CN110982011A - Light-directing bending material and preparation method thereof - Google Patents
Light-directing bending material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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Abstract
The invention provides a light-directing bending material and a preparation method thereof, wherein the preparation method comprises the following steps: (a) preparation of a uniformly dispersed MoS2An acrylamide prepolymerization solution of quantum dots and BN nanosheets; (b) placing the acrylamide prepolymerization solution prepared in the step (a) into a capillary glass tube through a capillary effect; (c) gelling a capillary glass tube filled with an acrylamide prepolymerization solution in a constant-temperature oxygen-free environment; (d) after the gel is finished, dissolving with hydrofluoric acidAnd (3) a capillary glass tube, soaking the gel in deionized water, and removing residual hydrofluoric acid to obtain the phototropic bent material. The light bending rate of the light bending material of the present invention is significantly greater than that of existing light bending materials. The preparation method provided by the invention is simple and easy to implement, good in operability and wide in application prospect.
Description
Technical Field
The invention relates to the technical field of light-directing bending materials, in particular to a light-directing bending material and a preparation method thereof.
Background
Bionics is one of the main means for solving the problem of the reality, and in the long history of bionics development, people can see the great propulsion effect of bionics on the human society. Recently, a light bending material simulating the phototaxis of sunflower is one of the hot problems in scientific research, for example, researchers at southeast university use graphene oxide to prepare a light bending material with excellent performance, but the physical performance of the material in light bending needs to be further improved. The light bending material can be applied to a plurality of fields such as intelligent sensors, color-changing anti-counterfeiting and the like, and has great application value.
Disclosure of Invention
The invention aims to provide a light-directing bending material to solve the problem that the comprehensive performance of the existing light-directing bending material is not ideal.
The invention also aims to provide a preparation method of the light-oriented bending material.
One of the purposes of the invention is realized by the following technical scheme: a light directing bending material prepared by:
(a) preparation of a uniformly dispersed MoS2An acrylamide prepolymerization solution of quantum dots and BN nanosheets;
(b) placing the acrylamide prepolymerization solution prepared in the step (a) into a capillary glass tube through a capillary effect;
(c) gelling a capillary glass tube filled with an acrylamide prepolymerization solution in a constant-temperature oxygen-free environment;
(d) and after the gelation is finished, dissolving the capillary glass tube by using hydrofluoric acid, then soaking the gel by using deionized water, and removing residual hydrofluoric acid to obtain the phototropic bent material.
In the step (a), the acrylamide prepolymerization solution is prepared by the following steps:
sequentially adding polyethylene glycol diacrylate, N-isopropylacrylamide and N, N' -methylenebisacrylamide into a glassware, and then adding MoS2Adding 5.0wt% of ammonium persulfate solution and N, N, N ', N' -tetramethyl ethylenediamine into the quantum dot dispersion liquid and the BN nanosheet dispersion liquid; wherein the content of the first and second substances,n-isopropylacrylamide, polyethylene glycol diacrylate and N, N' -methylenebisacrylamide =3 g: 15-20 mL: 0.1 g; n-isopropylacrylamide, N, N, N ', N' -tetramethylethylenediamine and ammonium persulfate solution =3g, 100-130 uL, 260-290 uL.
In step (a), the MoS2Quantum dot dispersion refers to MoS2Dispersion of quantum dots as solute and N-methylpyrrolidone as solvent, MoS2The concentration of the quantum dot dispersion liquid is 1mg/mL, MoS2The transverse size of the quantum dots is 1-10 nm, MoS2The dosage ratio of the quantum dot dispersion liquid to the N-isopropyl acrylamide is 1-2 mL: 3 g.
In the step (a), the BN nanosheet dispersion is a dispersion with BN nanosheets as solutes and a mixed solution of water and ethanol as a solvent, wherein the BN nanosheets are 1-10 layers thick and 0.05-1um in size, the concentration of the BN nanosheet dispersion is 1mg/mL, and the dosage ratio of the BN nanosheet dispersion to the N-isopropylacrylamide is 4-6 mL: 3 g.
In the step (b), the diameter of the capillary glass tube is 1mm, and the length of the capillary glass tube is 10 cm; in the step (c), putting a capillary glass tube containing the acrylamide prepolymerization solution into a plastic bag, exhausting air in the plastic bag, injecting nitrogen by using a nitrogen gun, sealing the plastic bag by using an adhesive tape, and then placing the plastic bag into a thermostat at 27 ℃ for gelation.
