CN101792120B - Method for dispersing nanowires based on epoxy resin drawing film - Google Patents

Abstract

The invention discloses a method for dispersing nanowires based on epoxy resin film drawing, which is characterized in that the nanowires are first dispersed into a tetrahydrofuran solution, and then a silicon coupling agent is injected to make the inorganic reactive groups of the nanowires and the silicon coupling agent Unite and synthesize chemical bonds; inject epoxy resin into the coupling agent treatment solution, stir to dissolve, then inject polyamide resin, and stir again to dissolve it into a nanowire suspension; pass the nanowire suspension through a water bath to solidify the resin and mix with The organic reactive groups of the coupling agent unite to form chemical bonds; finally, the film is pulled by a mold, and then the resin film is transferred to a silicon or glass substrate to realize the dispersion of nanowires. The method of the invention is simple, low in cost and easy to realize.

Description

A Method for Dispersing Nanowires Based on Epoxy Resin Drawing Film

technical field

The invention relates to a method for dispersing nanowires, more specifically, a method for drawing a film with epoxy resin to disperse nanowires on a large scale, and is especially used in the industry of assembling nanometer devices.

Background technique

With the continuous maturity of nanomaterial synthesis technology and people's in-depth understanding of the unique properties of nanomaterials, the research focus of nanotechnology is gradually developing towards the practicality, deviceization and multifunctionalization of nanomaterials. In recent years, one-dimensional semiconductor nanomaterials represented by nanowires have gradually attracted people's attention for their potential application in the construction of micro/nanoelectronic devices. Since the United States "Science" (Science, 2001, volume 294, pages 1313-1317) has reported the basic principle of using p-type Si nanowires and n-type GaN nanowires as structural units to construct p-n junction diodes and finally realize logic gate circuits. Since computing, after several years of unremitting efforts, people have achieved great results in the development of nanometer devices. In the process of using nanowires to construct nanoelectronic devices, there are many problems restricting its development, and the most important problem is the manipulation of nanowires. Scientists have also contributed a lot to dispersing nanowires so far. For example, the British "Nature" (Nature, 2001, volume 409, pages 66-69) reported that the dielectrophoresis method disperses InP nanowires, and uses an external electric field to polarize the nanowires and make them follow a certain direction under the action of the electric field. to arrange. But the biggest hurdle to this approach is the need to pre-assemble the electrodes, and the polarized nanowires are easily bonded together under the action of an electric field. The US "Materials Chemistry" (Chemistry of Materials, 2005, Volume 17, Pages 1320-1324) reported the dispersion of magnetic nanowires by means of an external magnetic field, but the nanowires that can be dispersed by this technique are limited to magnetic nanowires . The US "Nanoletters" (Nanoletters, 2003, volume 3, pages 1229-1233) reported that the Langmuir-Blodgett method was used to disperse silver nanowires, and the nanowires suspended on the gas-liquid interface formed a thick nanowire by compressing the LB groove. The film transfers the nanowires from the gas-liquid interface to the solid substrate during immersion-lifting, and the nanowires are adsorbed to the substrate by van der Waals force and electrostatic force. Although this process can disperse nanowires on a large scale, the process is very complicated, and the process conditions are difficult to control and will be accompanied by bonding.

Contents of the invention

In order to avoid the shortcomings of the above-mentioned prior art, the present invention provides a method for drawing and dispersing nanowires based on epoxy resin, so as to overcome the defects of pre-assembled electrodes, external electric field or magnetic field, and complicated process.

The feature of the present invention is based on the method for epoxy resin drawing film to disperse nanowires is to operate according to the following steps:

a. Pretreatment

Dispersing the nanowires in a tetrahydrofuran solution, injecting a silicon coupling agent into the tetrahydrofuran solution containing the nanowires, and stirring evenly to obtain a coupling agent treatment solution;

b. Preparation of resin solution

Inject epoxy resin into the coupling agent treatment solution, stir to dissolve it; then inject polyamide resin, stir again to dissolve it into a nanowire suspension; place the nanowire suspension in a water bath at 25-35°C , so that the resin is cured to a curing viscosity of 12-25Pa.s;

c. Pulling film

The nanowire suspension treated in the water bath in the step b is pulled by a mold to form a film, and the resin film is transferred to a silicon wafer or a glass substrate to realize dispersion of the nanowires.

