CN109752412A - Flexible humidity sensor and preparation method thereof based on nano fibrous membrane - Google Patents
Flexible humidity sensor and preparation method thereof based on nano fibrous membrane Download PDFInfo
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- CN109752412A CN109752412A CN201811592324.3A CN201811592324A CN109752412A CN 109752412 A CN109752412 A CN 109752412A CN 201811592324 A CN201811592324 A CN 201811592324A CN 109752412 A CN109752412 A CN 109752412A
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- fibrous membrane
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Abstract
The invention discloses a kind of preparation methods of flexible humidity sensor based on nano fibrous membrane, the flexible humidity sensor includes electrode layer and wetness sensitive polymer film based on flexible substrates, the present invention is using Electrospun nano-fibers film as flexible substrates, on its surface by screen printing technique printed conductive material, then the Electrospun nano-fibers film with wet sensitive function is carried out by hot-pressing technique with electrode layer compound.Have many advantages, such as easy to operate, at low cost, the prepared flexible humidity sensor structure based on nano fibrous membrane is simple, shapes and sizes can be changed with demand, and it is fast to the response of humidity and there is good recycling, there are certain market prospects.
Description
Technical field
The present invention relates to sensor technical field, in particular to a kind of flexible humidity sensor based on nano fibrous membrane and
Preparation method.
Background technique
Humidity sensor has in various fields such as scientific research, military affairs, agricultural, medical instruments widely to be applied, but conventional wet
Spending sensor is mostly rigid material, does not have flexibility, therefore is difficult the tactile detection etc. suitable for surface curvature, therefore develop tool
The novel humidity sensor that the advantages that standby high sensitivity, strong flexibility, flexible wearable is integrated becomes research hotspot.
In common flexible sensing device, it is also a committed step that electrode material is compound with flexible substrates, conventional
Electrode is formed in substrate by the techniques such as photoetching, vapor deposition or spin coating, be there is a problem of preparation process complexity, is substantially increased device
The difficulty of part preparation process, it is difficult to realize quickly large-scale preparation.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of flexible humidity sensors based on nano fibrous membrane.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows: a kind of flexible humidity based on nano fibrous membrane
Sensor, it is characterised in that: including electrode layer and wetness sensitive polymer film based on flexible substrates, the flexible substrates are quiet
Electrospun nano-fibers film.
The invention also discloses the preparation methods of the above-mentioned flexible humidity sensor based on nano fibrous membrane, including following step
Suddenly
S1: the preparation of flexible substrates: preparing hydrophobic polymer polymer electrospun solution, carries out electrostatic spinning, obtains
To certain thickness hydrophobic polymer nano fibrous membrane, as flexible substrates；
S2: the preparation of electrode layer: in the flexible substrates that step S1 is prepared, i.e. hydrophobic polymer nano fibrous membrane table
Face is by screen printing technique in its surface printing conductive material, as electrode layer；
S3: the preparation of wetness sensitive polymer film:
S31: humidity-sensitive material and hydrophobic polymer polymer are added in solvent jointly, are carried out magnetic agitation, are obtained
Doped with the hydrophobic polymer spinning solution of humidity-sensitive material, wherein the doping ratio of humidity-sensitive material is solution total amount
0.1wt%-5wt%, hydrophobic polymer polymer additive amount are 1.0~3.5g, and solvent volume is 5~20ml；
S32: spray head is added in the hydrophobic polymer spinning solution doped with humidity-sensitive material prepared, carries out Static Spinning
Silk, obtains nano fibrous membrane；
S33: the obtained nano fibrous membrane of step S32 being dried, so that its solvent is sufficiently volatilized, finally obtains,
Obtain the hydrophobic polymer nano fibrous membrane doped with humidity-sensitive material, as wetness sensitive polymer film；
S4: assembling: by hot-pressing technique by electrode layer and wetness sensitive polymer Film laminated to together to get.
Preferably, in the step S2 conductive material be silver nano-grain, silver nanowires, it is a kind of in carbon nanotube or
Any several mixture of person.
Preferably, humidity-sensitive material is lithium chloride, lithium bromide, silica gel, aluminium glue, calcium chloride, illiteracy in the step S31
One or any several mixture in de- stone.