The second purpose of the invention is realized by the following technical scheme: a method of making a light directing bending material comprising the steps of:
(a) preparation of a uniformly dispersed MoS2An acrylamide prepolymerization solution of quantum dots and BN nanosheets;
(b) placing the acrylamide prepolymerization solution prepared in the step (a) into a capillary glass tube through a capillary effect;
(c) gelling a capillary glass tube filled with an acrylamide prepolymerization solution in a constant-temperature oxygen-free environment;
(d) and after the gelation is finished, dissolving the capillary glass tube by using hydrofluoric acid, then soaking the gel by using deionized water, and removing residual hydrofluoric acid to obtain the phototropic bent material.
In the step (a), the acrylamide prepolymerization solution is prepared by the following steps:
sequentially adding polyethylene glycol diacrylate, N-isopropylacrylamide and N, N' -methylenebisacrylamide into a glassware, and then adding MoS2Adding 5.0wt% of ammonium persulfate solution and N, N, N ', N' -tetramethyl ethylenediamine into the quantum dot dispersion liquid and the BN nanosheet dispersion liquid; wherein, N-isopropyl acrylamide, polyethylene glycol diacrylate and N, N' -methylene bisacrylamide are =3g, 15-20 mL and 0.1 g; n-isopropylacrylamide, N, N, N ', N' -tetramethylethylenediamine and ammonium persulfate solution =3g, 100-130 uL, 260-290 uL.
In step (a), the MoS2Quantum dot dispersion refers to MoS2Dispersion of quantum dots as solute and N-methylpyrrolidone as solvent, MoS2The concentration of the quantum dot dispersion liquid is 1mg/mL, MoS2The transverse size of the quantum dots is 1-10 nm, MoS2The dosage ratio of the quantum dot dispersion liquid to the N-isopropyl acrylamide is 1-2 mL: 3 g.
In the step (a), the BN nanosheet dispersion is a dispersion with BN nanosheets as solutes and a mixed solution of water and ethanol as a solvent, wherein the BN nanosheets are 1-10 layers thick and 0.05-1um in size, the concentration of the BN nanosheet dispersion is 1mg/mL, and the dosage ratio of the BN nanosheet dispersion to the N-isopropylacrylamide is 4-6 mL: 3 g.
In the step (b), the diameter of the capillary glass tube is 1mm, and the length of the capillary glass tube is 10 cm; in the step (c), putting a capillary glass tube containing the acrylamide prepolymerization solution into a plastic bag, exhausting air in the plastic bag, injecting nitrogen by using a nitrogen gun, sealing the plastic bag by using an adhesive tape, and then placing the plastic bag into a thermostat at 27 ℃ for gelation.
The light bending material of the invention is a material with a great light bending speed, and the performance of the material is obviously better than that of the existing light bending material. The preparation method provided by the invention is simple and easy to implement, has good operability, and the prepared MoS-based material2The quantum dot and BN nanosheet light bending material has good performance, and can be applied to intelligent sensors and color-changing anti-counterfeitingAnd the like, and has wide application prospect.
Drawings
FIG. 1 is a schematic view of the sucking of an acrylamide prepolymerization solution by capillary effect. In the figure, 1 denotes a capillary glass tube, 2 denotes an open glass container, and 3 denotes an acrylamide prepolymerization solution.
FIG. 2 shows MoS-based samples prepared in example 12Pictures of photobent materials of quantum dots and BN nanosheets taken under Mshot microscope camera MD 50.
FIG. 3 shows MoS-based samples prepared in example 12And (3) a schematic diagram of the phenomenon that the quantum dots and the BN nanosheets bend to light under the irradiation of an epi-illumination system of a Mshot metallographic microscope MJ 33.
Fig. 4 is a graph comparing the rate of light bending and the maximum bending angle of the materials prepared in example 1 and comparative example 1.
Detailed Description
The following examples are intended to illustrate the present invention in further detail, but the present invention is not limited thereto in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1 MoS-based2Preparation of quantum dot and BN nanosheet light bending material
(1) Preparing a glass vessel with a cover, wiping the glass vessel with absorbent cotton dipped with acetone and absolute ethyl alcohol respectively to wipe off dust, oil stain and the like attached to the surface, then ultrasonically cleaning the glass vessel in acetone and alcohol respectively for 10min, then ultrasonically cleaning the glass vessel in deionized water for 5min, and finally, using N to clean the glass vessel2And (5) drying.