The present invention is based on the characteristics of the method of epoxy resin drawing film dispersion nanowire also in:

The step a is to disperse 3-4mg of nanowires into 4ml of tetrahydrofuran solution with ultrasound at room temperature, and the amount of the silicon coupling agent is 0.4-0.7ml;

The epoxy resin consumption in described step b is 2.8-3.2g, and the consumption of described polyamide resin is 2.0-2.8g,

The silicon coupling agent is KH560; the epoxy resin is E-44, and the polyamide resin epoxy resin is 650#. Compared with the prior art, the beneficial effects of the present invention are reflected in:

1. The present invention adopts a simple film pulling method. Compared with the existing dielectrophoresis and magnetic field methods, the operation process is simple and operable, and it overcomes the inconvenience caused by pre-assembling electrodes and using an external electric field or magnetic field;

2. Compared with the existing Langmuir-Blodgett method, the present invention avoids the limitation of the process in the operation process, and also overcomes the bonding phenomenon when the nanowires are dispersed;

3. The nanowires used in the method of the present invention are not limited by materials, and can be applied to nanowires of various materials;

4. The substrate used in the method of the present invention is only used as the substrate for carrying the nanowire resin film, so substrates of different materials can be selected as the substrate;

5. The reagents used in the method of the present invention are conventional reagents with low cost; meanwhile, the method of the present invention is simple to operate and easy to implement.

Description of drawings

Fig. 1 is the microscope photograph of silicon wafer magnified 1000 times after the film of embodiment 1 is drawn;

Fig. 2 is the microscope photograph of glass flake magnified 1000 times after drawing film of embodiment 2;

Fig. 3 is the microscope photograph of silicon wafer magnified 1000 times after the film of embodiment 3 is drawn;

Fig. 4 is the microscope photograph of silicon wafer magnified 1000 times after the film of embodiment 4 is drawn;

Provide specific implementation below, and further explain by accompanying drawing:

Detailed ways

Example 1

Follow the steps below to disperse CdS nanowires on a silicon substrate.

Step 1: Ultrasonic clean the silicon wafer in alcohol for 10 minutes at room temperature to remove the surface oil, then rinse with distilled water and set aside;

Step 2: Add 3-4mg of CdS nanowires and 4ml of tetrahydrofuran solution into a test tube with a volume of 15ml, and then perform ultrasonic dispersion treatment at room temperature; then inject 0.7ml of KH560 silicon coupling agent into the tetrahydrofuran solution containing nanowires , stir evenly to obtain a coupling agent treatment solution, in which the nanowires and the inorganic reactive groups of the coupling agent unite to form chemical bonds;

Step 3: Inject 3.2g of epoxy resin E-44 into the coupling agent treatment solution and stir for 5 minutes to completely dissolve epoxy resin E-44; then inject 2.0g of polyamide resin 650# into it and stir, The polyamide resin 650# was completely dissolved to obtain nanowire suspension, and the whole process was carried out in a water bath at 25° C.; the weight ratio of epoxy resin to polyamide resin was 1.6:1.

Step 4: Place the nanowire suspensions dissolved in epoxy resin E-44 and polyamide resin 650# in a water bath, set the temperature of the water bath to 25°C, and the water bath time to 25 hours to ensure that the test tube is well sealed. Prevent tetrahydrofuran from volatilizing; stir once every half an hour to make the resin and the organic reactive group of the coupling agent unite to form a strong chemical bond, and slowly solidify to make the viscosity reach 15-25Pa.s, so as to facilitate the improvement of the mold in the subsequent process. pull;

Step 5: Slowly pull the viscous solution with a comb-shaped mold, and keep it in the air for about 1 minute to form a resin film, in which the nanowires are regularly arranged in the direction of gravity; then transfer the resin film to a spare silicon wafer , to obtain well-dispersed CdS nanowires.

FIG. 1 is a micrograph of CdS nanowires dispersed on a silicon wafer in Example 1 at magnification of 1000 times. It can be seen from FIG. 1 that a regularly arranged array of CdS nanowires can be dispersed under the method of this example.

