazoles and 1- hexyl -3- first
One kind in base limidazolium hexafluorophosphate.
Preferably, the step 4) determined volume is 25-250 μ L.
Method according to the present invention, wherein step 5) the preferred volatilization time is 0.5-2 hours, preferable temperature
It is 10-70 DEG C.
By the present invention in that the nano thread structure of cluster is introduced in silicone rubber substrate with template, with its fetter liquid from
Sub- liquid greatly improves the fatigue performance of flexibility stress sensor as conductive layer.Sensor of the invention requires table
Face ionic liquid conductive layer is uniformly distributed, i.e., the ethanol solution of ionic liquid will reach super close (contact angle in substrate surface<5 °),
To improve sensor stability.The flexibility stress sensor of the present invention has the following advantages:Since ionic liquid is in drawing process
Middle no abrasion has superelevation fatigue performance:It is real by repeatedly stretching of more than 22500 stretch ratios from 0% to 100%
It tests, sensor remains to keep superperformance;Big range of stretch, maximum can detect 200% deformation;Minimum minimum stretch is visited
Deformation quantity is surveyed, minimum can detect 0.3% deformation;Preparation flow is simple, at low cost.
Description of the drawings
Fig. 1 is the surface texture micro image of the flexibility stress sensor of the present invention;
Fig. 2 is that mixed solution is being contact angle in 4 μm of silicone rubber substrate with nanowire length in embodiment 1;
Fig. 3 is influence of the nanowire length of substrate prepared by embodiment 1 to mixed solution contact angle;
Fig. 4 is influence of the strain gauge surface difference nanowire length of the preparation of embodiment 1 to sensor performance;
Fig. 5 is the strain gauge maximum tension of the preparation of embodiment 1 with nanowire length situation of change;
Fig. 6 is the nanowire length for preparing of embodiment 1 sensor gradient pulled out condition when being 4 μm;
Fig. 7 is the nanowire length for preparing of embodiment 1 sensor detection minimum stretch when being 4 μm;
Fig. 8 is the nanowire length for preparing of embodiment 1 sensor fatigue durability test case when being 4 μm;
Fig. 9 is that embodiment 1 prepares different stretch ratio lower sensor surface topography when nanowire length is 4 μm.
Specific implementation mode
Technical solution of the present invention is further described with reference to embodiment.
Embodiment 1
By the present invention in that with anodic oxidation aluminium formwork (depth of nano-pore is 300nm-6 μm, aperture 30-400nm)
The nano thread structure that cluster is introduced in silicone rubber substrate makes it fetter the ionic liquid of liquid as conductive liquid film layer, thus
Achieve the purpose that significantly improve sensor fatigue durability.It is as follows:
(1) silicone oligomer 10g, crosslinking agent 1g and 30 μ L of modifying agent are taken, is uniformly mixed, the organosilicon is oligomeric
Object is the dimethyl silicone polymer for the end-vinyl that the degree of polymerization is 10-200;The crosslinking agent is the polydimethylsiloxanes of terminal methyl
Alkane;The modifying agent is the ethyoxyl aq. polyethyleneimine of a concentration of 35~40wt%;
(2) take a small amount of gained mixture to be added drop-wise on anodic oxidation aluminium formwork, stand half an hour, at a temperature of 110 DEG C into
Then row polymerization crosslinking curing reaction 4 hours is immersed in 70-90 DEG C of corrosive liquid 2-4 hours to remove removing template, is obtained
Surface has the silicone rubber substrate of cluster nano thread structure;
(3) it takes 0.50mg 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimide salt to be dissolved in 50mL ethyl alcohol, shakes up
Obtain mixed solution;
(4) it takes the 25 above-mentioned mixed solutions of μ L to be added drop-wise in above-mentioned silicone rubber substrate, sprawls into uniform liquid film rapidly, (as schemed
2);
(5) above-mentioned material is stood to 1.5 hours at room temperature, after ethyl alcohol volatilization after substrate surface formed one layer uniformly from
Sub- liquid film successfully prepares sensor of the present invention (such as Fig. 1), it will be seen from figure 1 that the flexibility stress sensor includes
Surface has the silicone rubber substrate of cluster nano thread structure, and ionic liquid is fettered in cluster nano thread structure as conduction liquid
Film;The length of nano wire is 300nm-6 μm in the cluster nano thread structure, a diameter of 30-400nm.
