CN115652620A - Preparation method of cobweb-imitated cotton fabric-based flexible humidity sensor - Google Patents
Preparation method of cobweb-imitated cotton fabric-based flexible humidity sensor Download PDFInfo
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- CN115652620A CN115652620A CN202211341299.8A CN202211341299A CN115652620A CN 115652620 A CN115652620 A CN 115652620A CN 202211341299 A CN202211341299 A CN 202211341299A CN 115652620 A CN115652620 A CN 115652620A
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- carbon nanotube
- humidity sensor
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- 239000004744 fabric Substances 0.000 title claims abstract description 75
- 229920000742 Cotton Polymers 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 40
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 19
- 230000004044 response Effects 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 230000035945 sensitivity Effects 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 13
- 238000000151 deposition Methods 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 9
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims description 4
- 239000005750 Copper hydroxide Substances 0.000 claims description 4
- 229910001956 copper hydroxide Inorganic materials 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 abstract description 20
- 239000001913 cellulose Substances 0.000 abstract description 20
- 229920002521 macromolecule Polymers 0.000 abstract description 9
- 238000007711 solidification Methods 0.000 abstract description 7
- 230000008023 solidification Effects 0.000 abstract description 7
- 241000239290 Araneae Species 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 238000013459 approach Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 230000000638 stimulation Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007170 pathology Effects 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000241 respiratory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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Abstract
The invention provides a preparation method of a cobweb-imitated cotton fabric-based flexible humidity sensor. And then, in the process of slow heat treatment (40-50 ℃), enabling a small part of dissolved cellulose macromolecules to migrate to the carbon nanotube network layer and gradually approach to each other for solidification, forming cellulose solidification points in the carbon nanotube network structure, wherein each cellulose solidification point can be bonded with a plurality of carbon nanotubes to form nodes (similar to spider nets) communicated with the carbon nanotube network, and preparing the cotton fabric with the humidity sensing function and the advantages of wide humidity detection range, high sensitivity, short response time, good structural firmness and the like. The method and the technical process are simple, the efficiency is high, and special equipment is not needed; the cost of raw materials is low, and the large-scale production is facilitated; the preparation process is carried out in a water phase, and no organic solvent is required to be added, so that the preparation method is environment-friendly; the functional cotton fabric has the advantages of wide humidity detection range, high sensitivity, short response time, humidity sensing property and good structural firmness.
Description
Technical Field
The invention relates to a preparation method of a functional cotton fabric, in particular to a preparation method of a cobweb-imitated cotton fabric-based flexible humidity sensor.
Background
People need to know their health conditions, and small-sized and convenient wearable electronic products which can be used for health monitoring and disease monitoring are receiving more and more attention. Wearable microenvironment humidity monitoring products have been proven to be a new generation of clinical pathology detection technology, which monitors human sleep, rest and exercise. As a wearable intelligent electronic product, the fabric has the characteristics of softness, ventilation, flexibility, durability and the like besides the requirement on the sensing capability, and cotton fabric as one of common textiles can meet the requirement. To date, methods of constructing wearable humidity sensors based on cotton fabrics or cotton fibers have relied on coating techniques. Allison et al monitored the respiratory state of the human body at the mask microenvironment humidity by coating poly (3, 4-ethylenedioxythiophene): chloroform on cotton fabric. Maity et al coated polyurethane composites on carbon nanotubes on cotton fabric to enable detection of specific humidity ranges. Although these methods achieve flexible moisture sensors on cotton fabrics as substrates, significant challenges remain to be overcome. For example, textiles are woven from tight fibers that deform less when stimulated by moisture than loose fibers of film or paper base, resulting in lower sensitivity of cotton fabric-based sensors and longer response and recovery times of the textile. In addition, in order to endure abrasion and friction caused by body movement, the conductive material needs to be adhered to the surface of the cotton fabric by adding a cross-linking agent or using a coating agent, which may cause problems such as deterioration of wearability of the cotton fabric. The research designs a cotton fabric-based humidity sensor of a carbon nano tube humidity sensitive network formed by cellulose nodes by using a spider web structure