CN113387317A - Non-rotational-axis symmetric bowl-shaped double-sided magic micro-nano motor and preparation method and application thereof - Google Patents
Non-rotational-axis symmetric bowl-shaped double-sided magic micro-nano motor and preparation method and application thereof Download PDFInfo
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- CN113387317A CN113387317A CN202110585415.XA CN202110585415A CN113387317A CN 113387317 A CN113387317 A CN 113387317A CN 202110585415 A CN202110585415 A CN 202110585415A CN 113387317 A CN113387317 A CN 113387317A
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Abstract
The invention discloses a non-rotational axisymmetric bowl-shaped double-sided magic micro-nano motor and a preparation method and application thereof. The non-rotational axis symmetrical bowl-shaped double-sided magic micro-nano motor has a hollow bowl-shaped structure, is composed of double-sided magic bodies, has only one reflection plane, and has the characteristic of non-rotational symmetry. The preparation method comprises the following steps: dispersing the hollow spherical double-sided particles in the liquid 1 to fill the particles with the liquid 1, and drying; or the particles filled with the liquid 1 are placed in the liquid 2 again for dispersion, and the micro-nano motor is obtained by stirring or drying or the combination of stirring and drying, wherein: the liquid 1 is ethanol, water or a poly dimethyl diallyl ammonium chloride aqueous solution; the liquid 2 is ethanol or water, and the two are different. The obtained micro-nano motor can realize multiple mechanism driving under the microscale by regulating and controlling the double-sided magic composition, has wide application prospect in the aspect of enhancing liquid mixing and mass transfer, and is simple to prepare and has better universality and repeatability.
Description
Technical Field
The invention belongs to the technical field of micro-nano motors, and particularly relates to a non-rotational-axis symmetric bowl-shaped double-sided super micro-nano motor and a preparation method and application thereof.
Background
The micro-nano motor is an active micro-nano device capable of converting energy in other forms (chemical energy, light energy, electric energy, magnetic energy and the like) in the environment into self kinetic energy, and has wide application prospects in the fields of biomedicine, environment purification, micro-nano processing and the like. The motion behavior of the micro-nano motor is highly dependent on the construction of the asymmetric field around the micro-nano motor, and mainly comes from the asymmetry of the structure or composition of the micro-nano motor and the asymmetric reaction induced by the asymmetric external field. Therefore, it is possible to impart more complex motion patterns and enhanced driving force to the motor by micro-nano particles having multiple asymmetries (non-rotational axial symmetry) in structure and composition, thereby exhibiting enhanced performance in mixing and mass transfer related applications in liquid environments.
In recent years, research on regulating and controlling the motion behavior of the micro-nano motor through the structural design has made an important progress. Journal of American Chemical Society (2020, 5, 142 vol. 2213) reports an Au/ZnO duplex six-edge rod-shaped micron motor with different end face diameters, which takes hydrogen peroxide as fuel and shows multimode motion behavior integrating translation and rotation under the irradiation of ultraviolet light. However, at present, the material with non-rotational axial symmetry is mainly obtained by combining hydrothermal synthesis and an electrochemical deposition method, and the preparation process is complicated and the yield is not high, so that the practical application of the material is limited.
Disclosure of Invention
The invention aims to provide a non-rotational axis symmetric bowl-shaped double-sided magical micro-nano motor and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the provided non-rotational axis symmetric bowl-shaped double-sided magic micro-nano motor has a hollow bowl-shaped structure and a double-sided magic component, has only one reflection plane, and has the characteristic of non-rotational symmetry.
According to the scheme, the non-rotational axisymmetric bowl-shaped double-sided magic micro-nano motor is obtained by collapse of hollow spherical double-sided magic particles at junctions formed by different substances.
According to the scheme, the hollow spherical double-sided particle comprises a hollow spherical substrate and a semi-coating layer on the surface of the substrate, wherein the particle size of the hollow spherical substrate is 1-1.2 mu m, and the thickness of the semi-coating layer is 15-30 nm.
According to the scheme, the hollow spherical matrix substance is a polymer, and the semi-coating layer is a metal or nonmetal oxide.
According to the scheme, the polymer is polystyrene, the metal is any one of Au, Ag and Pt, and the nonmetal oxide is SiO2And TiO2Any one of them.
According to the scheme, the mode that the semi-coating layer is coated on the surface of the hollow spherical substrate is magnetron sputtering.
