CN109368628B - Ultrasound-assisted nano film preparation device and preparation method - Google Patents

Abstract

The invention discloses an ultrasonic-assisted nanometer film preparation device and a preparation method. The preparation device includes a piezoelectric transduction unit, a liquid storage groove for storing a suspension of nanomaterials, and a substrate. The bottom of the piezoelectric transduction unit is provided with a There is a four-dimensional adjustment platform, and the four-dimensional adjustment platform makes the piezoelectric transducer unit move in the directions of X-axis, Y-axis and Z-axis and rotate around the Z-axis; The radiating faces of the elements are connected and solidified as a whole. The present invention does not need to provide a special atmosphere range, and the equipment process is simple. In the process of film formation, the acoustic radiation force and acoustic flow and other nonlinear effects are generated by the ultrasonic field between the radiation surface of the piezoelectric transducer unit and the substrate. Nanomaterials are deposited and adsorbed on the surface of the substrate by force and acoustic cavitation, and the substrate undergoes reaction processes such as solvent evaporation and solute thermal decomposition, and finally forms a solid nanofilm on the substrate.

Description

Ultrasound-assisted nano film preparation device and preparation method

technical field

The invention relates to the technical field of nanomaterials, in particular to an ultrasonic-assisted nanometer film preparation device and a preparation method.

Background technique

Nano-film refers to the thin-film material formed by connecting and growing on the substrate with nanometer-sized (1-100nm) components, including thin-films composed of nano-sized sensitive functional materials (such as semiconductor materials, conductive polymers, etc.), Composite films formed by embedding nanocrystalline grains in films, and single-layer films or multi-layer composite films with a thickness of nanometers, etc., whose components are generally zero-dimensional or one-dimensional nanomaterials of 1 to 100 nm. Due to the specific structure and shape effect of nanomaterials in its thin film process, its carrier transport behavior, mechanical properties, magnetic, optical and thermal properties have undergone major changes. The performance of nano-sensitive thin films strongly depends on the particle size, film thickness, surface morphology and internal structure of the components. Compared with traditional macro-sized films, nano-sensitive films have unique properties such as superconductivity, giant Hall effect, and emission in the visible light region. The existing nano-sensitive film preparation methods are mainly divided into physical methods (vacuum evaporation method, sputtering deposition method, etc.) and chemical methods (chemical vapor deposition method, sol-gel method, electrochemical method, etc.).

In the existing nano-sensitive film production process, the traditional physical and chemical preparation methods have extremely strict requirements on the deposition or growth environment (high temperature or special atmosphere environment) of sensitive nano-materials, and there are complex equipment processes, high energy consumption, and high energy consumption. At the same time, it is difficult to control the thickness of the nano-film during the preparation process. Higher production cost and complex preparation process limit the popularization of nano-sensitive thin film technology.

Contents of the invention

Purpose of the invention: In order to overcome the deficiencies in the above-mentioned prior art, the present invention provides an ultrasonic-assisted nano-film preparation device and a preparation method. The preparation process is simple, low energy consumption and the thickness of the nano-film is easy to control during the preparation process.

Technical solution: The present invention is an ultrasonic-assisted nano-film preparation device, which includes a piezoelectric transduction unit, a liquid storage groove for storing nanomaterial suspensions and a substrate, and a four-dimensional adjustment platform is provided at the bottom of the piezoelectric transduction unit , the four-dimensional adjustment platform makes the piezoelectric transducer unit move in the direction of X axis, Y axis and Z axis and rotate around the Z axis; the liquid storage groove passes through the bonding layer and the radiation surface of the piezoelectric transducer unit Connect and solidify as a whole; the substrate is fixed in the liquid storage groove through the bracket and located below the liquid level of the nanomaterial suspension in the liquid storage groove or just in wetting contact with the liquid surface of the nanomaterial suspension , the substrate is kept at a certain distance from the bottom surface of the liquid storage groove and the substrate is not in contact with the liquid storage groove.

