CN114015080B - Preparation method and application of inorganic/organic composite hydrogel driver - Google Patents
Preparation method and application of inorganic/organic composite hydrogel driver Download PDFInfo
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- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 12
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- XCOBTUNSZUJCDH-UHFFFAOYSA-B lithium magnesium sodium silicate Chemical compound [Li+].[Li+].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3 XCOBTUNSZUJCDH-UHFFFAOYSA-B 0.000 claims description 6
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B25—HAND TOOLS; PORTABLE POWER-DRIVEN TOOLS; MANIPULATORS
- B25J—MANIPULATORS; CHAMBERS PROVIDED WITH MANIPULATION DEVICES
- B25J15/00—Gripping heads and other end effectors
- B25J15/0023—Gripper surfaces directly activated by a fluid
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/34—Silicon-containing compounds
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Abstract
The invention relates to a preparation method and application of an inorganic/organic composite hydrogel driver, which comprises the following steps: (1) preparation of hydrogel prepolymer; (2) preparation of inorganic particle dispersion liquid: preparing inorganic particle dispersion liquid, and uniformly dispersing inorganic particles in a dispersion medium by ultrasonic; (3) preparation of inorganic/organic composite hydrogel actuator: and taking a certain volume of inorganic particle dispersion liquid, carrying out vacuum suction filtration, pouring a certain amount of hydrogel prepolymerization liquid onto an inorganic particle layer obtained by suction filtration, and then carrying out in-situ free radical polymerization reaction by ultraviolet irradiation to obtain the inorganic/organic composite hydrogel driver. The inorganic/organic composite hydrogel driver has a fast bending rate and can be applied to the aspects of underwater intelligent robots, microfluidic valves, holders and the like.
Description
Technical Field
The invention belongs to the field of flexible intelligent driving, and particularly relates to a preparation method and application of an inorganic/organic composite hydrogel driver.
Background
Shape deformation (crawling, swimming, flying) in response to external stimuli is ubiquitous in nature and coordinates the survival of organisms in complex environments. For example, inchworm crawls through a change in shape with/without bending to achieve a coupling of radial contraction and axial extension of the body, walking forward. Inspired by the shape deformation of organisms, a variety of software drivers based on software materials have been widely developed and designed. Among them, hydrogels are considered as promising candidates for soft drivers. The high molecular hydrogel driver can generate a volume-changing soft driver under external stimulus (such as temperature, humidity, pH, electric field or magnetic field, and the like), and has great potential application value in the fields of soft robots, artificial muscles, artificial valves, and the like.
Hydrogel actuators are typically actuated by the release and absorption of water within a three-dimensional network upon exposure to an external stimulus. However, the isotropic structure of hydrogels and the resultant uniform expansion/contraction in all directions is insufficient for applications requiring complex movements. Recently, anisotropic hydrogel structures have been widely developed. Some out-of-plane deformations, such as bending, folding, twisting, or more complex deformations, can be achieved by eliminating internal unbalanced stresses generated by non-uniform strain domains corresponding to anisotropic structures in the designed hydrogel driver under external stimuli. It is important to control the driving behavior by designing a suitable anisotropic hydrogel structure.
Currently, the anisotropic structure of hydrogel drives is mainly a bilayer structure and a monolayer asymmetric structure. The hydrogel driver of the double-layer structure tends to delaminate during actual use, thereby limiting recycling and greater deformation. The design of the single-layer asymmetric structure generally requires complicated experimental conditions such as an electric field, a magnetic field and the like, and is complex to operate and difficult to control accurately. Therefore, it is very challenging to simply and rapidly prepare hydrogel drivers with excellent properties.
