CN115652620B - Preparation method of cobweb-like cotton fabric-based flexible humidity sensor - Google Patents
Preparation method of cobweb-like cotton fabric-based flexible humidity sensor Download PDFInfo
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- CN115652620B CN115652620B CN202211341299.8A CN202211341299A CN115652620B CN 115652620 B CN115652620 B CN 115652620B CN 202211341299 A CN202211341299 A CN 202211341299A CN 115652620 B CN115652620 B CN 115652620B
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- 239000004744 fabric Substances 0.000 title claims abstract description 77
- 229920000742 Cotton Polymers 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 41
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 41
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 17
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 13
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000151 deposition Methods 0.000 claims abstract description 10
- 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
- 238000004090 dissolution Methods 0.000 claims abstract description 8
- 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
- 238000004519 manufacturing process Methods 0.000 claims 3
- 229920002678 cellulose Polymers 0.000 abstract description 21
- 239000001913 cellulose Substances 0.000 abstract description 21
- 230000004044 response Effects 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 12
- 238000001514 detection method Methods 0.000 abstract description 11
- 229920002521 macromolecule Polymers 0.000 abstract description 11
- 230000035945 sensitivity Effects 0.000 abstract description 11
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- 238000013459 approach Methods 0.000 abstract description 3
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- 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
- 238000012544 monitoring process Methods 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
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- 238000009835 boiling Methods 0.000 description 2
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- 230000036541 health Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- -1 (3, 4-ethylenedioxythiophene) chloroform Chemical compound 0.000 description 1
- 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
- 229910052799 carbon Inorganic materials 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
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- 238000001000 micrograph Methods 0.000 description 1
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- 239000004814 polyurethane Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
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Abstract
The invention provides a preparation method of a cobweb-like cotton fabric-based flexible humidity sensor, which comprises the steps of firstly depositing a conductive carbon nano tube network layer on the surface of a cotton fabric, and then treating the cotton fabric by adopting a copper ammonia solution through micro-dissolution, 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 nano tube network layer. And then, in the slow heat treatment (40-50 ℃) process, a small part of dissolved cellulose macromolecules migrate to the carbon nano tube network layer and gradually approach each other to solidify, a cellulose solidifying point is formed in the carbon nano tube network structure, and each cellulose solidifying point is bonded with a plurality of carbon nano tubes to form nodes (similar to spider web nodes) communicated with the carbon nano tube network, so that 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 is prepared. The method and the technological process of the invention are simple, the efficiency is high, and special equipment is not needed; the raw material cost is low, and the large-scale production is facilitated; the preparation process is carried out in the water phase, does not need to add any organic solvent, and is environment-friendly; the functional cotton fabric has the advantages of wide humidity detection range, high sensitivity, short response time and good structural firmness.
Description
Technical Field
The invention relates to a preparation method of functional cotton fabric, in particular to a preparation method of a cobweb-like cotton fabric-based flexible humidity sensor.