Further, the four-dimensional adjustment platform is set on a horizontal workbench, the substrate is parallel to the horizontal plane of the horizontal workbench, and the substrate is parallel to the radiation surface of the piezoelectric transducer unit.

Further, the support is fixed to the substrate and adjusts the lifting of the substrate.

Further, the internal structure of the liquid storage groove is one of cylinder, cuboid or hemisphere.

Further, the piezoelectric transducer unit adopts one of a single-layer piezoelectric sheet, a piezoelectric stack, or a sandwich ultrasonic transducer.

The present invention also provides a method for preparing an ultrasonically assisted nano film, comprising the steps of:

(1) Configure a nanomaterial suspension with a certain concentration and pour it into the liquid storage groove;

(2) Set the substrate in the liquid storage groove, and the substrate is not in contact with the liquid storage groove, adjust the position of the substrate so that the substrate is located below the liquid level of the nanomaterial suspension in the liquid storage groove Or just in contact with the liquid surface of the nanomaterial suspension;

(3) Turn on the piezoelectric transducer unit, adjust the resonance frequency between 10 and 100 kHz, and set the reaction time to 1 to 2 hours, so that an ultrasonic field is generated between the inner surface of the liquid storage groove and the substrate, and the liquid storage groove The nanomaterials in the groove will be evenly deposited and adsorbed on the surface of the substrate under the action of the ultrasonic field;

(4) Close the device, move the substrate out of the liquid storage groove, and then process the substrate through solvent evaporation and solute thermal decomposition, and finally form a solid nanomaterial film on the substrate.

Further, the thickness of the nanomaterial thin film is jointly adjusted by the deposition time of the nanomaterial and the resonance frequency of the piezoelectric transducer unit.

Beneficial effects: the preparation device of the present invention does not need to provide a special atmosphere range, the equipment process is simple, and the nonlinear effects such as acoustic radiation force and acoustic flow are generated by relying on the ultrasonic field between the piezoelectric transducer unit and the substrate during the film formation process, And with the help of acoustic radiation force and acoustic cavitation, nanomaterials are deposited and adsorbed on the surface of the substrate, and finally a solid film is formed on the substrate after reaction; the preparation method can be used to prepare semiconductor nanomaterials, metal nanomaterials, conductive polymer nanomaterials, etc. Nano-films such as materials have wide application fields, simple operation, and excellent effect; meanwhile, the preparation device and preparation method of the present invention have the advantages of no noise, good reliability, miniaturization, and low cost, and have certain promotional value.

Description of drawings

Fig. 1 is a structural schematic diagram of the ultrasonic-assisted nano-thin film preparation device of the present invention.

Detailed ways

The present invention will be further described below in conjunction with accompanying drawing and embodiment:

As shown in Fig. 1, a kind of ultrasonic-assisted nano film preparation device of the present invention comprises piezoelectric transduction unit 2, storage groove 3 and substrate 5 that store nanomaterial suspension 4, piezoelectric transduction unit 2 Use one of single-layer piezoelectric sheet, piezoelectric stack or sandwich ultrasonic transducer; the bottom of the piezoelectric transducer unit 2 is provided with a four-dimensional adjustment platform 1, and the four-dimensional adjustment platform 1 is set on a horizontal workbench. The electric transduction unit 2 can change its position along with the movement of the four-dimensional adjustment platform 1, that is, the four-dimensional adjustment platform 1 enables the piezoelectric transduction unit 2 to move along the X-axis, Y-axis and Z-axis of the Cartesian rectangular coordinate system and move around the Z-axis. shaft rotation; at the same time, ensure that the radiation surface of the piezoelectric transducer unit 2 is parallel to the horizontal plane of the horizontal table; the liquid storage groove 3 is connected with the radiation surface of the piezoelectric transducer unit 2 through the adhesive layer 7, and solidified as a whole ; The liquid storage groove 3 is used to store the nanomaterial suspension 4, and the internal structure of the groove can be one of a cylinder, a cuboid or a hemisphere and other three-dimensional geometric structures; the substrate 5 is fixed on the liquid storage by a support 6 In the groove 3, the support 6 and the substrate 5 are fixed and the substrate 5 is adjusted to rise and fall, so that the substrate 5 is located below the liquid level of the nanomaterial suspension 4 in the liquid storage groove 3 or just in contact with the nanomaterial suspension 4 liquid. surface wetting contact, the substrate 5 is parallel to the horizontal plane of the horizontal worktable and the substrate 5 is parallel to the radiation surface of the piezoelectric transducer unit 2, the substrate 5 is kept at a certain distance from the bottom surface of the liquid storage groove 3 and the substrate 5 is in contact with the storage tank 3. Fluid groove 3 has no contact.