Fig. 2 is in the silicone rubber substrate for being 4 μm with nanowire length prepared by the method for mixed solution in embodiment 1
Contact angle.Fig. 3 is influence of the nanowire length for the substrate that in embodiment 1 prepared by method to mixed solution contact angle.Fig. 4 is
Influence of the strain gauge surface difference nanowire length that in embodiment 1 prepared by method to sensor performance.Fig. 5 is embodiment
The strain gauge maximum tension that in 1 prepared by method is with nanowire length situation of change.Fig. 6 is that in embodiment 1 prepared by method
Sensor gradient pulled out condition when nanowire length is 4 μm.Fig. 7 is nanowire length that in embodiment 1 prepared by method when being 4 μm
Sensor detects minimum stretch.Fig. 8 be nanowire length that in embodiment 1 prepared by method when being 4 μm sensor fatigue durability survey
Try situation.Fig. 9 is that method prepares different stretch ratio (0%-200%) lower sensor when nanowire length is 4 μm in embodiment 1
Surface topography.From above each figure as can be seen that the said goods significantly improve the fatigue durability of flexibility stress sensor, and have
There are big detection range of stretch, the detection of minimum minimum stretch.
Embodiment 2
By the present invention in that with porous silicon template (depth of nano-pore is 300nm-6 μm, aperture 30-400nm) in silicon
The nano thread structure that cluster is introduced in rubber substrate makes the ionic liquid of its constraint liquid as conductive layer, apparent to reach
Improve the purpose of sensor fatigue durability.It is as follows:
(1) silicone oligomer 10g, crosslinking agent 0.5g and 40 μ L of modifying agent are taken, is uniformly mixed, the organosilicon is low
Polymers is the dimethyl silicone polymer for the end-vinyl that the degree of polymerization is 10-200;The crosslinking agent is the poly dimethyl silicon of terminal methyl
Oxygen alkane;The modifying agent is the ethyoxyl aq. polyethyleneimine of a concentration of 35~40wt%;
(2) it takes a small amount of gained mixture to be added drop-wise in porous silicon template, stands half an hour, gathered at a temperature of 110 DEG C
Cross-linking and curing reaction 4 hours is closed, 2-4 hours is then immersed in 70-90 DEG C of corrosive liquid to remove removing template, obtains surface
Silicone rubber substrate with cluster nano thread structure;
(3) it takes 0.05mg 1- hexyl -3- methyl imidazolium tetrafluoroborates to be dissolved in 50mL ethyl alcohol, shakes up and mixed
Solution;
(4) it takes the 250 above-mentioned mixed solutions of μ L to be added drop-wise in above-mentioned silicone rubber substrate, sprawls into uniform liquid film rapidly, (as schemed
2);
(5) above-mentioned material is stood to 0.5 hour at room temperature, after ethyl alcohol volatilization after substrate surface formed one layer uniformly from
Sub- liquid film successfully prepares sensor of the present invention (such as Fig. 1), it will be seen from figure 1 that the flexibility stress sensor includes
Surface has the silicone rubber substrate of cluster nano thread structure, and ionic liquid is fettered in cluster nano thread structure as conduction liquid
Film;The length of nano wire is 300nm-6 μm in the cluster nano thread structure, a diameter of 30-400nm.