Preferably, in order to protrude the moisture pick-up properties of humidity-sensitive material, and to the sensitivity level of humidity reaction, selection it is hydrophobic
Property high molecular polymer be polyethylene terephthalate, thermoplastic polyurethane elastomer, Kynoar, poly dimethyl silicon
Oxygen alkane etc. is one such or a variety of, or water wetted material is carried out hydrophobically modified, and the water wetted material is polyacrylonitrile, gathers
One of amide 66, polyamide 6, polyvinyl alcohol, polyether sulfone, chitosan, polyoxyethylene, polylactic acid or polyvinylpyrrolidone
Or the mixture of several arbitrary proportions.
Preferably, solvent is tetrahydrofuran, trifluoroacetic acid, methylene chloride, N- crassitude in the step S31
The mixture of one or more of ketone, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide or toluene arbitrary proportion it is molten
Liquid.
Preferably, in the step S31, concentration 10wt%~30wt% of spinning solution；The time of magnetic agitation is 6h
More than；The parameter of electrostatic spinning in the step S32 are as follows: voltage 10kV~30kV, the fltting speed of spinning solution is 0.3~
5mL/h, the reception distance of spinning head to roller are 15cm~30cm, and spinning environment temperature is 20 DEG C~45 DEG C, ambient enviroment phase
It is 30%~80% to humidity.
The present invention combines electrostatic spinning technique with screen printing technique, is prepared for a based on the soft of nano fibrous membrane
Property humidity sensor, the advantages that have that device architecture is simple, form and dimension arbitrarily changes etc., at the same to the response of humidity it is fast and
Good recycling has certain market prospects.
Mature preparation process of the present invention, it is at low cost, and can be mass-produced.The nanometer prepared by electrostatic spinning technique
Tunica fibrosa has good flexibility, and electrostatic spinning technique combines the flexible electrode prepared with screen printing technique, instead of with
Past metal electrode realizes bendable folding endurance, extends its application range.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the flexible humidity sensor based on nano fibrous membrane；
Fig. 2 is the preparation flow figure of the flexible humidity sensor based on nano fibrous membrane；
Fig. 3 is that the SEM of PAN nanofiber membrane schemes；
Fig. 4 is the SEM figure doped with the PAN nanofiber membrane of lithium chloride；
Fig. 5 is the figure that prints electrode.
Specific embodiment
Specific embodiments of the present invention will be further explained below.It should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, invention described below
Technical characteristic involved in each embodiment can be combined with each other as long as they do not conflict with each other.
Embodiment 1:
This example with Static Spinning PAN, Static Spinning doped with lithium chloride PAN composite nano-fiber membrane and printing carbon nanometer
It is illustrated for pipe.
Fig. 1 is the structural schematic diagram of the flexible humidity sensor based on nano fibrous membrane, and the sensor is by two layers of Nanowire
It ties up film to constitute, silver nano-grain conductive material 2 is printed in Static Spinning PAN nanofiber membrane flexible substrates 1, as electrode layer,
It is covered on electrode layer doped with the Static Spinning PAN nanofiber membrane 3 of lithium chloride.
Fig. 2 is the preparation flow figure of the flexible humidity sensor based on nano fibrous membrane.As shown, PAN spinning first
Solution 4 obtains Static Spinning PAN nanofiber membrane flexible substrates 1 by electrostatic spinning technique, doped with the PAN spinning solution of lithium chloride
5 obtain the Static Spinning PAN nanofiber membrane 3 doped with lithium chloride by electrostatic spinning technique, as wetness sensitive polymer film,
In Static Spinning PAN nanofiber membrane flexible substrates 1, silver nano-grain conductive material 2 is printed by screen printing technique, as electricity
Pole layer, is finally carried out electrode layer and humidity sensitive layer by hot-pressing technique compound, obtains resulting devices 6.