Disclosure of Invention
In order to solve the technical problems, the invention improves the driving performance of the hydrogel by adding inorganic hydrogel particles into the organic hydrogel, and the preparation method is simple and easy to operate.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a method for preparing an inorganic/organic composite hydrogel actuator, comprising the steps of:
(1) Preparation of hydrogel prepolymerization solution: adding 1.14g of XLG type synthetic magnesium lithium silicate into 50mL of deionized water, sealing and stirring for 2 hours to obtain a suspension, simultaneously adding 0.226g of 1-hydroxycyclohexyl phenyl ketone into 10mL of methanol to prepare an initiator solution, sequentially adding 5.65g of monomer N-isopropyl acrylamide and 0.5mL of initiator solution into the suspension, stirring for 2 hours at room temperature in a dark place, and finally introducing high-purity nitrogen to bubble, and removing dissolved oxygen contained in the solution to obtain a transparent (N-isopropyl acrylamide) -clay hydrogel prepolymer;
(2) Preparation of inorganic Dispersion: adding inorganic particles into deionized water, and performing ultrasonic treatment to uniformly disperse the inorganic particles to prepare a dispersion liquid with the concentration of 5 mg/mL;
(3) Preparation of inorganic/organic composite hydrogel drivers: and (3) taking a certain volume of inorganic dispersion liquid in the step (2), carrying out vacuum suction filtration, pouring a certain volume of hydrogel prepolymer liquid onto a SiO 2 particle layer obtained by suction filtration, irradiating the solution for a certain time from top to bottom after the solution is paved on the surface of the inorganic particle layer, carrying out in-situ free radical polymerization reaction, and then washing unreacted residual liquid and solid particles on the surface by deionized water to obtain the inorganic/organic composite hydrogel driver.
Further, the inorganic particles are one or more of silica, titania or calcium carbonate.
Further, the particle diameter of the inorganic particles is 50 to 500nm.
Further, the volume of the inorganic dispersion liquid in the step (3) is 0-30 mL, and the vacuum filtration time is 2-10 min.
Further, the volume ratio of the hydrogel prepolymer to the dispersing agent is 5:2 to 60.
Further, the ultraviolet lamp used for ultraviolet irradiation has the wavelength of 350-380 nm, the power of 250W and the time of ultraviolet irradiation of 2-10 min.
Further: the bending amplitude of the inorganic/organic composite hydrogel driver is 0-330 degrees, and the bending rate is 5-20 degrees/s.
Use of an inorganic/organic composite hydrogel actuator as described above, characterized in that: the inorganic/organic composite hydrogel driver is manufactured into a gripper model, and then the gripper model is placed into water with the temperature higher than the volume phase transition temperature to achieve water loss shrinkage, and when placed into water with the temperature lower than the volume phase transition temperature, the gripper model absorbs water to expand, so that the gripping and releasing functions are achieved.
The invention has the beneficial effects that:
according to the invention, the inorganic/organic composite hydrogel driver is prepared by vacuum suction filtration and in-situ free radical polymerization, so that on one hand, the preparation process of the hydrogel driver is simplified, the cost is saved, and the hydrogel driver has a relatively high bending rate, so that a rapid response is realized; on the other hand, the inorganic/organic composite hydrogel driver regulates and controls the thickness of the hydrogel driver by selecting proper inorganic particles and controlling the volume of inorganic particle dispersion liquid required by suction filtration, and further regulates and controls the bending angle and the bending rate, thereby realizing the control of the asymmetric structure of the hydrogel, achieving the purposes of bending in different degrees in water higher than the volume phase transition temperature of the hydrogel, grabbing objects, recovering in water lower than the volume phase transition temperature of the hydrogel and releasing the objects.