as inspiration on the basis of a cotton fabric slightly-dissolving technology. Firstly, depositing a conductive carbon nano tube network layer on the surface of a cotton fabric, and then treating the cotton fabric by slightly dissolving a cellulose good solvent-cuprammonium solution, so that cellulose molecules on the surface of the fabric are dissolved, macromolecules in the fabric are not influenced, and the dissolved cellulose macromolecules can be adhered to the carbon nano tube network layer. And then, in the process of slow heat treatment (40-50 ℃), ammonia and water in the cuprammonium solution volatilize in a gas form, the surface layer volatilizes quickly, and the cuprammonium solution carries a small part of dissolved cellulose macromolecules to migrate to the carbon nanotube network layer. Because the boiling point of ammonia is lower than that of water, cellulose macromolecules migrated into the carbon nanotube network layer gradually approach each other and solidify to form cellulose solidification points in the carbon nanotube network structure, and each cellulose solidification point can be bonded with a plurality of carbon nanotubes to form nodes (similar to spider webs) communicated with the carbon nanotube network. When being stimulated by external humidity, the cellulose nodes can expand rapidly due to large specific surface area, connectivity among carbon nano tubes in the nodes is reduced, and resistance of the conductive cotton fabric is reduced, namely, the humidity stimulation is converted into an electric signal, and a spider immediately senses existence of a prey through vibration of the nodes. The prepared cotton fabric humidity sensor has the advantages of wide detection range, high sensitivity, short response time, good structural firmness and the like.
Disclosure of Invention
The technical problem to be solved by the invention is to provide the preparation method of the cotton fabric with the humidity sensing function, which is simple and feasible in process and suitable for large-scale production, and the prepared functional cotton fabric has the advantages of wide detection range, high sensitivity, short response time, good structural firmness and the like in humidity sensing.
In order to solve the technical problems, the technical scheme of the invention is to provide a preparation method of a cobweb-imitated cotton fabric-based flexible humidity sensor, which is characterized by comprising the following steps of:
step 1: depositing the carbon nanotubes in the carbon nanotube dispersion liquid on the cotton fabric through vacuum assistance, and covering uniformly distributed carbon nanotube network layers on two sides of the cotton fabric after multiple depositions;
step 2: preparing a copper ammonia solution as a slightly-dissolved treatment solution;
and step 3: soaking the cotton fabric covered with the carbon nano tube network layer in a slightly soluble solution treatment solution at 15 ℃, and taking out the cotton fabric from the slightly soluble solution treatment solution after 3 min;
and 4, step 4: heating the cotton fabric treated in the step (3) until the cotton fabric is completely dried;
and 5: and finally, taking the processed cotton fabric out, washing with water, and drying to prepare the cotton fabric with the humidity sensing function, which has the advantages of wide detection range, high sensitivity, short response time, good structural firmness and the like.
Preferably, in the step 1, the concentration of the carbon nanotube dispersion liquid is 2.5 g/L-7.5 g/L.
Preferably, in the step 2, the copper ammonia solution is prepared by completely dissolving copper hydroxide (0.5 g to 1.0 g) in 100mL of ammonia water.
Preferably, in the step 4, the heating temperature is 40 ℃ to 50 ℃.
The method comprises the steps of firstly depositing a conductive carbon nanotube network layer on the surface of the cotton fabric, and then treating the cotton fabric by slightly dissolving with a copper ammonia solution, so that cellulose molecules on the surface of the fabric are dissolved, macromolecules in the fabric are not affected, and the dissolved cellulose macromolecules can be adhered to the carbon nanotube network layer. And then, in the process of slow heat treatment (at 40-50 ℃), ammonia and water in the copper ammonia solution volatilize in a gas form, the surface layer volatilizes quickly, and the copper ammonia solution carries a small part of dissolved cellulose macromolecules to migrate to the carbon nanotube network layer. Because the boiling point of ammonia is lower than that of water, cellulose macromolecules migrated into the carbon nanotube network layer gradually approach each other and solidify to form cellulose solidification points in the carbon nanotube network structure, and each cellulose solidification point can be bonded with a plurality of carbon nanotubes to form nodes (similar to spider webs) communicated with the carbon nanotube network. When the cellulose nodes are stimulated by external humidity, the cellulose nodes can expand rapidly due to large specific surface area, the connectivity among carbon nano tubes in the nodes is reduced, and the resistance of the conductive cotton fabric is reduced, namely, the humidity stimulation is converted into an electric signal, and the existence of a prey is immediately sensed by the vibration of the nodes of a spider. The prepared cotton fabric humidity sensor has the advantages of wide detection range, high sensitivity, short response time, good structural firmness and the like.