Embodiment 2:
A kind of preparation method of the flexible humidity sensor based on nano fibrous membrane, including the following steps:
S1: the preparation of flexible substrates: preparing Kynoar electrostatic spinning solution, carries out electrostatic spinning, obtains certain thickness
The hydrophobic polymer nano fibrous membrane of degree, as flexible substrates；
S2: the preparation of electrode layer: in the flexible substrates that step S1 is prepared, i.e. hydrophobic polymer nano fibrous membrane table
By screen printing technique in its surface printing conductive material, as electrode layer, conductive material is silver nano-grain, silver nanoparticle in face
One or any several mixture in line, carbon nanotube；
S3: the preparation of wetness sensitive polymer film:
S31: lithium chloride and Kynoar are added in tetrahydrofuran jointly, carry out magnetic agitation, magnetic agitation
Time is 6h or more, obtains the hydrophobic polymer spinning solution doped with humidity-sensitive material, wherein the doping ratio of humidity-sensitive material
For the 0.1wt%-5wt% of solution total amount, hydrophobic polymer polymer additive amount is 1.0~3.5g, solvent volume is 5~
20ml, the concentration of spinning solution are 10wt%~30wt%；
S32: spray head is added in the hydrophobic polymer spinning solution doped with humidity-sensitive material prepared, carries out Static Spinning
Silk, the parameter of electrostatic spinning are as follows: voltage 10kV~30kV, the fltting speed of spinning solution are 0.3~5mL/h, spinning head to roller
Reception distance be 15cm~30cm, spinning environment temperature be 20 DEG C~45 DEG C, ambient relative humidity be 30%~80%,
Obtain nano fibrous membrane；
S33: the obtained nano fibrous membrane of step S32 being dried, so that its solvent is sufficiently volatilized, finally obtains,
Obtain the hydrophobic polymer nano fibrous membrane doped with humidity-sensitive material, as wetness sensitive polymer film；
S4: assembling: by hot-pressing technique by electrode layer and wetness sensitive polymer Film laminated to together to get.
Embodiment 3:
A kind of preparation method of the flexible humidity sensor based on nano fibrous membrane, it is characterised in that: include the following steps
S1: the preparation of flexible substrates: preparing polyethylene terephthalate electrostatic spinning solution, carries out electrostatic spinning,
Obtain certain thickness hydrophobic polymer nano fibrous membrane, as flexible substrates；
S2: the preparation of electrode layer: in the flexible substrates that step S1 is prepared, i.e. hydrophobic polymer nano fibrous membrane table
By screen printing technique in its surface printing conductive material, conductive material is silver nano-grain, silver nanowires, carbon nanotube in face
In one or any several mixture, as electrode layer；
S3: the preparation of wetness sensitive polymer film:
S31: lithium chloride and polyethylene terephthalate are added in trifluoroacetic acid jointly, carry out magnetic agitation, magnetic
The time of power stirring is 6h or more, obtains the hydrophobic polymer spinning solution doped with humidity-sensitive material, the concentration of spinning solution
10wt%~30wt%, wherein the doping ratio of lithium chloride is the 0.1wt%-5wt% of solution total amount, poly terephthalic acid second
Diol ester additive amount is 1.0~3.5g, and solvent volume is 5~20ml；
S32: spray head is added in the hydrophobic polymer spinning solution doped with humidity-sensitive material prepared, carries out Static Spinning
Silk, obtains nano fibrous membrane, the parameter of electrostatic spinning are as follows: voltage 10kV~30kV, the fltting speed of spinning solution are 0.3~5mL/
H, the reception distance of spinning head to roller are 15cm~30cm, and spinning environment temperature is 20 DEG C~45 DEG C, and ambient enviroment is relatively wet
Degree is 30%~80%.
S33: the obtained nano fibrous membrane of step S32 being dried, so that its solvent is sufficiently volatilized, finally obtains,
Obtain the hydrophobic polymer nano fibrous membrane doped with humidity-sensitive material, as wetness sensitive polymer film；
S4: assembling: by hot-pressing technique by electrode layer and wetness sensitive polymer Film laminated to together to get.