Drawings
FIG. 1 is an SEM image of a PNIPAM hydrogel having a pure water gel and different types of solid particles on one side of the surface;
FIG. 2 is a graph showing the driving process and angle change of a PNIPAM hydrogel having different amounts of SiO 2 solid particles on one side of the surface;
FIG. 3 is a graph showing the driving process and angle change of PNIPAM hydrogel with different types of solid particles on one side of the surface;
FIG. 4 is a response closing process of the soft body jaw driver in hot water;
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the present findings in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
Example 1
Preparation of inorganic/organic composite hydrogel actuator PNIPAM-SiO 2:
step (1), preparation of hydrogel prepolymer: adding 1.14g of XLG type synthetic magnesium lithium silicate into 50mL of deionized water, sealing and stirring for 2 hours to obtain a suspension, simultaneously adding 0.226g of 1-hydroxycyclohexyl phenyl ketone into 10mL of methanol to prepare an initiator solution, sequentially adding 5.65g of monomer N-isopropyl acrylamide and 0.5mL of initiator solution into the suspension, stirring for 2 hours at room temperature in a dark place, and finally introducing high-purity nitrogen to bubble, and removing dissolved oxygen contained in the solution to obtain a transparent (N-isopropyl acrylamide) -clay hydrogel prepolymer;
Step (2), preparation of inorganic dispersion liquid: adding 1g of SiO 2 into deionized water, and carrying out ultrasonic treatment to uniformly disperse inorganic particles to prepare 200mL of dispersion liquid with the concentration of 5 mg/mL;
Step (3), preparation of PNIPAM-SiO 2: taking 1,3,5,10,15,20 and 30mL of SiO 2 particle dispersion liquid respectively, carrying out vacuum suction filtration for 5min, pouring 2.5mL of hydrogel prepolymerization liquid onto a SiO 2 particle layer obtained by suction filtration, carrying out in-situ free radical polymerization reaction by using an ultraviolet lamp with the power of 250W and the wavelength of 365nm to irradiate for 4min from top to bottom after the solution is fully paved on the surface of the inorganic particle layer, and then cleaning unreacted residual liquid and solid particles on the surface by using deionized water to obtain the inorganic/organic composite hydrogel driver, which is marked as PNIPAM-xSiO 2', wherein x is the volume of the suction filtration SiO 2 particle dispersion liquid, and x= 1,3,5,10,15,20 or 30.
Fig. 1 is an SEM image of the hydrogel driver, where the combination of solid particles and hydrogel is such that the front side is granular and the back side is porous, forming an anisotropic structure. Fig. 2 and 3 show the driving performance of the hydrogel, and it can be seen that the maximum bending angle of the hydrogel increases and decreases as the content of SiO 2 particles increases, and the maximum bending amplitude of the hydrogel is about 328.1 ° when 10mL of SiO 2 particle dispersion is suction-filtered.
Example 2
Preparation of inorganic/organic composite hydrogel actuator PNIPAM-TiO 2:
Step (1), preparation of hydrogel prepolymer: adding 1.14g of XLG type synthetic magnesium lithium silicate into 50mL of deionized water, sealing and stirring for 2 hours to obtain a suspension, simultaneously adding 0.226g of 1-hydroxycyclohexyl phenyl ketone into 10mL of methanol to prepare an initiator solution, sequentially adding 5.65g of monomer N-isopropyl acrylamide and 0.5mL of initiator solution into the suspension, stirring for 2 hours at room temperature in a dark place, and finally introducing high-purity nitrogen to bubble, and removing dissolved oxygen contained in the solution to obtain a transparent (N-isopropyl acrylamide) -clay hydrogel prepolymer;
Step (2), preparation of inorganic dispersion liquid: adding 1g of TiO 2 into deionized water, and performing ultrasonic treatment to uniformly disperse inorganic particles to prepare 200mL of dispersion liquid with the concentration of 5 mg/mL;
Step (3), preparation of PNIPAM-10TiO 2: respectively taking 10mL of TiO 2 particle dispersion liquid, carrying out vacuum suction filtration for 5min, pouring 2.5mL of hydrogel prepolymerization liquid onto a TiO 2 particle layer obtained by suction filtration, after the solution is fully paved on the surface of an inorganic particle layer, carrying out in-situ free radical polymerization reaction by irradiating an ultraviolet lamp with power of 250W and wavelength of 365nm from top to bottom for 4min, and then cleaning unreacted residual liquid and solid particles on the surface by deionized water to obtain the inorganic/organic composite hydrogel driver, which is marked as PNIPAM-10TiO 2.