Compared with the prior art, the method provided by the invention has the following beneficial effects:
(1) The method and the technical process are simple, the efficiency is high, and special equipment is not needed;
(2) The raw material cost is low, and the large-scale production is facilitated;
(3) The preparation process is carried out in a water phase, and no organic solvent is required to be added, so that the preparation method is environment-friendly;
(4) The functional cotton fabric has the humidity sensing characteristics of wide detection range, high sensitivity, short response time and good structural firmness.
Drawings
Fig. 1 is a scanning electron microscope image of the cotton fabric with humidity sensing function prepared in example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) Depositing the carbon nanotubes in the 2.5 g/L carbon nanotube dispersion liquid on the cotton fabric through vacuum assistance, and covering uniformly distributed carbon nanotube network layers on two sides of the cotton fabric after multiple depositions;
(2) Completely dissolving 1.0g of copper hydroxide in 100mL of ammonia water to prepare a prepared copper ammonia solution serving as a slightly-dissolved treatment solution;
(3) Soaking the cotton fabric covered with the carbon nano tube network layer in a slightly soluble solution treatment solution at 15 ℃, and taking out the cotton fabric from the slightly soluble solution treatment solution after 3 min;
(4) Heating the cotton fabric treated in the step (3) at 40 ℃ until the cotton fabric is completely dried;
(5) And finally, taking out the processed cotton fabric, washing with water, and drying to prepare the cotton fabric with the humidity sensing function, which has the advantages of wide detection range, high sensitivity, short response time, good structural firmness and the like. The SEM image of the product is shown in figure 1. The maximum response of the fabric to humidity is 50%, and the humidity response and recovery time are 345 s and 200 s respectively; the response signal of the sensor drifts less than 5% after 50 dynamic cycling tests from 11% to 98% RH. There is no significant drop; the response signal drift of the sensor after the fabric can endure 50 times of bending, 20 times of friction test or 3 months of storage is about 5%.
Example 2
(1) Depositing the carbon nanotubes in the 7.5 g/L carbon nanotube dispersion liquid on the cotton fabric through vacuum assistance, and covering uniformly distributed carbon nanotube network layers on two sides of the cotton fabric after multiple depositions;
(2) Completely dissolving 0.5g of copper hydroxide in 100mL of ammonia water to prepare a copper ammonia solution serving as a slightly-dissolved treatment solution;
(3) Soaking the cotton fabric covered with the carbon nano tube network layer in a slightly soluble solution treatment solution at 15 ℃, and taking out the cotton fabric from the slightly soluble solution treatment solution after 3 min;
(4) Heating the cotton fabric treated in the step (3) at 50 ℃ until the cotton fabric is completely dried;
(5) And finally, taking out the processed cotton fabric, washing with water, and drying to prepare the cotton fabric with the humidity sensing function, which has the advantages of wide detection range, high sensitivity, short response time, good structural firmness and the like. The maximum response of the fabric to humidity is 20%, and the humidity response and recovery time are 352 s and 200 s respectively; after 50 dynamic cycling tests from 11% to 98% RH, the response signal drift of the sensor was less than 6%. There is no significant drop; the response signal drift of the sensor after the fabric can endure 50 times of bending, 20 times of friction test or 3 months of storage is about 6%.