Embodiment 4:
A kind of preparation method of the flexible humidity sensor based on nano fibrous membrane, including the following steps:
S1: the preparation of flexible substrates: preparing thermoplastic polyurethane elastomer electrostatic spinning solution, carries out electrostatic spinning, obtains
To certain thickness hydrophobic polymer nano fibrous membrane, as flexible substrates；
S2: the preparation of electrode layer: in the flexible substrates that step S1 is prepared, i.e. hydrophobic polymer nano fibrous membrane table
By screen printing technique in its surface printing conductive material, conductive material is silver nano-grain, silver nanowires, carbon nanotube in face
In one or any several mixture, as electrode layer；
S3: the preparation of wetness sensitive polymer film:
S31: humidity-sensitive material and thermoplastic polyurethane elastomer are added in solvent jointly, carry out magnetic agitation 6h with
On, obtain the hydrophobic polymer spinning solution doped with humidity-sensitive material, concentration 10wt%~30wt% of spinning solution；Wherein,
The doping ratio of humidity-sensitive material is the 0.1wt% of solution total amount, thermoplastic polyurethane elastomer 3.5g, and solvent volume is
20ml, humidity-sensitive material are lithium chloride, lithium bromide, silica gel, aluminium glue, calcium chloride, one or any several mixing in montmorillonite
Object, solvent are tetrahydrofuran, trifluoroacetic acid, methylene chloride, N-Methyl pyrrolidone, n,N-Dimethylformamide, N, N- diformazan
The solution of the mixture of one or more of yl acetamide or toluene arbitrary proportion；
S32: spray head is added in the hydrophobic polymer spinning solution doped with humidity-sensitive material prepared, carries out Static Spinning
Silk, obtains nano fibrous membrane, the parameter of electrostatic spinning are as follows: voltage 10kV~30kV, the fltting speed of spinning solution are 0.3~5mL/
H, the reception distance of spinning head to roller are 15cm~30cm, and spinning environment temperature is 20 DEG C~45 DEG C, and ambient enviroment is relatively wet
Degree is 30%~80%；
S33: the obtained nano fibrous membrane of step S32 being dried, so that its solvent is sufficiently volatilized, finally obtains,
Obtain the hydrophobic polymer nano fibrous membrane doped with humidity-sensitive material, as wetness sensitive polymer film；
S4: assembling: by hot-pressing technique by electrode layer and wetness sensitive polymer Film laminated to together to get.
Claims (7)
1. a kind of flexible humidity sensor based on nano fibrous membrane, it is characterised in that: including the electrode layer based on flexible substrates
With wetness sensitive polymer film, the flexible substrates are Electrospun nano-fibers film.
2. a kind of preparation method of the flexible humidity sensor based on nano fibrous membrane, it is characterised in that: include the following steps
S1: the preparation of flexible substrates: preparing hydrophobic polymer polymer electrospun solution, carries out electrostatic spinning, obtains one
Determine the hydrophobic polymer nano fibrous membrane of thickness, as flexible substrates；
S2: the preparation of electrode layer: in the flexible substrates that step S1 is prepared, i.e., hydrophobic polymer nanofiber film surface is logical
Screen printing technique is crossed in its surface printing conductive material, as electrode layer；
S3: the preparation of wetness sensitive polymer film:
S31: humidity-sensitive material and hydrophobic polymer polymer are added in solvent jointly, are carried out magnetic agitation, are adulterated
There is the hydrophobic polymer spinning solution of humidity-sensitive material, wherein the doping ratio of humidity-sensitive material is the 0.1wt%- of solution total amount
5wt%, hydrophobic polymer polymer additive amount are 1.0~3.5g, and solvent volume is 5~20ml；
S32: spray head is added in the hydrophobic polymer spinning solution doped with humidity-sensitive material prepared, electrostatic spinning is carried out, obtains
To nano fibrous membrane；
S33: the obtained nano fibrous membrane of step S32 is dried, so that its solvent is sufficiently volatilized, finally obtains, obtain
Doped with the hydrophobic polymer nano fibrous membrane of humidity-sensitive material, as wetness sensitive polymer film；
S4: assembling: by hot-pressing technique by electrode layer and wetness sensitive polymer Film laminated to together to get.
3. the preparation method of the flexible humidity sensor based on nano fibrous membrane as claimed in claim 2, it is characterised in that: institute
Conductive material is silver nano-grain, silver nanowires, one or any several mixture in carbon nanotube in the step S2 stated.
4. the preparation method of the flexible humidity sensor based on nano fibrous membrane as claimed in claim 2, it is characterised in that: institute
In the step S31 stated, humidity-sensitive material is lithium chloride, lithium bromide, silica gel, aluminium glue, calcium chloride, one or any several in montmorillonite
The mixture of kind.
5. the preparation method of the flexible humidity sensor based on nano fibrous membrane as claimed in claim 2, it is characterised in that: institute
The hydrophobic polymer polymer stated is polyethylene terephthalate, thermoplastic polyurethane elastomer, Kynoar, gathers
Dimethyl siloxane etc. is one such or a variety of；Or water wetted material is subjected to hydrophobically modified, the water wetted material is poly-
Acrylonitrile, polyamide 66, polyamide 6, polyvinyl alcohol, polyether sulfone, chitosan, polyoxyethylene, polylactic acid or polyvinylpyrrolidine
The mixture of one or more of ketone arbitrary proportion.