The present invention also provides a method for preparing an ultrasonically assisted nano film, comprising the steps of:

(1) configure a nanomaterial suspension 4 with a certain concentration, and pour it into the liquid storage groove 3;

(2) Set the substrate 5 in the liquid storage groove 3, and the substrate 5 is not in contact with the liquid storage groove 3, adjust the position of the substrate 5 so that the substrate 5 is located in the liquid storage groove 3 and the nanomaterial is suspended Below the liquid level of the liquid 4 or just in contact with the liquid surface of the nanomaterial suspension 4;

(3) Turn on the piezoelectric transducer unit 2, adjust the resonant frequency between 10-100 kHz, set the response time to 1-2 hours, so that an ultrasonic field is generated between the inner surface of the liquid storage groove 3 and the substrate 5, The nanomaterials in the liquid storage groove 3 will be uniformly deposited and adsorbed on the surface of the substrate 5 under the action of the ultrasonic field;

(4) Close the device, move the substrate 5 out of the liquid storage groove 3, and then process the substrate 5 through solvent evaporation and solute thermal decomposition, and finally form a thin film of solid nanomaterials on the substrate 5. The thickness of the nanomaterial thin film is adjusted jointly by the deposition time of the nanomaterial and the resonance frequency of the piezoelectric transducer unit 2 .

The principle of the present invention: when the piezoelectric transducer unit 2 is turned on by the excitation voltage, vibration will be generated. Since the liquid storage groove 3 and the piezoelectric transducer unit 2 are solidified as a whole, the vibration generated by the piezoelectric transducer unit 2 will also At this time, an ultrasonic field will be formed in the gap between the bottom surface of the liquid storage groove 3 and the substrate 5, and the nonlinear effects such as acoustic radiation force and acoustic flow generated by the ultrasonic field will drive the storage The nanomaterials in the nanomaterial suspension 4 in the liquid groove 3 migrate. When the nanomaterials migrate to the vicinity of the substrate 5, the nanomaterials will be affected by multiple impacts such as strong shock waves or high-speed jets generated by acoustic radiation and acoustic cavitation. Under the influence of factors, the nanomaterials will be deposited and adsorbed on the surface of the substrate 5. After the deposition and adsorption of the nanomaterials on the surface of the substrate 5 is completed, the substrate 5 is removed from the liquid storage groove 3, and the deposited and adsorbed nanomaterials on the surface of the substrate 5 pass through The evaporation of the solvent and the thermal decomposition reaction process of the solute finally form a solid nano-film on the substrate 5; the thickness of the nano-film can be adjusted by adjusting the deposition and adsorption time of the nano-material and the resonance frequency of the piezoelectric transducer unit 2.