Background
People need to know the health condition of themselves, and small and convenient wearable electronic products which can be used for health monitoring and disease monitoring are attracting more and more attention. Wearable microenvironment humidity monitoring products have proven to be a new generation of clinical pathology detection technology, monitoring human sleep, rest, and exercise. As a wearable intelligent electronic product, the sensing capability requirement is met, and the sensing device has the characteristics of softness, ventilation, flexibility, durability and the like, and cotton fabric is one of common textiles, so that the requirement can be met. To date, methods of constructing wearable humidity sensors based on cotton fabrics or cotton fibers have relied on coating techniques. Allison et al realize the monitoring of the breathing state of a human body under the micro-environment humidity of a mask by coating poly (3, 4-ethylenedioxythiophene) chloroform on cotton fabric. The Maity et al coated polyurethane composites on carbon nanotubes on cotton fabrics to achieve detection in specific humidity ranges. While these methods have achieved flexible humidity sensors with cotton fabric as a substrate, significant challenges remain to be overcome. For example, textiles are woven from tight fibers that deform less under moisture stimulation than loose fibers that are film or paper based, resulting in lower sensitivity of the cotton-based sensor and longer response and recovery times of the textile. In addition, in order to withstand abrasion and friction caused by body movement, the conductive material needs to be adhered to the surface of the cotton fabric by adding a crosslinking agent or using a coating agent, which may cause problems such as deterioration in the wearing properties of the cotton fabric. Based on the cotton fabric micro-dissolution technology, the research designs a cotton fabric based humidity sensor of a carbon nano Guan Shimin network formed by cellulose nodes by taking a spider web structure as inspiration. Firstly, depositing a conductive carbon nano tube network layer on the surface of cotton fabric, and then treating the cotton fabric by adopting a good cellulose solvent-copper ammonia solution through micro-dissolution, 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 nano tube network layer. And then, in the slow heat treatment (40-50 ℃) process, ammonia and water in the copper ammonia solution volatilize in a gas form, the surface layer volatilizes faster, and a small part of cellulose macromolecules dissolved in the copper ammonia solution are carried to migrate to the carbon nano tube network layer. Because the boiling point of ammonia is lower than that of water, cellulose macromolecules migrating into the carbon nano tube network layer gradually approach each other to solidify, a cellulose solidifying point is formed in the carbon nano tube network structure, and each cellulose solidifying point is bonded with a plurality of carbon nano tubes to form nodes (similar to spider web nodes) communicated with the carbon nano tube network. When stimulated by external humidity, these cellulose nodes expand rapidly due to the large specific surface area, and connectivity between the carbon nanotubes in the nodes decreases, resulting in a decrease in the resistance of the conductive cotton fabric, i.e., the humidity stimulus is converted into an electrical signal, as if the spider immediately senses the presence of a prey through the 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 invention aims to solve the technical problem of providing 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-like cotton fabric-based flexible humidity sensor, which is characterized by comprising the following steps:
step 1: depositing carbon nanotubes in the carbon nanotube dispersion liquid onto 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 copper ammonia solution as a micro-dissolution treatment solution;
step 3: soaking the cotton fabric covered with the carbon nano tube network layer in a micro-solution treatment solution at 15 ℃ for 3min, and taking out the cotton fabric from the micro-solution treatment solution;
step 4: heating the cotton fabric treated in the step 3 until the cotton fabric is completely dried;
step 5: and finally, taking out the treated cotton fabric, washing with water, and drying to prepare the humidity sensing functional cotton fabric with 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-1.0 g) in 100mL of ammonia water.
Preferably, in the step 4, the heating temperature is 40 ℃ to 50 ℃.
According to the invention, firstly, a conductive carbon nano tube network layer is deposited on the surface of cotton fabric, and then, the cotton fabric is treated by adopting copper ammonia solution through micro-dissolution, 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 nano tube network layer. And then, in the slow heat treatment (40-50 ℃) process, ammonia and water in the copper ammonia solution volatilize in a gas form, the surface layer volatilizes faster, and a small part of cellulose macromolecules dissolved in the copper ammonia solution are carried to migrate to the carbon nano tube network layer. Because the boiling point of ammonia is lower than that of water, cellulose macromolecules migrating into the carbon nano tube network layer gradually approach each other to solidify, a cellulose solidifying point is formed in the carbon nano tube network structure, and each cellulose solidifying point is bonded with a plurality of carbon nano tubes to form nodes (similar to spider web nodes) communicated with the carbon nano tube network. When stimulated by external humidity, these cellulose nodes expand rapidly due to the large specific surface area, and connectivity between the carbon nanotubes in the nodes decreases, resulting in a decrease in the resistance of the conductive cotton fabric, i.e., the humidity stimulus is converted into an electrical signal, as if the spider immediately senses the presence of a prey through the 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.
Compared with the prior art, the method provided by the invention has the following beneficial effects:
(1) The method and the 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 the water phase, does not need to add any organic solvent, and is environment-friendly;
(4) The functional cotton fabric has the advantages of wide detection range, high sensitivity, short response time, humidity sensitivity and good structural firmness.
Drawings
Fig. 1 is a scanning electron microscope image of a cotton fabric with a humidity sensing function prepared in example 1.
