CN114276564A - Conductive double-network hydrogel and preparation method thereof - Google Patents
Conductive double-network hydrogel and preparation method thereof Download PDFInfo
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- CN114276564A CN114276564A CN202110921221.2A CN202110921221A CN114276564A CN 114276564 A CN114276564 A CN 114276564A CN 202110921221 A CN202110921221 A CN 202110921221A CN 114276564 A CN114276564 A CN 114276564A
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 45
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 45
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 229920000161 Locust bean gum Polymers 0.000 claims abstract description 24
- 239000000711 locust bean gum Substances 0.000 claims abstract description 24
- 235000010420 locust bean gum Nutrition 0.000 claims abstract description 23
- -1 sodium tetrafluoroborate Chemical compound 0.000 claims abstract description 22
- 229910001495 sodium tetrafluoroborate Inorganic materials 0.000 claims abstract description 22
- 239000006258 conductive agent Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 239000002041 carbon nanotube Substances 0.000 claims description 10
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 239000004020 conductor Substances 0.000 claims description 2
- 239000000499 gel Substances 0.000 abstract description 16
- 229910021538 borax Inorganic materials 0.000 abstract description 4
- 230000006835 compression Effects 0.000 abstract description 4
- 238000007906 compression Methods 0.000 abstract description 4
- 239000004328 sodium tetraborate Substances 0.000 abstract description 4
- 235000010339 sodium tetraborate Nutrition 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000001514 detection method Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 238000005034 decoration Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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Abstract
The invention provides a preparation method of a conductive double-network hydrogel, which comprises the following steps: ultrasonically dispersing a conductive agent and water to obtain a dispersion liquid; and heating, stirring and mixing the dispersion, polyvinyl alcohol and locust bean gum, cooling, and mixing with a sodium tetrafluoroborate solution to obtain the conductive double-network hydrogel. According to the invention, the conductive agent, the polyvinyl alcohol and the locust bean gum are mixed by heating, and then the two polymers are crosslinked by the sodium tetrafluoroborate (borax) to form the double-network gel, so that the conductivity is high, and the conductive adhesive has excellent self-repairing performance, excellent tensile property and excellent compression property.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a conductive double-network hydrogel and a preparation method thereof.
Background
In recent years, wearable strain sensors have received much attention and research due to the large market prospects in human motion detection, health care, and the like. An ideal flexible strain sensing device should have both high sensitivity and a wide strain detection range to meet the requirements of full-scale human motion detection. Therefore, the development material is low in cost, safe, simple in preparation process and easy to industrialize, and the flexible sensing material has important value and significance and has high sensitivity and wide strain detection range.
With the rapid development of the flexible electronic industry, the internet of things and the ever-increasing demand for human-computer interfaces, the conductive hydrogel attracts attention due to its high flexibility, adjustable mechanical properties, conductivity and other characteristics. The aim of the present invention is to produce an electrically conductive hydrogel that meets the application of flexible mechanical sensors.
The single hydrogel disclosed in the prior art does not have good performance, so that it is necessary to develop a double-network hydrogel with good mechanical property and self-healing capability.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a conductive double-network hydrogel, which has high conductivity and excellent tensile property and compressive property.
The invention discloses a preparation method of a conductive double-network hydrogel, which comprises the following steps:
ultrasonically dispersing a conductive agent and water to obtain a dispersion liquid;
and heating, stirring and mixing the dispersion, polyvinyl alcohol and locust bean gum, cooling, and mixing with a sodium tetrafluoroborate solution to obtain the conductive double-network hydrogel.
Preferably, the mass ratio of the water to the polyvinyl alcohol to the locust bean gum is 500-2000: 100: 5-20.
Preferably, the ratio of the conductive agent to the water is 100-500 mg: 30-50 ML.
Preferably, the ultrasonic dispersion time is 0.5-12 h.
Preferably, the conductive agent is one or more of carbon nanotube, graphene and carbon powder conductive materials.
Preferably, the heating and stirring temperature is 70-140 ℃; the cooling is to 20-30 ℃.
Preferably, the mass fraction of the sodium tetrafluoroborate solution is 1 to 5 percent; the ratio of the mass g of the polyvinyl alcohol to the volume mL of the sodium tetrafluoroborate solution is 4-5: (2-5).
The invention provides a conductive double-network hydrogel which is prepared by the preparation method of any one of the technical schemes.
The invention provides a sensing layer, which comprises a hydrogel prepared by the preparation method of any one of the technical schemes and conductive layers respectively arranged on the upper surface and the lower surface of the hydrogel; the conductive layer is made of a conductive agent.
The invention provides a flexible electronic device, which comprises the conductive double-network hydrogel prepared by the preparation method according to any one of the technical schemes or the sensing layer according to the technical scheme.