Embodiment 3
By the present invention in that with anodic oxidation aluminium formwork (depth of nano-pore is 300nm-6 μm, aperture 30-400nm)
The nano thread structure that cluster is introduced in silicone rubber substrate makes it fetter the ionic liquid of liquid as conductive layer, to reach
Significantly improve the purpose of sensor fatigue durability.It is as follows:
(1) silicone oligomer 5g, crosslinking agent 1g and 20 μ L of modifying agent are taken, is uniformly mixed, the organosilicon is oligomeric
Object is the dimethyl silicone polymer for the end-vinyl that the degree of polymerization is 10-200;The crosslinking agent is the polydimethylsiloxanes of terminal methyl
Alkane;The modifying agent is the ethyoxyl aq. polyethyleneimine of a concentration of 35~40wt%;
(2) take a small amount of gained mixture to be added drop-wise on anodic oxidation aluminium formwork, stand half an hour, at a temperature of 110 DEG C into
Then row polymerization crosslinking curing reaction 4 hours is immersed in 70-90 DEG C of corrosive liquid 2-4 hours to remove removing template, is obtained
Surface has the silicone rubber substrate of cluster nano thread structure;
(3) two (trimethyl fluoride sulfonyl) inferior amine salt of 0.25mg 1- octyl -3- methylimidazoles is taken to be dissolved in 50mL ethyl alcohol,
It shakes up to obtain mixed solution;
(4) it takes the 50 above-mentioned mixed solutions of μ L to be added drop-wise in above-mentioned silicone rubber substrate, sprawls into uniform liquid film rapidly, (as schemed
2);
(5) above-mentioned material is stood to 1 hour at room temperature, substrate surface forms one layer of uniform ion after ethyl alcohol volatilization
Liquid film successfully prepares sensor of the present invention (such as Fig. 1), it will be seen from figure 1 that the flexibility stress sensor includes table
Face has the silicone rubber substrate of cluster nano thread structure, and ionic liquid is fettered in cluster nano thread structure as conductive liquid film;
The length of nano wire is 300nm-6 μm in the cluster nano thread structure, a diameter of 30-400nm.
Embodiment 4
By the present invention in that introducing the nano thread structure of cluster in silicone rubber substrate with PET plastic template, make its constraint
The ionic liquid of liquid is as conductive layer, to achieve the purpose that significantly improve sensor fatigue durability.It is as follows:
(1) silicone oligomer 5g, crosslinking agent 0.5g and 10 μ L of modifying agent are taken, is uniformly mixed, the organosilicon is low
Polymers is the dimethyl silicone polymer for the end-vinyl that the degree of polymerization is 10-200;The crosslinking agent is the poly dimethyl silicon of terminal methyl
Oxygen alkane;The modifying agent is the ethyoxyl aq. polyethyleneimine of a concentration of 35~40wt%;
(2) it takes a small amount of gained mixture to be added drop-wise in PET plastic template, stands half an hour, gathered at a temperature of 110 DEG C
Cross-linking and curing reaction 4 hours is closed, 2-4 hours is then immersed in 70-90 DEG C of corrosive liquid to remove removing template, obtains surface
Silicone rubber substrate with cluster nano thread structure;
(3) it takes 1.00mg 1- hexyl -3- methylimidazole hexafluorophosphates to be dissolved in 50mL ethyl alcohol, shakes up and mixed
Solution;
(4) it takes the 250 above-mentioned mixed solutions of μ L to be added drop-wise in above-mentioned silicone rubber substrate, sprawls into uniform liquid film rapidly, (as schemed
2);
(5) above-mentioned material is stood to 2 hours at room temperature, substrate surface forms one layer of uniform ion after ethyl alcohol volatilization
Liquid film successfully prepares sensor of the present invention (such as Fig. 1), it will be seen from figure 1 that the flexibility stress sensor includes table
Face has the silicone rubber substrate of cluster nano thread structure, and ionic liquid is fettered in cluster nano thread structure as conductive liquid film;
The length of nano wire is 300nm-6 μm in the cluster nano thread structure, a diameter of 30-400nm.
Certainly, the present invention can also there are many embodiments, without deviating from the spirit and substance of the present invention, are familiar with
Those skilled in the art can disclosure according to the present invention make various corresponding change and deformations, but these it is corresponding change and
Deformation should all belong to the scope of the claims of the present invention.