The preparation method of the non-rotational axisymmetric bowl-shaped double-sided magic micro-nano motor specifically comprises the following steps:
dispersing the hollow spherical double-sided particles in the liquid 1 to ensure that the hollow spherical double-sided particles are filled with the liquid 1, and then drying the double-sided particles; or the hollow spherical double-side particles filled with the liquid 1 are placed in the liquid 2 again for dispersion, and the double-side particles are obtained by stirring or drying or the combination of stirring and drying, wherein: the liquid 1 is ethanol, water or a poly dimethyl diallyl ammonium chloride aqueous solution; the liquid 2 is ethanol or water, and the liquid 1 is different from the liquid 2. Preferably, the stirring is magnetic stirring.
According to the scheme, the hollow spherical double-sided particle is prepared by a hollow spherical substrate through magnetron sputtering and semi-coating sputtering layers.
Preferably, the hollow spherical base material is a polymer, and the sputtering layer is a metal or goldA metal oxide; more preferably, the polymer is Polystyrene (PS), the metal is any one of Au, Ag and Pt, and the non-metal oxide is SiO2And TiO2Any one of them.
Preferably, the particle size of the hollow spherical matrix is 1-1.2 μm, and the thickness of the sputtering layer is 15-30 nm.
According to the scheme, the volume percentage concentration of the poly dimethyl diallyl ammonium chloride (PDADMAC) aqueous solution is 0.01-0.12%.
According to the scheme, the stirring time is 24-120 h.
According to the scheme, the drying time is 24-120 h, and the temperature is 30-60 ℃.
The non-rotational axisymmetric bowl-shaped double-sided magic micro-nano motor is provided to be used as an artificial rotor to accelerate liquid mixing and mass transfer.
The method is applied to enhanced SERS sensing according to the scheme.
The micro-nano motor prepared by the invention is mainly prepared by utilizing the stress concentration of the junctions of different compositions of the hollow spherical double-sided nerve ions, and then generating osmotic pressure inside and outside the hollow spherical double-sided nerve particles to ensure that the junctions of different compositions of the hollow spherical double-sided nerve ions collapse due to the stress concentration under the action of the osmotic pressure. The method specifically comprises the following steps: the liquid environment that the cavity is different inside and outside is provided in the spherical double-sided particle cavity of cavity, and the intracavity outer liquid can take place to dissolve mutually, and the mass transfer can take place outside the intracavity, because the intracavity liquid volume is far less than the outer liquid volume of cavity, and intracavity liquid is the solute, and the mass transfer produces the mass flux outside pointing to the cavity, and then produces inward osmotic pressure, and the formation of collapsing easily takes place because of stress concentration in the basement of the spherical double-sided particle of cavity and half cladding layer juncture under the effect of osmotic pressure the non-rotational axisymmetric double-sided structure of bowl form. More simply, the liquid in the hollow spherical double-sided particle cavity is evaporated to generate osmotic pressure, so that the hollow spherical double-sided particle with the cavity filled with the liquid can be directly dried to prepare the non-rotational axisymmetric bowl-shaped double-sided particle micro-nano motor. The obtained micro-nano motor with a special asymmetric geometric structure can induce the surface of the micro-nano motor to generate asymmetric physical or chemical reactions, and different gradient fields (such as bubbles, temperature, concentration, surface tension, magnetic fields and the like) are generated according to the difference of reaction types to drive the motor to move.
The invention has the beneficial effects that:
1. the invention provides a double-sided magic micro-nano motor with non-rotational axial symmetry, which has the characteristics of a hollow bowl-shaped structure and double-sided magic composition, has and only has one reflecting plane and has the characteristic of non-rotational axial symmetry; by regulating the double-sided god composition of the micro-nano motor, multiple mechanism driving can be realized under the microscale, enhanced oscillatory multiple motion behaviors different from those of the traditional double-sided god micro-nano motor are shown in a liquid environment, ballistic motion and self-rotation motion are considered, and the micro-nano motor has a wide application prospect in the aspect of enhancing liquid mixing and mass transfer.
2. In the preparation method provided by the invention, liquid osmotic pressure difference is formed between the inner cavity and the outer cavity of the hollow spherical double-sided particles in a stirring or drying or stirring and drying combined mode, and the collapse of the hollow spherical double-sided particles at the stress concentration part of the connection of the hollow spherical double-sided particles is controlled, so that the micro-nano motor with the hollow bowl-shaped structure and the double-sided particles can be prepared; the preparation method is simple, has good universality and repeatability, is high in yield, and has wide application prospect.