Compared with the prior art, the invention provides a preparation method of a conductive double-network hydrogel, which comprises the following steps: ultrasonically dispersing a conductive agent and water to obtain a dispersion liquid; and heating, stirring and mixing the dispersion, polyvinyl alcohol and locust bean gum, cooling, and mixing with a sodium tetrafluoroborate solution to obtain the conductive double-network hydrogel. According to the invention, the conductive agent, the polyvinyl alcohol and the locust bean gum are mixed by heating, and then the two polymers are crosslinked by the sodium tetrafluoroborate (borax) to form the double-network gel, so that the conductivity is high, and the conductive adhesive has excellent self-repairing performance, excellent tensile property and excellent compression property.
Drawings
Fig. 1 is a self-healing schematic diagram according to embodiment 1 of the present invention;
fig. 2 is a self-healing performance result chart of embodiment 1 of the present invention;
FIG. 3 is a graph showing tensile property results of examples of the present invention and comparative examples;
FIG. 4 is a graph showing the results of the compression properties of the inventive examples and comparative examples.
Detailed Description
The invention provides a conductive double-network hydrogel and a preparation method thereof, and a person skilled in the art can appropriately improve process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope of the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The invention provides a preparation method of a conductive double-network hydrogel, which comprises the following steps:
ultrasonically dispersing a conductive agent and water to obtain a dispersion liquid;
and heating, stirring and mixing the dispersion, polyvinyl alcohol and locust bean gum, cooling, and mixing with a sodium tetrafluoroborate solution to obtain the conductive double-network hydrogel.
The conductive double-network hydrogel provided by the invention is prepared by ultrasonically dispersing a conductive agent and water to obtain a dispersion liquid.
The conductive agent is preferably one or more of carbon nano tube, graphene and carbon powder; more preferably carbon nanotubes or graphene; most preferably carbon nanotubes.
According to the invention, the ratio of the conductive agent to water is preferably 100-500 mg: (30-50) mL; more preferably 150-450 mg: (35-45) mL; most preferably 200 mg: 40 mL.
The time for ultrasonic dispersion is preferably 0.5-12 h; more preferably 1-10 h; most preferably 2-8 h.
Heating, stirring and mixing the dispersion, the polyvinyl alcohol and the locust bean gum. Preferably, the dispersion and polyvinyl alcohol are heated and stirred until the PVA is completely dissolved, and then locust bean gum is added and stirred to be fully mixed with the PVA solution.
According to the invention, the mass ratio of the water to the polyvinyl alcohol to the locust bean gum is 500-2000: 100: 5-20; preferably, the mass ratio of the water to the polyvinyl alcohol to the locust bean gum is 900-1100: 100: 7-18.
The heating and stirring temperature is preferably 70-140 ℃; more preferably 80 ℃ to 130 ℃; most preferably from 90 ℃ to 120 ℃.
In the present invention, the sources of the polyvinyl alcohol and the locust bean gum are not limited and may be commercially available.
After mixing, cooling. And then mixing with a sodium tetrafluoroborate solution to obtain the conductive double-network hydrogel.
The cooling is to 20-30 ℃. In the present invention, the cooling method is not limited, but natural cooling is preferable.
The mass fraction of the sodium tetrafluoroborate solution is preferably 1 to 5 percent; more preferably 2% to 4%.
The ratio of the mass g of the polyvinyl alcohol to the volume mL of the sodium tetrafluoroborate solution is preferably 4-5: (2-5).
The invention provides a conductive double-network hydrogel which is prepared by the preparation method of any one of the technical schemes.
The present invention has been described in detail with respect to the above preparation method, and will not be described herein again.
The gel of the invention can be obtained by mixing two gel networks, and the formed gel takes PVA as a first network and LBG as a second network. A large number of dynamic covalent bonds exist among PVA-sodium tetrafluoroborate-LBG, and the gel self-repairing capability is endowed by the rapid breakage and restoration of the dynamic covalent bonds. Meanwhile, the mechanical property of PVA-sodium tetrafluoroborate-LBG is better than that of a single component.
FIG. 1 is a schematic diagram of the conductive double-network hydrogel of the present invention, wherein polyvinyl alcohol and locust bean gum form a double-network hydrogel solution, and B (OH) is formed after borax solution is added-1The ions can form hydrogen bonds with hydroxyl groups in the hydrogel, and the hydrogen bonds can be dynamically formed and disconnected between breakage and contact, so that the self-repairing function is realized.
The invention provides a sensing layer, which comprises a hydrogel prepared by the preparation method of any one of the technical schemes and conductive layers respectively arranged on the upper surface and the lower surface of the hydrogel; the conductive layer is made of a conductive agent.
The sensing layer provided by the invention comprises the hydrogel prepared by the preparation method in any one of the technical schemes.