(2) Preparation of acrylamide prepolymerization solution:
1mL of polyethylene glycol diacrylate (average molecular weight 600), 0.15g of N-isopropylacrylamide (NIPAM, AR content 98%) and 0.005g of N, N' -methylenebisacrylamide (BIS) were added to the above glassware, followed by 0.1mL of MoS2Quantum dot dispersion and 0.3mL of BN nanosheet dispersion. Reuse pipettor plus14.5uL of ammonium persulfate solution (5 wt%) and 6.5uL of N, N, N ', N' -tetramethylethylenediamine (TEMED, 99%) were added. Wherein, MoS2Quantum dot dispersion refers to MoS2The dispersion liquid with quantum dots as solute and N-methyl pyrrolidone as solvent has the concentration of 1mg/mL and MoS2The transverse size of the quantum dots is 1-10 nm; the BN nanosheet dispersion liquid is a dispersion liquid which takes the BN nanosheet as a solute and takes a mixed liquid of water and ethanol as a solvent, the concentration of the dispersion liquid is 1mg/mL, the thickness of the BN nanosheet is 1-10 layers, and the size of the dispersion liquid is 0.05-1 um. It is noted that ammonium persulfate acts as an initiator and N, N' -Tetramethylethylenediamine (TEMED) acts as a catalyst, catalyzing ammonium persulfate to generate radicals, thereby accelerating the polymerization of acrylamide gel. And finally, ultrasonically mixing for 1h in an ice bath until the prepared prepolymerization solution is completely and uniformly mixed, and no layering occurs.
(3) Gel in oxygen-free environment:
as shown in FIG. 1, the prepolymerization solution was placed in a capillary glass tube by using the capillary effect, and then the capillary glass tube filled with the prepolymerization solution was placed in a petri dish. The petri dish was placed in a plastic bag, the air therein was exhausted by squeezing (oxygen stops the binding of free radicals to inhibit the gel), nitrogen was injected into the plastic bag with a nitrogen gun, and the plastic bag was sealed with an adhesive tape. And putting the sealed plastic bag into a thermostat, and gelling for 10 hours at the temperature of 27 ℃. After the gelation is finished, the plastic bag is cut, the culture dish is taken out, the capillary glass tube is soaked in hydrofluoric acid, the gel is clamped out by using tweezers after the glass is completely decomposed, the gel is placed in deionized water to be soaked for 10min, and the water is changed for soaking. The cycle is repeated for three times, and the gel is taken out and stored in deionized water. The finished gel was prepared as shown in FIG. 2, and was cylindrical in shape, similar to a capillary glass tube.
Comparative example 1 preparation of graphene oxide-based phototropic Material
(1) Preparing a glass vessel with a cover, wiping the glass vessel with absorbent cotton dipped with acetone and absolute ethyl alcohol respectively to wipe off dust, oil stain and the like attached to the surface, ultrasonic cleaning the glass vessel in acetone and alcohol respectively for 10min, and ultrasonic cleaning in deionized waterWashing for 5min, and finally using N2And (5) drying.
(2) Preparation of acrylamide prepolymerization solution:
to the above glassware was added 1mL of polyethylene glycol diacrylate (average molecular weight 600), 0.15g of N-isopropylacrylamide (NIPAM, AR content 98%) and 0.005g of N, N' -methylenebisacrylamide (BIS), respectively, followed by 0.4mL of an aqueous graphene oxide solution (1 mg/mL). Then, 14.5uL of a solution of ammonium persulfate (5 wt%) and 6.5uL of N, N, N ', N' -tetramethylethylenediamine (TEMED, 99%) were added using a pipette. And finally, ultrasonically mixing for 1h in an ice bath until the prepared prepolymerization solution is completely and uniformly mixed, and no layering occurs.