Drawings
Fig. 1 is a field emission scanning electron microscope image of a PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in example 1 of the present invention.
Fig. 2 is a transmission electron microscope image of the PS-Ag non-rotational axisymmetric bowl-shaped bifacial magic micro-nano motor synthesized in example 1 of the present invention.
Fig. 3 is an X-ray energy spectrum of the PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in example 1 of the present invention, where a is Ag and b is C.
Fig. 4 is a comparison of the motion behaviors of the PS-Ag non-rotational axisymmetric bowl-shaped bi-facial magic micro-nano motor synthesized in example 1 of the present invention and the conventional PS-Ag bi-facial magic micro-nano motor, where a is the PS-Ag non-rotational axisymmetric bowl-shaped bi-facial magic micro-nano motor, and b is the conventional PS-Ag bi-facial magic micro-nano motor.
Fig. 5 shows SERS performance characteristics of the PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in embodiment 1 of the present invention.
Fig. 6 is a field emission scanning electron microscope image of the PS-Pt non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in embodiment 2 of the present invention.
Fig. 7 is an X-ray energy spectrum of the PS-Pt non-rotational axisymmetric bowl-shaped dihedral micro nano-motor synthesized in embodiment 2 of the present invention, wherein a is Pt and b is C.
Fig. 8 is a field emission scanning electron microscope image of the PS-Au non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in embodiment 3 of the present invention.
FIG. 9 shows PS-SiO synthesized in example 4 of the present invention2-field emission scanning electron microscopy of a Ag non-rotational axisymmetric bowl-shaped double-sided Shen micro-nano motor.
FIG. 10 shows PS-SiO synthesized in example 4 of the present invention2An X-ray line energy scanning spectrogram of the Ag non-rotation axis symmetric bowl-shaped double-sided Shen micro-nano motor.
Fig. 11 is a field emission scanning electron microscope image of the PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in example 5 of the present invention.
Fig. 12 is a field emission scanning electron microscope image of the PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in embodiment 6 of the present invention.
Fig. 13 is a field emission scanning electron microscope image of the PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in example 7 of the present invention.
Fig. 14 is a field emission scanning electron microscope image of the PS-Pt non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in embodiment 8 of the present invention.
Fig. 15 is a field emission scanning electron microscope image of the PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in example 9 of the present invention.
Fig. 16 is a field emission scanning electron microscope image of the PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor synthesized in embodiment 10 of the present invention.
Detailed Description
The following examples further illustrate the technical aspects of the present invention, but should not be construed as limiting the scope of the present invention.
Example 1
The non-rotational axisymmetric double-sided Shen micro-nano motor is provided, and the specific preparation steps are as follows:
1) firstly, dispersing 1mg of Polystyrene (PS) hollow microspheres (with the diameter of 1 mu m) on a glass substrate, carrying out Ag magnetron sputtering for 60s, and obtaining PS-Ag hollow spherical double-sided particles, wherein the surface of the PS hollow microspheres is coated with an Ag layer in a half way, and the thickness of the Ag layer is 25 nm.
2) Dispersing the PS-Ag hollow spherical double-sided particles (the diameter is 1 mu m, the thickness of the Ag layer is 25nm) obtained in the step 1) with ethanol, centrifugally washing for 3 times until the supernatant is clear, removing the supernatant to obtain the PS-Ag hollow spherical double-sided particles with ethanol filled in the hollow cavity, dispersing the particles into 8mL of water, magnetically stirring for 24 hours, centrifugally separating, drying at 30 ℃ for 48 hours, and dispersing the obtained product in the water for storage.
As can be seen from the field emission scanning electron microscope image and the transmission electron microscope image of the product of the embodiment in FIGS. 1 and 2, the obtained product has a hollow bowl-shaped structure and a double-sided structure, has only one reflection plane, and has the characteristic of non-rotational axis symmetry.
The X-ray energy spectrum surface scanning result in fig. 3 further illustrates the asymmetric distribution of the Ag element on the motor, and the collapse of the original hollow spherical double-sided particle occurs at the PS-Ag interface, which proves that the prepared micro-nano motor has the non-rotational axisymmetric characteristic.