The sensing layer provided by the invention comprises a conductive layer; the conductive layer is made of a conductive agent. The conductive agent is preferably one or more of carbon nano tube, graphene and carbon powder; more preferably carbon nanotubes or graphene; most preferably carbon nanotubes.
In the present invention, it is preferable that a thin film of CNTs is spin-coated on glass by a spin-coating process, and then the thin film of CNTs formed on glass is transferred to the upper and lower surfaces of the double-network gel formed as described above.
The invention can further improve the conductivity by arranging the conductive layer on the gel.
The thickness of the conductive layer of the present invention is preferably 0.5 cm.
The invention provides a flexible electronic device, which comprises the conductive double-network hydrogel prepared by the preparation method according to any one of the technical schemes or the sensing layer according to the technical scheme.
The invention provides a preparation method of a conductive double-network hydrogel, which comprises the following steps: ultrasonically dispersing a conductive agent, water and a defoaming agent to obtain a dispersion liquid; and heating, stirring and mixing the dispersion, polyvinyl alcohol and locust bean gum, cooling, and mixing with a sodium tetrafluoroborate solution to obtain the conductive double-network hydrogel. According to the invention, the conductive agent, the polyvinyl alcohol and the locust bean gum are mixed by heating, and then the two polymers are crosslinked by the sodium tetrafluoroborate (borax) to form the double-network gel, so that the conductivity is high, and the conductive adhesive has excellent self-repairing performance, excellent tensile property and excellent compression property.
In order to further illustrate the present invention, the following describes a conductive double-network hydrogel and a preparation method thereof in detail with reference to examples.
Example 1
200mg of CNT were added to 40mL of deionized water, ultrasonically dispersed for 1h, followed by addition of 4g of PVA, and heated with stirring at 90 degrees Celsius until the PVA was completely dissolved. Then 0.5g locust bean gum was added and mixed well with the PVA solution with stirring. Cooling to room temperature, adding 3mL of sodium tetrafluoroborate solution with the mass fraction of 4%, and stirring to form the gel.
Example 2
300mg of CNT was added to 50mL of deionized water, ultrasonically dispersed for 1h, followed by addition of 5g of PVA, and heated with stirring at 100 ℃ until the PVA was completely dissolved. Then 0.6g of locust bean gum was added and mixed well with the PVA solution with stirring. Cooling to room temperature, adding 4mL of sodium tetrafluoroborate solution with the mass fraction of 4%, and stirring to form the gel.
Example 3
350mg of CNT was added to 50mL of deionized water, ultrasonically dispersed for 1.5h, followed by addition of 5g of PVA, and heated with stirring at 100 ℃ until the PVA was completely dissolved. Then 0.6g of locust bean gum was added and mixed well with the PVA solution with stirring. Cooling to room temperature, adding 4mL of sodium tetrafluoroborate solution with the mass fraction of 4%, and stirring to form the gel.
Example 4
200mg of CNT were added to 40mL of deionized water, ultrasonically dispersed for 1h, followed by addition of 4g of PVA, and heated with stirring at 90 degrees Celsius until the PVA was completely dissolved. Then 0.5g locust bean gum was added and mixed well with the PVA solution with stirring. Cooling to room temperature, adding 3mL of sodium tetrafluoroborate solution with the mass fraction of 4%, and stirring to form the gel.
And (3) through a spin coating process, coating CNT on glass to form a thin film, and then transferring the CNT thin film formed on the glass to the upper surface and the lower surface of the double-network gel formed in the way.
Through the process of two-step CNT addition, the electron resistivity can be made to reach 5.94 x 102Ωm。
Comparative example 1
PVA-LBG: 4g of PVA was added to 40mL of deionized water and stirred with heating at 90 ℃ until the PVA was completely dissolved. 0.5g of locust bean gum was then added and mixed well with the PVA solution with stirring. Cooling to room temperature, adding 3mL of sodium tetrafluoroborate solution with the mass fraction of 4%, and stirring to form the gel.
Comparative example 2
PVA: 4g of PVA was added to 40mL of deionized water and stirred with heating at 90 ℃ until the PVA was completely dissolved. Cooling to room temperature, adding 3mL of sodium tetrafluoroborate solution with the mass fraction of 4%, and stirring to form the gel.
Verification example
The results of measuring the performance of the inventive example and the comparative example are shown in fig. 1 to 4; fig. 2 is a self-healing performance result chart of embodiment 1 of the present invention; fig. 3 is a graph showing the results of tensile properties of examples of the present invention and comparative examples, and fig. 4 is a graph showing the results of compressive properties of examples of the present invention and comparative examples.
Self-healing performance: after breaking, the contact was 5s and a weight of 100g could be borne.
As can be seen from the figure, the polyvinyl alcohol-locust bean gum double-network hydrogel (PVA-LBG)) in the example of the present invention can have a stretching ratio of 250%, and has better stretching performance compared with the hydrogel (PVA) containing only polyvinyl alcohol.