Detailed Description
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
Example 1
(1) Depositing carbon nano tubes in 2.5g/L carbon nano tube dispersion liquid on cotton fabric by vacuum assistance, and covering uniformly distributed carbon nano tube network layers on two sides of the cotton fabric after multiple depositions;
(2) 1.0g of copper hydroxide is completely dissolved in 100mL of ammonia water to prepare a copper ammonia solution as a micro-dissolution treatment solution;
(3) Soaking the cotton fabric covered with the carbon nano tube network layer in a micro-solution treatment solution at 15 ℃ for 3min, and taking out the cotton fabric from the micro-solution treatment solution;
(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 treated cotton fabric, washing with water, and drying to obtain the humidity sensing functional cotton fabric with the advantages of wide detection range, high sensitivity, short response time, good structural firmness and the like. SEM images of the products are shown in figure 1. The maximum response of the fabric to humidity was 50% and the humidity response and recovery time were 345 s and 200 s, respectively; after 50 dynamic cycling tests from 11% to 98% RH, the sensor response signal drifts less than 5%. There was no significant drop; the fabric can withstand 50 bends, 20 rub tests, or after 3 months storage, the sensor response signal drifts by about 5%.
Example 2
(1) Depositing the carbon nano tubes in the 7.5g/L carbon nano tube dispersion liquid on the cotton fabric by vacuum assistance, and covering the two sides of the cotton fabric with uniformly distributed carbon nano tube network layers after multiple depositions;
(2) Preparing copper ammonia solution by completely dissolving 0.5g of copper hydroxide in 100mL of ammonia water, and taking the copper ammonia solution as a micro-dissolution treatment solution;
(3) Soaking the cotton fabric covered with the carbon nano tube network layer in a micro-solution treatment solution at 15 ℃ for 3min, and taking out the cotton fabric from the micro-solution treatment solution;
(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 treated cotton fabric, washing with water, and drying to obtain the humidity sensing functional cotton fabric with 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 was 20% and the humidity response and recovery time were 352 s and 200 s, respectively; after 50 dynamic cycling tests from 11% to 98% RH, the sensor response signal drifts less than 6%. There was no significant drop; the fabric can withstand 50 bends, 20 rub tests, or after 3 months storage, the sensor response signal drifts by about 6%.
Claims (4)
1. The preparation method of the cobweb-like cotton fabric-based flexible humidity sensor is characterized by comprising the following steps of:
step 1: depositing carbon nanotubes in the carbon nanotube dispersion liquid onto 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 copper ammonia solution as a micro-dissolution treatment solution;
step 3: soaking the cotton fabric covered with the carbon nano tube network layer in a micro-solution treatment solution at 15 ℃ for 3min, and taking out the cotton fabric from the micro-solution treatment solution;
step 4: heating the cotton fabric treated in the step 3 until the cotton fabric is completely dried;
step 5: and finally, taking out the treated cotton fabric, washing with water, and drying to prepare the cobweb-like cotton fabric-based flexible humidity sensor.
2. A method of making a spider-web-like cotton fabric-based flexible humidity sensor according to claim 1, wherein: in the step 1, the concentration of the carbon nano tube dispersion liquid is 2.5 g/L-7.5 g/L.
3. A method of making a spider-web-like cotton fabric-based flexible humidity sensor according to claim 1, wherein: in the step 2, the cuprammonium solution is prepared by completely dissolving 0.5 g-1.0 g of copper hydroxide in 100mL of ammonia water.
4. A method of making a spider-web-like cotton fabric-based flexible humidity sensor according to claim 1, wherein: in the step 4, the heating temperature is 40-50 ℃.
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Citations (6)
| 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 |
| KR20200132266A (en) * | 2019-05-16 | 2020-11-25 | 단국대학교 천안캠퍼스 산학협력단 | Chitosan-carbon nanotube core-shell nanohybrid based humidity sensor |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20200180264A1 (en) * | 2017-04-19 | 2020-06-11 | University Of Delaware | Carbon nanotube based sensor |
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Patent Citations (6)
| 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 |
| 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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