Dispersing the prepared PS-Ag non-rotation axisymmetric bowl-shaped double-sided Shen micro-nano motor in H with the mass fraction of 1.7%2O2Solution, KCl solution with concentration of 600 mu mol/L and using strength of 500mW/cm2As shown in fig. 4, the bowl-shaped non-rotational axisymmetric micro-nano motor (fig. 4(a)) shows enhanced oscillatory multiple motions compared with the conventional PS-Ag double-sided magic micro-nano motor (fig. 4(b)), and the specific motion characteristics are as follows: (1) the translation is accompanied with the rotation in the non-acceleration stage; (2) an oscillatory sudden velocity change; (3) the speed is higher than that of the Janus motor; (4) the acceleration phase undergoes a motion direction transition and there is a velocity threshold.
The prepared PS-AgH with mass fraction of 1.7% for non-rotating shaft symmetrical bowl-shaped double-sided magic micro-nano motor2O2Solution, KCl solution with concentration of 600 mu mol/L and 1X 10-8The mixed solution of M and R6G is uniformly dispersed in 500mW/cm2The ultraviolet light irradiation is carried out for 30 minutes, and the Raman spectrum test is carried out on the motor after the recovery and drying. As can be seen from FIG. 5, the PS-Ag non-rotating axisymmetric bowl-shaped double-sided magic micro-nano motor (Active NAJ-SPs) has stronger Raman signals than traditional PS-Ag hollow spherical double-sided magic particles (Active PS-Ag Janus) and inert particles (Active NAJ-SPs), and the application of the motor in the aspect of mass transfer enhancement is proved. Wherein the traditional PS-Ag hollow spherical double-sided particles are prepared in the example 1, the diameter is 1 μm, and the thickness of the Ag layer is 25 nm. Inert particles being no fuel (H)2O2KCl) PS-Ag non-rotation axis symmetrical bowl-shaped double-sided magic micro-nano motor.
Under ultraviolet light, Ag-AgCl oscillation reaction occurs on the surface of the motor, and due to the limiting effect of the bowl-shaped structure on ion diffusion, an enhanced self-built electric field is formed around the motor and acts on the negatively charged motor to provide a driving force deviating from the center of mass, so that torque is generated, and enhanced oscillatory multiple motion behaviors are formed. The enhanced movement improves the contact probability of the motor and the molecules of the object to be detected, enhances the mass transfer of the motor in the liquid, and further improves the detection effect of the motor as an SERS substrate. Meanwhile, the AgCl-Ag composite structure on the surface of the motor is that the motor is in H2O2Provides good chemical stability.
Example 2
The hollow spherical PS-Ag double-sided particles obtained in example 1 were adjusted to hollow spherical PS-Pt double-sided particles (diameter: 1 μm, Pt layer thickness: 25nm), and the procedure of example 1 was repeated to obtain the product. The structure and composition of the product are characterized by using a field emission scanning electron microscope and an X-ray energy spectrum, and as shown in figures 6 and 7, the obtained product is a PS-Pt non-rotation axis symmetrical bowl-shaped double-sided magic micro-nano motor.
Example 3
The hollow spherical PS-Ag double-sided particles in example 1 were adjusted to hollow spherical PS-Au double-sided particles (diameter 1 μm, Au layer thickness 25nm), and the procedure of example 1 was repeated to obtain the product. The structure of the product of the field emission scanning electron microscope is used for characterization, and as shown in fig. 8, the obtained product is a PS-Au non-rotational axisymmetric bowl-shaped double-sided magic micro-nano motor.
Example 4
The hollow spherical PS-Ag double-sided particles of example 1 were adjusted to PS-SiO2Hollow spherical Ag double-sided particle (diameter 1 μm, TiO)2Layer thickness 4nm, Ag layer thickness 15nm) and the procedure of example 1 above was repeated to obtain the product. Here, SiO is used here2The purpose of sputtering a layer of Ag over the layer was to facilitate later SEM characterization of the product. The structure and composition of the product were characterized by using a field emission scanning electron microscope and X-ray energy spectroscopy, as shown in FIGS. 9 and 10, indicating that the obtained product was PS-SiO2the-Ag non-rotation axis symmetric bowl-shaped double-sided Shen micro-nano motor.
Example 5
The water of example 1 was adjusted to 0.12% PDADMAC in water and the procedure of example 1 was repeated to obtain the product. The structure of the product of the field emission scanning electron microscope is used for characterization, and as shown in fig. 11, the obtained product is a PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor.