(3) Gel in oxygen-free environment:
as shown in FIG. 1, the prepolymerization solution was placed in a capillary glass tube by using the capillary effect, and then the capillary glass tube filled with the prepolymerization solution was placed in a petri dish. The petri dish was placed in a plastic bag, the air therein was exhausted by squeezing (oxygen stops the binding of free radicals to inhibit the gel), nitrogen was injected into the plastic bag with a nitrogen gun, and the plastic bag was sealed with an adhesive tape. And putting the sealed plastic bag into a thermostat, and gelling for 10 hours at the temperature of 27 ℃. After the gelation is finished, the plastic bag is cut, the culture dish is taken out, the capillary glass tube is soaked in hydrofluoric acid, the gel is clamped out by using tweezers after the glass is completely decomposed, the gel is placed in deionized water to be soaked for 10min, and the water is changed for soaking. This was repeated three times, and the gel was taken out and placed in a hydrazine monohydrate solution (0.33M) to swell, to reduce the graphene oxide dispersed in the gel network. After two days, the gel was removed and then placed in deionized water for two days.
Example 2 Performance testing
Because of the MoS2The acrylamide gel has some special properties due to the incorporation of quantum dots and BN nano-sheets. As shown in FIG. 3, the material prepared in example 1 was placed on the stage of Mshot Mingmei gold phase microscope MJ33, the light source of the microscope (light from the epi-illumination system of Mshot Mingmei gold phase microscope MJ 33) was turned on, and the material was irradiated, and the material exhibited biomimetic characteristics like a sunflower toward the light sourceBending, and the bending angle increases with increasing irradiation time, eventually stopping bending. Because of the MoS2The quantum dot has unique optical performance and BN nanosheet wide-bandgap high-thermal conductivity, the light-to-light bending material has excellent photo-thermal conversion efficiency, and can cause the material to be reversibly bent to light during illumination, and has a large light-to-light bending rate.
MoS-based prepared in example 12The phototropic bending rates and the maximum phototropic bending angles of the quantum dots and BN nanosheets were compared to those of the material prepared in comparative example 1. Several tens of the two materials were taken, each 6.5mm in length, and were illuminated with the same light source (light from the epi-illumination system of Mshot Mingmei gold phase microscope MJ 33) and the only experimental variables were the species incorporated. We monitored the rate of light bending and the maximum bend angle at which bending ceased for both materials, and the results are shown in fig. 4. Based on MoS2The maximum bending angle of the photobending material of the quantum dots and the BN nanosheets is about 49 degrees, while the maximum bending angle of the material prepared in comparative example 1 is about 40 degrees; in addition, it is apparent that the material prepared in example 1 has a higher light bending rate than that of comparative example 1.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A light directing bending material, wherein the light directing bending material is prepared by:
(a) preparation of a uniformly dispersed MoS2An acrylamide prepolymerization solution of quantum dots and BN nanosheets;
(b) placing the acrylamide prepolymerization solution prepared in the step (a) into a capillary glass tube through a capillary effect;
(c) gelling a capillary glass tube filled with an acrylamide prepolymerization solution in a constant-temperature oxygen-free environment;
(d) and after the gelation is finished, dissolving the capillary glass tube by using hydrofluoric acid, then soaking the gel by using deionized water, and removing residual hydrofluoric acid to obtain the phototropic bent material.
2. A light redirecting material as claimed in claim 1 wherein in step (a) said pre-polymerization solution of acrylamide is prepared as follows:
sequentially adding polyethylene glycol diacrylate, N-isopropylacrylamide and N, N' -methylenebisacrylamide into a glassware, and then adding MoS2Adding 5.0wt% of ammonium persulfate solution and N, N, N ', N' -tetramethyl ethylenediamine into the quantum dot dispersion liquid and the BN nanosheet dispersion liquid; wherein, N-isopropyl acrylamide, polyethylene glycol diacrylate and N, N' -methylene bisacrylamide are =3g, 15-20 mL and 0.1 g; n-isopropylacrylamide, N, N, N ', N' -tetramethylethylenediamine and ammonium persulfate solution =3g, 100-130 uL, 260-290 uL.
3. A light directing bending material according to claim 2, wherein in step (a), said MoS is2Quantum dot dispersion refers to MoS2Dispersion of quantum dots as solute and N-methylpyrrolidone as solvent, MoS2The concentration of the quantum dot dispersion liquid is 1mg/mL, MoS2The transverse size of the quantum dots is 1-10 nm, MoS2The dosage ratio of the quantum dot dispersion liquid to the N-isopropyl acrylamide is 1-2 mL: 3 g.