As can be seen from FIG. 4, the PVA-locust bean gum double-network hydrogel (PVA-LBG)) in the examples of the present invention has a higher compressive modulus, and improved strength and mechanical properties, compared to the hydrogel (PVA) containing only PVA.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of the conductive double-network hydrogel is characterized by comprising the following steps:
ultrasonically dispersing a conductive agent and water to obtain a dispersion liquid;
and heating, stirring and mixing the dispersion, polyvinyl alcohol and locust bean gum, cooling, and mixing with a sodium tetrafluoroborate solution to obtain the conductive double-network hydrogel.
2. The preparation method of claim 1, wherein the mass ratio of the water to the polyvinyl alcohol to the locust bean gum is 500-2000: 100: 5-20.
3. The preparation method according to claim 1, wherein the ratio of the conductive agent to the water is 100-500 mg: 30-50 ML.
4. The preparation method according to claim 1, wherein the time for ultrasonic dispersion is 0.5 to 12 hours.
5. The preparation method according to claim 1, wherein the conductive agent is one or more of carbon nanotube, graphene and carbon powder conductive materials.
6. The preparation method according to claim 1, wherein the temperature of the heating and stirring is 70 ℃ to 140 ℃; the cooling is to 20-30 ℃.
7. The preparation method according to claim 1, wherein the mass fraction of the sodium tetrafluoroborate solution is 1% to 5%; the ratio of the mass g of the polyvinyl alcohol to the volume mL of the sodium tetrafluoroborate solution is 4-5: (2-5).
8. An electrically conductive double-network hydrogel, which is prepared by the preparation method of any one of claims 1 to 7.
9. A sensing layer, which comprises the hydrogel prepared by the preparation method of any one of claims 1 to 7 and conductive layers respectively arranged on the upper surface and the lower surface of the hydrogel; the conductive layer is made of a conductive agent.
10. A flexible electronic device comprising the conductive double-network hydrogel prepared by the preparation method of any one of claims 1 to 8 or the sensing layer of claim 9.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115219078A (en) * | 2022-06-08 | 2022-10-21 | 中山大学 | Piezoresistive sensor based on locust bean gum hydrogel and preparation method and application thereof |
| CN115595019A (en) * | 2022-10-17 | 2023-01-13 | 广西至善新材料科技有限公司（Cn） | Locust bean gum conductive coating and preparation method thereof |
| CN117626471A (en) * | 2023-10-30 | 2024-03-01 | 福建理工大学 | A continuous preparation method of high-strength ion-conducting hydrogel fibers |
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| US4406827A (en) * | 1979-09-04 | 1983-09-27 | Minnesota Mining And Manufacturing Company | Cohesive nonsticky electrically conductive gel composition |
| US20180311358A1 (en) * | 2015-11-05 | 2018-11-01 | Lubrizol Advanced Materials, Inc. | Thermoformable dual network hydrogel compositions |
| CN110563968A (en) * | 2019-09-20 | 2019-12-13 | 河南理工大学 | Preparation method of high-strength high-tensile ionic conductive hydrogel |
| CN111944167A (en) * | 2020-08-10 | 2020-11-17 | 北京科技大学 | A kind of conductive hydrogel and its preparation method and application |
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2021
- 2021-08-11 CN CN202110921221.2A patent/CN114276564A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4406827A (en) * | 1979-09-04 | 1983-09-27 | Minnesota Mining And Manufacturing Company | Cohesive nonsticky electrically conductive gel composition |
| US20180311358A1 (en) * | 2015-11-05 | 2018-11-01 | Lubrizol Advanced Materials, Inc. | Thermoformable dual network hydrogel compositions |
| CN110563968A (en) * | 2019-09-20 | 2019-12-13 | 河南理工大学 | Preparation method of high-strength high-tensile ionic conductive hydrogel |
| CN111944167A (en) * | 2020-08-10 | 2020-11-17 | 北京科技大学 | A kind of conductive hydrogel and its preparation method and application |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115219078A (en) * | 2022-06-08 | 2022-10-21 | 中山大学 | Piezoresistive sensor based on locust bean gum hydrogel and preparation method and application thereof |
| CN115219078B (en) * | 2022-06-08 | 2025-09-05 | 中山大学 | A piezoresistive sensor based on locust bean gum hydrogel and its preparation method and application |
| CN115595019A (en) * | 2022-10-17 | 2023-01-13 | 广西至善新材料科技有限公司（Cn） | Locust bean gum conductive coating and preparation method thereof |
| CN117626471A (en) * | 2023-10-30 | 2024-03-01 | 福建理工大学 | A continuous preparation method of high-strength ion-conducting hydrogel fibers |
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Application publication date: 20220405 |