Claims (4)
1. A preparation method of a cobweb-imitated cotton fabric-based flexible humidity sensor is characterized by comprising the following steps of:
step 1: depositing the carbon nanotubes in the carbon nanotube dispersion liquid on the cotton fabric through vacuum assistance, and covering uniformly distributed carbon nanotube network layers on two sides of the cotton fabric after multiple depositions;
step 2: preparing a copper ammonia solution as a slightly-dissolved treatment solution;
and 3, step 3: soaking the cotton fabric covered with the carbon nano tube network layer in a slightly soluble solution treatment solution at 15 ℃, and taking out the cotton fabric from the slightly soluble solution treatment solution after 3 min;
and 4, step 4: heating the cotton fabric treated in the step 3 until the cotton fabric is completely dried;
and 5: and finally, taking out the processed cotton fabric, washing with water, and drying to prepare the cotton fabric with the humidity sensing function, which has the advantages of wide detection range, high sensitivity, short response time, good structural firmness and the like.
2. The method for preparing the cobweb-imitated cotton fabric-based flexible humidity sensor according to claim 1, wherein the method comprises the following steps: in the step 1, the concentration of the carbon nano tube dispersion liquid is 2.5 g/L-7.5 g/L.
3. The method for preparing the cobweb-imitated cotton fabric-based flexible humidity sensor according to claim 1, wherein the method comprises the following steps: in the step 2, the copper ammonia solution is prepared by completely dissolving copper hydroxide (0.5 g to 1.0 g) in 100mL of ammonia water.
4. The method for preparing the cobweb-imitated cotton fabric-based flexible humidity sensor according to claim 1, wherein the method comprises the following steps: in the step 4, the heating temperature is 40-50 ℃.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100652065B1 (en) * | 2005-12-19 | 2006-12-01 | 인하대학교 산학협력단 | A method for producing a conductive cellulose film and the same manufactured by the same |
| CN102605608A (en) * | 2012-02-11 | 2012-07-25 | 东华大学 | Method for preparing super-hydrophobic conductive cellulose fabrics by CNT (carbon nano tube) finishing technology |
| CN109115266A (en) * | 2018-07-25 | 2019-01-01 | 复旦大学 | A kind of wearable multifunction flexible sensor and preparation method thereof |
| WO2019034188A2 (en) * | 2017-08-15 | 2019-02-21 | miomove s.r.o. | Sensor suitable for a smart shoe and smart clothing for complex monitoring of user data |
| CN110714337A (en) * | 2019-09-30 | 2020-01-21 | 安徽工程大学 | Preparation method of CNTs coating sensing fabric based on different fabric textures |
| US20200180264A1 (en) * | 2017-04-19 | 2020-06-11 | University Of Delaware | Carbon nanotube based sensor |
| KR20200132266A (en) * | 2019-05-16 | 2020-11-25 | 단국대학교 천안캠퍼스 산학협력단 | Chitosan-carbon nanotube core-shell nanohybrid based humidity sensor |
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- 2022-10-31 CN CN202211341299.8A patent/CN115652620B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100652065B1 (en) * | 2005-12-19 | 2006-12-01 | 인하대학교 산학협력단 | A method for producing a conductive cellulose film and the same manufactured by the same |
| CN102605608A (en) * | 2012-02-11 | 2012-07-25 | 东华大学 | Method for preparing super-hydrophobic conductive cellulose fabrics by CNT (carbon nano tube) finishing technology |
| US20200180264A1 (en) * | 2017-04-19 | 2020-06-11 | University Of Delaware | Carbon nanotube based sensor |
| WO2019034188A2 (en) * | 2017-08-15 | 2019-02-21 | miomove s.r.o. | Sensor suitable for a smart shoe and smart clothing for complex monitoring of user data |
| CN109115266A (en) * | 2018-07-25 | 2019-01-01 | 复旦大学 | A kind of wearable multifunction flexible sensor and preparation method thereof |
| KR20200132266A (en) * | 2019-05-16 | 2020-11-25 | 단국대학교 천안캠퍼스 산학협력단 | Chitosan-carbon nanotube core-shell nanohybrid based humidity sensor |
| CN110714337A (en) * | 2019-09-30 | 2020-01-21 | 安徽工程大学 | Preparation method of CNTs coating sensing fabric based on different fabric textures |
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