4. The photobending material of claim 2, wherein in the step (a), the BN nanosheet dispersion is a dispersion with BN nanosheets as a solute and a mixed solution of water and ethanol as a solvent, wherein the BN nanosheets are 1-10 layers thick and 0.05-1um in size, the concentration of the BN nanosheet dispersion is 1mg/mL, and the dosage ratio of the BN nanosheet dispersion to N-isopropylacrylamide is 4-6 mL: 3 g.
5. The light directing curved material of claim 1, wherein in step (b), the capillary glass tube has a diameter of 1mm and a length of 10 cm; in the step (c), putting a capillary glass tube containing the acrylamide prepolymerization solution into a plastic bag, exhausting air in the plastic bag, injecting nitrogen by using a nitrogen gun, sealing the plastic bag by using an adhesive tape, and then placing the plastic bag into a thermostat at 27 ℃ for gelation.
6. A method of making a light directing material comprising the steps of:
(a) preparation of a uniformly dispersed MoS2An acrylamide prepolymerization solution of quantum dots and BN nanosheets;
(b) placing the acrylamide prepolymerization solution prepared in the step (a) into a capillary glass tube through a capillary effect;
(c) gelling a capillary glass tube filled with an acrylamide prepolymerization solution in a constant-temperature oxygen-free environment;
(d) and after the gelation is finished, dissolving the capillary glass tube by using hydrofluoric acid, then soaking the gel by using deionized water, and removing residual hydrofluoric acid to obtain the phototropic bent material.
7. The method for preparing a light redirecting material according to claim 6, wherein in step (a), the acrylamide pre-polymerization solution is prepared as follows:
sequentially adding polyethylene glycol diacrylate, N-isopropylacrylamide and N, N' -methylenebisacrylamide into a glassware, and then adding MoS2Adding 5.0wt% of ammonium persulfate solution and N, N, N ', N' -tetramethyl ethylenediamine into the quantum dot dispersion liquid and the BN nanosheet dispersion liquid; wherein, N-isopropyl acrylamide, polyethylene glycol diacrylate and N, N' -methylene bisacrylamide are =3g, 15-20 mL and 0.1 g; n-isopropylacrylamide, N, N, N ', N' -tetramethylethylenediamine and ammonium persulfate solution =3g, 100-130 uL, 260-290 uL.
8. The light directing bendable material of claim 7, whereinIn step (a), the MoS2Quantum dot dispersion refers to MoS2Dispersion of quantum dots as solute and N-methylpyrrolidone as solvent, MoS2The concentration of the quantum dot dispersion liquid is 1mg/mL, MoS2The transverse size of the quantum dots is 1-10 nm, MoS2The dosage ratio of the quantum dot dispersion liquid to the N-isopropyl acrylamide is 1-2 mL: 3 g.
9. The photobending material of claim 7, wherein in the step (a), the BN nanosheet dispersion is a dispersion with BN nanosheets as a solute and a mixed solution of water and ethanol as a solvent, wherein the BN nanosheets are 1-10 layers thick and 0.05-1um in size, the concentration of the BN nanosheet dispersion is 1mg/mL, and the dosage ratio of the BN nanosheet dispersion to N-isopropylacrylamide is 4-6 mL: 3 g.
10. The light-redirecting material of claim 6 wherein in step (b) the capillary glass tube has a diameter of 1mm and a length of 10 cm; in the step (c), putting a capillary glass tube containing the acrylamide prepolymerization solution into a plastic bag, exhausting air in the plastic bag, injecting nitrogen by using a nitrogen gun, sealing the plastic bag by using an adhesive tape, and then placing the plastic bag into a thermostat at 27 ℃ for gelation.
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| US11306159B2 (en) * | 2020-04-21 | 2022-04-19 | Saudi Arabian Oil Company | Nanosheet polymer composite for water shutoff |
| US11421141B2 (en) | 2020-04-21 | 2022-08-23 | Saudi Arabian Oil Company | Nanosheet polymer composite for water shutoff |
| US11725131B2 (en) | 2020-04-21 | 2023-08-15 | Saudi Arabian Oil Company | Polymer-sand nanocomposite for water shutoff |
| US11578543B2 (en) | 2020-10-09 | 2023-02-14 | Saudi Arabian Oil Company | Polymer-sand nanocomposite lost circulation material |
| US11828116B2 (en) | 2020-10-09 | 2023-11-28 | Alfaisal University | Polymer-sand nanocomposite lost circulation material |
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