Fig. 1 is an SEM image of the hydrogel driver, where the combination of solid particles and hydrogel is such that the front side is granular and the back side is porous, forming an anisotropic structure. FIG. 3 is a graph showing the driving performance of hydrogels containing different types of solid particles on one surface, wherein the maximum bending amplitude of PNIPAM-10TiO 2 hydrogel was reduced to 151.5℃when 10mL of TiO 2 particle dispersion was suction-filtered due to the non-uniformity of water dispersion rate caused by the different particle sizes.
Example 3
Preparation method of PNIPAM-CaCO 3 of inorganic/organic composite hydrogel driver
Step (1), preparation of hydrogel prepolymer: adding 1.14g of XLG type synthetic magnesium lithium silicate into 50mL of deionized water, sealing and stirring for 2 hours to obtain a suspension, simultaneously adding 0.226g of 1-hydroxycyclohexyl phenyl ketone into 10mL of methanol to prepare an initiator solution, sequentially adding 5.65g of monomer N-isopropyl acrylamide and 0.5mL of initiator solution into the suspension, stirring for 2 hours at room temperature in a dark place, and finally introducing high-purity nitrogen to bubble to remove dissolved oxygen contained in the solution; obtaining transparent (N-isopropyl acrylamide) -clay hydrogel prepolymer;
step (2), preparation of inorganic dispersion liquid: adding 1g of CaCO 3 into deionized water, and carrying out ultrasonic treatment to uniformly disperse inorganic particles to prepare 200mL of dispersion liquid with the concentration of 5 mg/mL;
Step (3), preparation of PNIPAM-10 CaCO 3: respectively taking 10mL of CaCO 3 particle dispersion liquid, carrying out vacuum suction filtration for 5min, pouring 2.5mL of hydrogel prepolymerization liquid onto a CaCO 3 particle layer obtained by suction filtration, after the solution is fully paved on the surface of the inorganic particle layer, carrying out in-situ free radical polymerization reaction by irradiating an ultraviolet lamp with the power of 250W and the wavelength of 365nm from top to bottom for 4min, and then washing unreacted residual liquid and solid particles on the surface by deionized water to obtain the inorganic/organic composite hydrogel driver, which is marked as PNIPAM-10 CaCO 3.
Fig. 1 is an SEM image of the hydrogel driver, where the combination of solid particles and hydrogel is such that the front side is granular and the back side is porous, forming an anisotropic structure. FIG. 3 is a graph showing the driving performance of hydrogels containing different types of solid particles on one side of the surface, and the variation in the water dispersion rate due to the different particle sizes, and the maximum bending amplitude of PNIPAM-10 CaCO 3 hydrogels was also reduced to some extent, about 228.1 degrees, when 10mL CaCO 3 particle dispersion was suction filtered.
As can be seen from example 1, the driving performance of the prepared inorganic/organic composite hydrogel drivers was different with different addition amounts of the inorganic, and the driving performance of the hydrogels was increased and then decreased with the increase of the SiO 2 particle content, so that the maximum bending angle was increased first; from examples 1 to 3, it is understood that the driving performance of the inorganic/organic composite hydrogel driver prepared by using different kinds of inorganic additives is different, and the proper kind of inorganic particles and the proper amount of inorganic particles can be selected according to the practical application requirements.
Example 4
The inorganic/organic composite hydrogel driver PNIPAM-10SiO 2 obtained by the preparation method in the embodiment 1 is manufactured into different-shape gripper models (shown in figure 4), and then the gripper models are put into water with the temperature higher than the volume phase transition temperature to realize rapid water loss shrinkage closure, and the whole grabbing process is completed rapidly within 10 seconds.