6. the preparation method of the flexible humidity sensor as claimed in claim 2 based on nano fibrous membrane, it is characterised in that: described
In step S31, solvent be tetrahydrofuran, trifluoroacetic acid, methylene chloride, N-Methyl pyrrolidone, N,N-dimethylformamide, N,
The solution of the mixture of one or more of N- dimethyl acetamide or toluene arbitrary proportion.
7. the preparation method of the flexible humidity sensor based on nano fibrous membrane as claimed in claim 2, it is characterised in that: institute
It states in step S31, concentration 10wt%~30wt% of spinning solution；The time of magnetic agitation is 6h or more；In the step S32
The parameter of electrostatic spinning are as follows: the fltting speed of voltage 10kV~30kV, spinning solution are 0.3~5mL/h, and spinning head to roller connects
Receiving distance is 15cm~30cm, and spinning environment temperature is 20 DEG C~45 DEG C, and ambient relative humidity is 30%~80%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110453513A (en) * | 2019-07-31 | 2019-11-15 | 太仓碧奇新材料研发有限公司 | A kind of preparation method of polyether-ether-ketone flexible sensing array |
| CN112485298A (en) * | 2020-11-06 | 2021-03-12 | 电子科技大学 | Manufacturing method of polyvinylidene fluoride-based flexible humidity sensor |
| CN112924492A (en) * | 2021-03-18 | 2021-06-08 | 电子科技大学 | Self-powered humidity sensor based on composite spinning film and preparation method thereof |
| CN113026209A (en) * | 2021-02-08 | 2021-06-25 | 东华大学 | Self-driven piezoelectric response surface hydrophilicity and hydrophobicity regulating fiber membrane and preparation method thereof |
| CN113189150A (en) * | 2021-04-15 | 2021-07-30 | 上海工程技术大学 | Flexible humidity sensor based on high molecular polymer and preparation method thereof |
| CN113334956A (en) * | 2021-05-31 | 2021-09-03 | 泉州师范学院 | Electrostatic jet flexible transfer printing method |
| CN113790831A (en) * | 2021-09-18 | 2021-12-14 | 青岛大学 | Ultrafast-response breathable flexible pressure sensor and preparation method thereof |
| CN114216937A (en) * | 2021-12-24 | 2022-03-22 | 济南大学 | Flexible humidity sensing material, sensor and preparation method thereof |
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- 2018-12-25 CN CN201811592324.3A patent/CN109752412A/en not_active Withdrawn
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110453513A (en) * | 2019-07-31 | 2019-11-15 | 太仓碧奇新材料研发有限公司 | A kind of preparation method of polyether-ether-ketone flexible sensing array |
| CN110453513B (en) * | 2019-07-31 | 2022-02-11 | 太仓碧奇新材料研发有限公司 | Preparation method of polyether-ether-ketone flexible sensing array |
| CN112485298A (en) * | 2020-11-06 | 2021-03-12 | 电子科技大学 | Manufacturing method of polyvinylidene fluoride-based flexible humidity sensor |
| CN113026209A (en) * | 2021-02-08 | 2021-06-25 | 东华大学 | Self-driven piezoelectric response surface hydrophilicity and hydrophobicity regulating fiber membrane and preparation method thereof |
| CN113026209B (en) * | 2021-02-08 | 2021-12-21 | 东华大学 | Self-driven piezoelectric response surface hydrophilicity and hydrophobicity regulating fiber membrane and preparation method thereof |
| CN112924492A (en) * | 2021-03-18 | 2021-06-08 | 电子科技大学 | Self-powered humidity sensor based on composite spinning film and preparation method thereof |
| CN113189150A (en) * | 2021-04-15 | 2021-07-30 | 上海工程技术大学 | Flexible humidity sensor based on high molecular polymer and preparation method thereof |
| CN113334956A (en) * | 2021-05-31 | 2021-09-03 | 泉州师范学院 | Electrostatic jet flexible transfer printing method |
| CN113790831A (en) * | 2021-09-18 | 2021-12-14 | 青岛大学 | Ultrafast-response breathable flexible pressure sensor and preparation method thereof |
| CN114216937A (en) * | 2021-12-24 | 2022-03-22 | 济南大学 | Flexible humidity sensing material, sensor and preparation method thereof |
| CN114235212A (en) * | 2021-12-24 | 2022-03-25 | 济南大学 | Flexible temperature sensing material, sensor and preparation method thereof |
| CN114216937B (en) * | 2021-12-24 | 2023-10-24 | 济南大学 | Flexible humidity sensing material, sensor and preparation method thereof |
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Application publication date: 20190514 |