CN109942746B - Temperature-sensitive photoconductive valve and preparation method thereof - Google Patents
Temperature-sensitive photoconductive valve and preparation method thereof Download PDFInfo
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- CN109942746B CN109942746B CN201910237164.9A CN201910237164A CN109942746B CN 109942746 B CN109942746 B CN 109942746B CN 201910237164 A CN201910237164 A CN 201910237164A CN 109942746 B CN109942746 B CN 109942746B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000008358 core component Substances 0.000 claims abstract description 40
- 239000000017 hydrogel Substances 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011148 porous material Substances 0.000 claims abstract description 9
- 238000005520 cutting process Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 13
- 239000003599 detergent Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 8
- 239000010935 stainless steel Substances 0.000 description 8
- 230000007704 transition Effects 0.000 description 8
- 239000000178 monomer Substances 0.000 description 6
- 238000005452 bending Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 4
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000008014 freezing Effects 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000005457 ice water Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 210000004872 soft tissue Anatomy 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention provides a temperature-sensitive photoconductive valve and a preparation method thereof, wherein the temperature-sensitive photoconductive valve comprises a core component (3), the core component (3) is hydrogel with a gradient pore structure, and the preparation method comprises the following steps: 1) cutting the core assembly (3) into strips; 2) one end of the core component (3) is fixed by a clamp (2) and is completely immersed into a water-storing transparent vessel (1), and the bottom end of the core component (3) keeps a distance from the bottom of the transparent vessel (1); 3) the laser (4) is attached to the outer wall of the transparent vessel (1), when the water temperature in the transparent vessel (1) is lower than LCST, the core component (3) keeps a vertical state, and when the water temperature in the transparent vessel (1) is higher than LCST, the core component (3) bends, so that the temperature-sensitive photoconductive valve is manufactured.
Description
Technical Field
The invention relates to the technical field of temperature-sensitive photoconductive valves, in particular to a preparation method of a temperature-sensitive photoconductive valve.
Background
Hydrogels have a variety of stimulus-responsive properties, with water contents similar to those of biological soft tissues. Therefore, the hydrogel has wide potential application value in the fields of biomedicine and soft robots. Hydrogels can undergo reversible changes in response to external stimuli, such as water-loss contraction and water-absorption expansion, but these changes are often indiscriminately and uncontrollable. Therefore, the hydrogel needs to be structurally designed to have an anisotropic structure, so that the deformation can be controlled.
The design and control of hydrogel actuator heterostructures is critical to manipulating their actuation behavior. The traditional strategy is the stepwise polymerization of passive and active polymer hydrogels to form a bilayer structure. Generally, such bilayer structures exhibit slow bending/straightening deformation and tend to delaminate along weak interfaces after a large number of repeated actuations, particularly in the case of large scale bending. And conventional hydrogel actuation is often associated with water absorption and release, and this response is slow, small-scale, exhibiting a slow macroscopic response, ranging in size from a few minutes to a few hours.
The existing hydrogel-based temperature-sensitive photoconductive valve is high in manufacturing cost and cannot be automatically opened and closed, so that a temperature-sensitive photoconductive valve which is simple and easy to prepare, low in cost and capable of being automatically opened and closed is urgently needed in the market.
Disclosure of Invention
In view of the current situation of the prior art, the technical problem to be solved by the present invention is to provide a temperature-sensitive photoconductive valve and a preparation method thereof, wherein the preparation method is simple and easy to implement, the cost is low, and the temperature-sensitive photoconductive valve can be automatically opened and closed.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a temperature-sensitive photoconductive valve comprises a core component, wherein the core component is hydrogel with a gradient pore structure; the length, width and height of the core component are 50mm multiplied by 10mm multiplied by 2 mm.
Further, the preparation method of the temperature-sensitive photoconductive valve comprises the following steps:
1) cutting the core assembly into strips;
2) fixing one end of the core component by using a clamp, and completely immersing the core component into a water-storing transparent vessel, wherein the bottom end of the core component keeps a distance from the bottom of the transparent vessel;
3) the laser is attached to the outer wall of the transparent vessel, when the water temperature in the transparent vessel is lower than LCST, the core component keeps a vertical state, and when the water temperature in the transparent vessel is higher than LCST, the core component bends, so that the temperature-sensitive photoconductive valve is manufactured.
Further, the core assembly was held parallel to the transparent vessel, and the bottom end of the core assembly was held at a distance of 1/5 f, which is the total length of the core assembly, from the bottom of the transparent vessel.
Further, LCST 33 ℃.
Has the advantages that:
the temperature-sensitive photoconductive valve prepared by the method is based on a good hydrogel gradient structure, so that when the water temperature is lower than the phase transition temperature of the hydrogel, a laser beam is shielded by the hydrogel, and when the water temperature reaches the phase transition temperature, a hydrogel film with an anisotropic structure can contract to generate directional deformation, so that the photoconductive valve is bent, and the laser passes through, thereby realizing the automatic closing/opening state of the temperature-sensitive photoconductive valve; the preparation method is simple and easy to implement and low in cost.