Comparative example
Preparation method of pure water gel
Step (1), preparation of hydrogel prepolymer: adding 1.14g of XLG type synthetic magnesium lithium silicate into 50mL of deionized water, sealing and stirring for 2 hours to obtain a suspension, simultaneously adding 0.226g of 1-hydroxycyclohexyl phenyl ketone into 10mL of methanol to prepare an initiator solution, sequentially adding 5.65g of monomer N-isopropyl acrylamide and 0.5mL of initiator solution into the suspension, stirring for 2 hours at room temperature in a dark place, and finally introducing high-purity nitrogen to bubble to remove dissolved oxygen contained in the solution; obtaining transparent (N-isopropyl acrylamide) -clay hydrogel prepolymer;
Step (2), preparation of pure water gel: 2.5mL of hydrogel prepolymer solution is directly poured onto a filter membrane, after the surface of the filter membrane is fully paved with the solution, an ultraviolet lamp with the power of 250W and the wavelength of 365nm is irradiated from top to bottom for 4min to carry out in-situ radical polymerization, and then deionized water is used for cleaning residual liquid unreacted on the surface to obtain the pure water gel. As shown in FIG. 1, the pure water gel has an isotropic structure in which both the front and back surfaces are porous. In fig. 2, the pure water gel is not substantially deformed due to the isotropic structure.
From examples 1 to 4 and comparative examples, it is understood that the addition of the inorganic particles provides the inorganic/organic composite hydrogel actuator with a good driving function.
Finally, it should be noted that the above-mentioned embodiments are only for illustrating the technical solution of the present invention, and are not limiting; while the invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will appreciate that modifications may be made to the techniques described in the foregoing embodiments, or that equivalents may be substituted for elements thereof; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (4)
1. A method for preparing an inorganic/organic composite hydrogel actuator, comprising the steps of:
(1) Preparation of hydrogel prepolymerization solution: adding 1.14g of XLG type synthetic magnesium lithium silicate into 50mL of deionized water, sealing and stirring for 2 hours to obtain a suspension, simultaneously adding 0.226g of 1-hydroxycyclohexyl phenyl ketone into 10mL of methanol to prepare an initiator solution, sequentially adding 5.65g of monomer N-isopropyl acrylamide and 0.5mL of initiator solution into the suspension, stirring for 2 hours at room temperature in a dark place, and finally introducing high-purity nitrogen to bubble, and removing dissolved oxygen contained in the solution to obtain a transparent (N-isopropyl acrylamide) -clay hydrogel prepolymer;
(2) Preparation of inorganic Dispersion: adding inorganic particles into deionized water, and performing ultrasonic treatment to uniformly disperse the inorganic particles to prepare a dispersion liquid with the concentration of 5 mg/mL; the inorganic particles are silicon dioxide; the particle size of the inorganic particles is 50-500 nm;
(3) Preparation of inorganic/organic composite hydrogel drivers: vacuum filtering a certain volume of inorganic dispersion liquid in the step (2), and pouring a certain volume of hydrogel prepolymer liquid onto a SiO 2 particle layer obtained by suction filtering, wherein the volume ratio of the hydrogel prepolymer liquid to the dispersion liquid is 5: and 2-60, irradiating the solution with an ultraviolet lamp from top to bottom for a certain time to perform in-situ free radical polymerization reaction after the solution is fully paved on the surface of the inorganic particle layer, and then cleaning residual liquid and solid particles unreacted on the surface with deionized water to obtain the inorganic/organic composite hydrogel driver.
2. The method for preparing an inorganic/organic composite hydrogel actuator according to claim 1, wherein the volume of the inorganic dispersion liquid in the step (3) is 0-30 ml, and the vacuum filtration time is 2-10 min.
3. The method for preparing the inorganic/organic composite hydrogel driver according to claim 1, wherein the ultraviolet lamp used for ultraviolet irradiation has a wavelength of 350-380 nm, a power of 250W and an ultraviolet irradiation time of 2-10 min.
4. Use of an inorganic/organic composite hydrogel actuator prepared according to any one of claims 1-3, characterized in that: the inorganic/organic composite hydrogel driver is manufactured into a gripper model, and then the gripper model is placed into water with the temperature higher than the volume phase transition temperature to achieve water loss shrinkage, and when placed into water with the temperature lower than the volume phase transition temperature, the gripper model absorbs water to expand, so that the gripping and releasing functions are achieved.
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