Claims (9)
1. a kind of flexibility stress sensor fettering conduction liquid film based on nano wire, which is characterized in that the flexibility stress sensing
Device includes the silicone rubber substrate that surface has cluster nano thread structure, and constraint ionic liquid, which is used as, in cluster nano thread structure leads
Electro-hydraulic film;The length of nano wire is 300nm-6 μm in the cluster nano thread structure, a diameter of 30-400nm.
2. a kind of preparation method of flexibility stress sensor fettering conduction liquid film based on nano wire described in claim 1, institute
Preparation method is stated to include the following steps:
1) liquid prepolymer mixed liquor is prepared:Silicone oligomer, crosslinking agent and modifying agent are mixed;
2) silicone rubber substrate with cluster nano thread structure is prepared:Liquid prepolymer mixed liquor obtained by step 1) is added drop-wise to tool
Have in the template of nano-pore, carries out polymerization crosslinking curing reaction, be then immersed in 70-90 DEG C of corrosive liquid 2-20 hours
To remove removing template;
3) ionic liquid hybrid solution is configured:By ion liquid dissolving in low boiling point volatile organic solvent;
4) homogeneous conductive liquid film is prepared:The configuration in the step 3) that determined volume is added dropwise in the silicone rubber substrate surface that step 2) obtains
Ionic liquid hybrid solution;
5) the flexibility stress sensor that conduction liquid film is fettered based on nano wire is formed:Ion is added dropwise in the surface obtained in step 4)
The silicone rubber substrate of liquid hybrid solution, which is stored at room temperature, makes low boiling point volatile organic solvent volatilize.
3. a kind of preparation side of flexibility stress sensor fettering conduction liquid film based on nano wire according to claim 2
Method, which is characterized in that the silicone oligomer is the dimethyl silicone polymer for the end-vinyl that the degree of polymerization is 10-200;It is described
Crosslinking agent is the dimethyl silicone polymer of terminal methyl;The modifying agent is the ethyoxyl polyethyleneimine of a concentration of 35~40wt%
Aqueous solution.
4. a kind of preparation side of flexibility stress sensor fettering conduction liquid film based on nano wire according to claim 2
Method, which is characterized in that the silicone oligomer:Crosslinking agent:The ratio of modifying agent is 5-10g:0.5-1g:10-40μL.
5. a kind of preparation side of flexibility stress sensor fettering conduction liquid film based on nano wire according to claim 2
Method, which is characterized in that the template with nano-pore is in anodic oxidation aluminium formwork, porous silicon template and PET plastic template
One kind, the depth of the nano-pore is 300nm-6 μm, a diameter of 30-400nm.
6. a kind of preparation side of flexibility stress sensor fettering conduction liquid film based on nano wire according to claim 2
Method, which is characterized in that a concentration of 0.001mg/mL-0.1mg/mL of the ionic liquid hybrid solution;The ionic liquid is
Hydrophobic ionic liquid.
7. a kind of preparation side of flexibility stress sensor fettering conduction liquid film based on nano wire according to claim 6
Method, which is characterized in that the hydrophobic ionic liquid is 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, 1- hexyls -
3- methyl imidazolium tetrafluoroborates, two (trimethyl fluoride sulfonyl) inferior amine salt of 1- octyl -3- methylimidazoles and 1- hexyl -3- methyl miaows
One kind in azoles hexafluorophosphate.
8. a kind of preparation side of flexibility stress sensor fettering conduction liquid film based on nano wire according to claim 2
Method, which is characterized in that the step 4) determined volume is 25-250 μ L.
9. a kind of preparation side of flexibility stress sensor fettering conduction liquid film based on nano wire according to claim 2
Method, which is characterized in that the volatilization time of the step 5) volatilization is 0.5-2 hours.
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CN110371919A (en) * | 2019-07-19 | 2019-10-25 | 北京航空航天大学 | A kind of self-assembly preparation method thereof of micro-nano multistage rod structure |
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