Example 1

The present embodiment is to utilize the present invention to prepare graphene film:

(1) configure a certain amount of graphene suspension with a concentration of 0.1mol/L, and pour it into the liquid storage groove 3;

(2) Adopt the PDMS film that has been ultrasonically cleaned by ethanol and deionized water successively as the substrate 5, and fix the substrate 5 on the support 6, set the substrate 5 in the liquid storage groove 3, and the substrate 5 No contact with the liquid storage groove 3, adjust the position of the substrate 5, so that the substrate 5 is completely infiltrated with the graphene suspension in the liquid storage groove 3;

(3) Turn on the piezoelectric transducer unit 2, adjust the resonant frequency to 50kHz, and set the reaction time to 1.5 hours, so that an ultrasonic field is generated between the inner surface of the liquid storage groove 3 and the substrate 5, and the graphene is suspended The graphene material in the liquid is transported to the vicinity of the substrate 5 under the action of nonlinear effects such as acoustic radiation force and acoustic flow generated by the ultrasonic field. Graphene will be evenly deposited and adsorbed on the surface of the substrate 5 under the action of multiple influencing factors such as high-speed jets;

(4) Close the device, move the substrate 5 out of the liquid storage groove 3, and then dry the substrate 5 under vacuum conditions at 70°C for 2 hours. After the solvent evaporates and the solute thermal decomposition reaction is completed, a Solid nanographene films. The thickness of the solid nano-graphene film is adjusted jointly by the deposition time of the nano-material and the resonance frequency of the piezoelectric transducing unit 2 .

Claims (5)

1. An ultrasonically assisted nano-film preparation device, characterized in that: it includes a piezoelectric transducer unit, a liquid storage groove and a substrate for storing a suspension of nanomaterials, and the bottom of the piezoelectric transducer unit is provided with a four-dimensional adjustment platform, the four-dimensional adjustment platform makes the piezoelectric transducer unit move in the directions of X-axis, Y-axis and Z-axis and rotate around the Z-axis; The substrate is connected to the surface and solidified as a whole; the substrate is fixed in the liquid storage groove through the bracket and is located below the liquid level of the nanomaterial suspension in the liquid storage groove or just infiltrated with the liquid surface of the nanomaterial suspension contact, the substrate is kept at a certain distance from the bottom surface of the liquid storage groove and the substrate is not in contact with the liquid storage groove, the four-dimensional adjustment platform is set on the horizontal worktable, and the substrate and the horizontal worktable The horizontal plane is parallel and the substrate is parallel to the radiating surface of the piezoelectric transducer unit, and the support is fixed to the substrate and adjusted to lift the substrate. 2 . The ultrasonic-assisted nano film preparation device according to claim 1 , wherein the internal structure of the liquid storage groove is one of a cylinder, a cuboid or a hemisphere. 3 . 3. A kind of ultrasonic-assisted nano-film preparation device according to claim 1, characterized in that: the piezoelectric transducer unit adopts single-layer piezoelectric sheet, piezoelectric stack or sandwich ultrasonic transducer A sort of. 4. An ultrasonic-assisted nano-film preparation method, characterized in that the ultrasonic-assisted nano-film preparation device described in any one of claims 1 to 3 comprises the steps of: (1) Configure a nanomaterial suspension with a certain concentration and pour it into the liquid storage groove; (2) Set the substrate in the liquid storage groove, and the substrate is not in contact with the liquid storage groove, adjust the position of the substrate so that the substrate is located below the liquid level of the nanomaterial suspension in the liquid storage groove Or just in contact with the liquid surface of the nanomaterial suspension; (3) Turn on the piezoelectric transducer unit, adjust the resonance frequency between 10 and 100 kHz, and set the reaction time to 1 to 2 hours, so that an ultrasonic field is generated between the inner surface of the liquid storage groove and the substrate, and the liquid storage groove The nanomaterials in the groove will be evenly deposited and adsorbed on the surface of the substrate under the action of the ultrasonic field; (4) Close the device, move the substrate out of the liquid storage groove, and then process the substrate through solvent evaporation and solute thermal decomposition, and finally form a solid nanomaterial film on the substrate. 5 . The ultrasonic-assisted nano-film preparation method according to claim 4 , wherein the thickness of the nano-material film is adjusted jointly by the deposition time of the nano-material and the resonance frequency of the piezoelectric transducer unit. 6 .

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