Drawings
FIG. 1 shows detergent sudsing in a natural state;
FIG. 2 is a film obtained after the hydrogel melts ice and washes away residual detergent;
FIG. 3 is a longitudinal cross-sectional SEM image of a hydrogel;
FIG. 4 is a schematic view of a 2mm thickness-wise structure of the core assembly;
FIG. 5 is a close state of the temperature sensitive photoconductive valve;
fig. 6 shows the open state of the temperature-sensitive photoconductive valve.
The device comprises a transparent vessel 1, a clamp 2, a core component 3 and a laser 4.
Detailed Description
So that the manner in which the above recited features of the present invention can be understood and readily understood, a more particular description of the invention, briefly summarized above, may be had by reference to embodiments, some of which are illustrated in the appended drawings, wherein:
example 1
1) Taking 10ml of solution of a commercial detergent and deionized water in a mass ratio of 1:10 in a stainless steel cup with the diameter of about 10cm, weighing 2.03g of isopropyl acrylamide monomer and 0.002g N, N '-methylene bisacrylamide in the detergent solution, and stirring for 30min to fully dissolve the isopropyl acrylamide monomer and the N' -methylene bisacrylamide;
2) introducing high-purity nitrogen into the solution, and bubbling for 3min to remove oxygen contained in the solution;
3) 1.19ml of a tetramethylethylenediamine aqueous solution having a concentration of 7.75mg/ml and 1.49ml of potassium persulfate having a concentration of 10mg/ml, which had been prepared in advance, were added thereto, and stirred in an ice-water bath for 1min to disperse them uniformly.
4) The solution in the stainless steel cup is vigorously stirred by a hand-held stirrer to be foamed to the height of about 2-5cm, the surface tension of water can be greatly reduced due to the existence of the surfactant, so that the stability of the foam is ensured to a certain extent, the foam is easily prevented from being broken, and the density of the bubbles with larger volume is smaller than that of the bubbles with small volume, so that the bubbles in the cup can be in gradient distribution from bottom to top as shown in figure 1;
5) transferring the stainless steel cup onto a copper column of a freezing bath at-90 ℃ for 3-5min to enable bubbles to be rapidly frozen and shaped directionally from bottom to top, and then transferring the stainless steel cup into a low-temperature refrigerator to stand for more than 7 days;
6) and (3) taking the crosslinked hydrogel out of the refrigerator, slowly melting, washing out the non-crosslinked hydrogel monomer and the detergent by using deionized water, collapsing the originally frozen porous hydrogel block to obtain the hydrogel film shown in the figure 2, wherein the film thickness is about 1.5mm, and the longitudinal section structure of the film after freeze drying is shown in a scanning electron microscope (magnified 100 times in the figure 3), and the hydrogel film has a good directional gradient pore structure.
7) The obtained hydrogel film is cut into strips with the length, width and height of 50mm multiplied by 10mm multiplied by 2mm, and the core component 3 of the temperature-sensitive photoconductive valve is obtained.
8) One end of a core component 3 is fixed by a clamp 2 and is completely and vertically immersed into a transparent vessel 1 for storing water, the transparent vessel 1 can be a square glass vessel, the core component 3 is parallel to the outer wall of the transparent vessel 1, and the distance of 1/5 (the total length of the core component 3) is kept between the bottom end of the core component 3 and the bottom of the transparent vessel 1.
9) The laser 4 is attached to the outer wall of the transparent vessel 1 and irradiates a laser beam at a position 2/5 below the core assembly 3. The lower critical transition temperature (LCST) of the hydrogel is 33 ℃, when the temperature of water in the transparent vessel 1 is lower than the lower critical transition temperature (LCST), the hydrogel is always kept in a hydrophilic state, and the volume of the hydrogel cannot shrink, so that the core component 3 is kept in a vertical state, laser is blocked, and the temperature-sensitive light guide valve is in a closed state; when the temperature of water in the transparent vessel 1 is higher than or equal to the lower critical transition temperature (LCST), the hydrogel will start to change from the hydrophilic state to the hydrophobic state, and thus a large amount of water in the pores of the hydrogel flows out, resulting in volume shrinkage thereof, as shown in fig. 4, the pore structure of the core component 3 in the thickness direction of 2mm has a large gradient drop, so that the two sides have differences in the degree of volume shrinkage, thereby bending the core component 3, and allowing the laser to pass through from below, i.e. the temperature-sensitive photoconductive valve is in an open state.
Typically, the commercial detergent may be a commercial "white cat" detergent.