Example 6
The stirring time in example 1 was adjusted to 120 hours and the drying step was omitted, and the steps of example 1 were repeated to obtain a product, which was characterized by the structure of the product of a field emission scanning electron microscope, as shown in fig. 12, which indicates that the obtained product was a PS-Ag non-rotational axisymmetric bowl-shaped bifacial micro-nano motor.
Example 7
Adjusting the thickness of the Ag layer in example 1 to 17nm, repeating the steps in example 1 to obtain a product, and characterizing the product by using the structure of a field emission scanning electron microscope product, as shown in FIG. 13, which indicates that the obtained product is a PS-Ag non-rotational axisymmetric bowl-shaped biconvex micro-nano motor.
Example 8
And (3) centrifuging and washing 1mg of PS-Pt hollow spherical double-surface particles (the diameter is 1 mu m, the thickness of the Pt layer is 25nm) for 3 times by using water, clarifying the supernatant, removing the supernatant, dropwise adding the residual precipitate into a culture dish in an ultrasonic dispersion manner, and drying for 24 hours at the temperature of 30 ℃ to obtain the product. As shown in fig. 14, the obtained product is a PS-Pt non-rotational axisymmetric bowl-shaped dihedral micro-nano motor.
Example 9
The drying time in example 1 was adjusted to 120h, and the procedure in example 1 was repeated to obtain the product. As shown in fig. 15, the obtained product is a PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor.
Example 10
The drying temperature in example 1 was adjusted to 60 ℃, and the procedure of example 1 was repeated to obtain a product. As shown in fig. 16, the obtained product is a PS-Ag non-rotational axisymmetric bowl-shaped dihedral micro-nano motor.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The non-rotational axis symmetrical bowl-shaped double-sided magic micro-nano motor is characterized by having a hollow bowl-shaped structure, a double-sided magic component, only one reflection plane and non-rotational symmetry.
2. The micro-nano motor according to claim 1, wherein the non-rotational axisymmetric bowl-shaped double-sided god micro-nano motor is obtained by collapse of hollow spherical double-sided god particles at a boundary of different material compositions.
3. The micro-nano motor according to claim 2, wherein the hollow spherical double-sided particle comprises a hollow spherical substrate and a semi-coating layer on the surface of the substrate, wherein the hollow spherical substrate has a particle size of 1-1.2 μm, and the thickness of the semi-coating layer is 15-30 nm.
4. The micro-nano motor according to claim 3, wherein the hollow spherical matrix substance is a polymer, and the semi-coating layer is a metal or a non-metal oxide.
5. The micro-nano motor according to claim 4, wherein the polymer is polystyrene, the metal is any one of Au, Ag and Pt, and the non-metal oxide is SiO2And TiO2Any one of them.
6. The preparation method of the non-rotational axisymmetric bowl-shaped bifacial magic micro-nano motor according to any one of claims 1 to 5, which is characterized by comprising the following steps:
dispersing the hollow spherical double-sided particles in the liquid 1 to enable the liquid 1 to be filled with the hollow spherical double-sided particles, and then drying the double-sided particles to obtain the non-rotational axis symmetrical bowl-shaped double-sided micro-nano motor; or the hollow spherical double-sided god particles filled with the liquid 1 are placed in the liquid 2 again for dispersion, and the non-rotational axis symmetrical bowl-shaped double-sided god micro-nano motor is obtained by stirring or drying or the combination of stirring and drying, wherein: the liquid 1 is ethanol, water or a poly dimethyl diallyl ammonium chloride aqueous solution; the liquid 2 is ethanol or water, and the liquid 1 is different from the liquid 2.
7. The method according to claim 6, wherein the hollow spherical Shuangshen particles are prepared by magnetron sputtering a semi-coating sputtering layer on a hollow spherical substrate.
8. The production method according to claim 7, wherein the hollow spherical substrate has a particle diameter of 1 to 1.2 μm, and the thickness of the sputtered layer is 15 to 30 nm; the hollow spherical matrix substance is a polymer, and the sputtering layer is metal or metal oxide.
9. The method of claim 6, wherein the concentration of the aqueous solution of poly (dimethyldiallylammonium chloride) is 0.01 to 0.12% by volume; the stirring time is 24-120 h; the drying time is 24-120 h, and the temperature is 30-60 ℃.
10. The non-rotational axisymmetric bowl-shaped bifacial magic micro-nano motor as claimed in any one of claims 1 to 5 is used as an artificial rotor for accelerating liquid mixing and mass transfer.
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