Example 2
1) Taking 10ml of solution of a commercial detergent and deionized water in a mass ratio of 1:10 in a stainless steel cup with the diameter of about 10cm, weighing 2.03g of isopropyl acrylamide monomer and 0.002g N, N '-methylene bisacrylamide in the detergent solution, and stirring for 30min to fully dissolve the isopropyl acrylamide monomer and the N' -methylene bisacrylamide;
2) introducing high-purity nitrogen into the solution, and bubbling for 3min to remove oxygen contained in the solution;
3) 1.19ml of a tetramethylethylenediamine aqueous solution having a concentration of 7.75mg/ml and 1.49ml of potassium persulfate having a concentration of 10mg/ml, which had been prepared in advance, were added thereto, and the mixture was stirred in an ice-water bath for 1min to disperse the mixture uniformly.
4) The solution in the stainless steel cup is vigorously stirred by a handheld stirrer to be foamed to the height of about 2-5cm, the surface tension of water can be greatly reduced due to the existence of the surfactant, so that the stability of foam is ensured to a certain extent, the foam is easily prevented from being broken, and the density of the bubbles with larger volume is smaller than that of the bubbles with small volume, so that the bubbles in the cup can be in a gradient state with large top and small bottom as shown in figure 1;
5) transferring the stainless steel cup onto a copper column of a liquid nitrogen freezing bath for 3-5min, wherein the temperature of the liquid nitrogen freezing bath is-196 ℃, so that bubbles are rapidly frozen and shaped directionally from bottom to top, and then transferring the stainless steel cup into a low-temperature refrigerator to stand for more than 7 days;
6) and (3) taking the crosslinked hydrogel out of the refrigerator, slowly melting the hydrogel, washing out the non-crosslinked hydrogel monomer and the detergent by using deionized water, collapsing the originally frozen porous hydrogel to obtain a hydrogel film, wherein the longitudinal section structure of the film after freeze drying is shown as a scanning electron microscope amplified by 100 times in figure 4, the hydrogel film also has a good gradient pore structure, and the thickness of the film obtained after ice melting is about 1.5 mm.
7) The obtained hydrogel film is cut into strips with the length, width and height of 50mm multiplied by 10mm multiplied by 2mm, and the core component 3 of the temperature-sensitive photoconductive valve is obtained.
8) One end of a core component 3 is fixed by a clamp 2 and is completely and vertically immersed into a transparent vessel 1 for storing water, the transparent vessel 1 can be a square glass vessel, the core component 3 is parallel to the outer wall of the transparent vessel 1, and the bottom end of the core component 3 keeps 1/5 distance of the total length of the bottom end of the transparent vessel 1.
9) The laser 4 is attached to the outer wall of the transparent vessel 1 and irradiates a laser beam at a position 2/5 below the core assembly 3. The lower critical transition temperature (LCST) of the hydrogel is 33 ℃, when the temperature of water in the transparent vessel 1 is lower than the lower critical transition temperature (LCST), the hydrogel is always kept in a hydrophilic state, and the volume of the hydrogel cannot shrink, so that the core component 3 is kept in a vertical state, laser is blocked, and the temperature-sensitive light guide valve is in a closed state; when the temperature of water in the transparent vessel 1 is higher than or equal to the lower critical transition temperature (LCST), the hydrogel will start to change from the hydrophilic state to the hydrophobic state, and thus a large amount of water in the pores of the hydrogel flows out, resulting in volume shrinkage thereof, as shown in fig. 4, the pore structure of the core component 3 in the thickness direction of 2mm has a large gradient drop, so that the two sides have differences in the degree of volume shrinkage, thereby bending the core component 3, and allowing the laser to pass through from below, i.e. the temperature-sensitive photoconductive valve is in an open state.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (3)
1. The preparation method of the temperature-sensitive photoconductive valve is characterized in that the temperature-sensitive photoconductive valve comprises a core component (3), wherein the core component (3) is hydrogel with a gradient pore structure; the length, width and height of the core component (3) are 50mm multiplied by 10mm multiplied by 2 mm;
the preparation method of the temperature-sensitive photoconductive valve comprises the following steps:
1) -cutting the core assembly (3) into strips;
2) fixing one end of the core component (3) by using a clamp (2), and completely immersing the core component into a transparent vessel (1) for storing water, wherein the bottom end of the core component (3) keeps a distance with the bottom of the transparent vessel (1);
3) and (2) attaching a laser (4) to the outer wall of the transparent vessel (1), wherein when the water temperature in the transparent vessel (1) is lower than LCST, the core component (3) keeps a vertical state, and when the water temperature in the transparent vessel (1) is higher than LCST, the core component (3) bends, so that the temperature-sensitive photoconductive valve is manufactured.
2. The method for preparing a temperature-sensitive photoconductive valve according to claim 1, wherein: the core component (3) is parallel to the transparent vessel (1), and the bottom end of the core component (3) is kept at the distance of 1/5 of the total length of the bottom end of the transparent vessel (1).
3. The method for preparing a temperature-sensitive photoconductive valve according to claim 2, wherein: the LCST =33 ℃.
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