Example 2

Disperse CdS nanowires on a glass flake substrate as follows.

Step 1: Ultrasonic clean the glass sheet in alcohol for 10 minutes at room temperature to remove the surface oil, then rinse with distilled water and set aside;

Step 2: same as step 2 in Example 1;

Step 3: Inject 3.2g of epoxy resin E-44 into the coupling agent treatment solution and stir for 5 minutes to completely dissolve epoxy resin E-44; then inject 2.0g of 650# polyamide resin into it and stir, Dissolving the polyamide resin to obtain nanowire suspension, the whole process is carried out in a water bath at 35°C; the weight ratio of epoxy resin to polyamide resin is 1.6:1;

Step 4: Put the nanowire suspensions dissolved with epoxy resin E-44 and polyamide resin 650# respectively in a water bath, set the temperature of the water bath to 35°C, and the water bath time to 21 hours, and ensure that the test tube is well sealed , to prevent the volatilization of tetrahydrofuran; stir every half an hour to make the resin and the organic reactive group of the coupling agent unite to form a strong chemical bond, and slowly solidify to make the viscosity within the range of 15-25Pa.s;

Step 5: Slowly pull the solution with a viscosity of 15-25Pa.s with a comb-shaped mold, and keep it in the air for about 1 minute to form a resin film, in which the nanowires are regularly arranged in the direction of gravity; then the resin film Transfer to a spare glass slide to obtain well-dispersed CdS nanowires.

FIG. 2 is a microscope photo enlarged 1000 times of CdS nanowires dispersed on a glass sheet in Example 2. FIG. As shown in FIG. 2 , in this embodiment, a regularly arranged array of CdS nanowires can be dispersed.

Example 3

Follow the steps below to disperse CdS nanowires on a silicon substrate.

Step 1: same as Step 1 in Example 1;

Step 2: Add 3-4mg of CdS nanowires and 4ml of tetrahydrofuran solution into a test tube with a volume of 15ml, then perform ultrasonic dispersion treatment at room temperature, then add 0.4ml of coupling agent KH560 into the tetrahydrofuran solution containing nanowires, and stir evenly A coupling agent treatment solution is obtained, in which the nanowires and the inorganic reactive groups of the coupling agent unite to form strong chemical bonds;

Step 3: Inject 2.8g of E-44 epoxy resin into the coupling agent treatment solution, stir for 5 minutes to completely dissolve the epoxy resin, then inject 2.8g of 650# polyamide resin into it and stir to make the polyamide The amide resin is completely dissolved to obtain a suspension of nanowires, and the whole process is carried out in a water bath at 25°C; the weight ratio of epoxy resin to polyamide resin is 1:1;

Step 4: Place the nanowire suspensions dissolved in epoxy resin E-44 and polyamide resin 650# in a water bath, set the temperature of the water bath to 25°C, and the water bath time to 18 hours to ensure that the test tube is well sealed. Prevent tetrahydrofuran from volatilizing; stir once every half an hour to make the resin and the organic reactive group of the coupling agent unite to form a strong chemical bond, and slowly solidify to make the viscosity reach 15-25Pa.s;

Step 5: Slowly pull the viscous solution with a comb-shaped mold, and keep it in the air for about 1 minute to form a resin film, in which the nanowires are regularly arranged in the direction of gravity; then transfer the resin film to the place in step 1. On the spare silicon wafer, well-dispersed CdS nanowires were obtained.

FIG. 3 is a 1000 times magnified micrograph of CdS nanowires dispersed on a silicon wafer in Example 3. FIG. Fig. 3 shows that according to the method of this embodiment, a regularly arranged CdS nanowire array can be obtained by dispersing.

Example 4

Follow the steps below to disperse CdS nanowires on a silicon wafer substrate

Step 1: same as Step 1 in Example 1;

Step 2: Add 3-4mg of CdS nanowires and 4ml of tetrahydrofuran solution into a test tube with a volume of 15ml, then perform ultrasonic dispersion treatment at room temperature, then add 0.4ml of coupling agent KH560 to the tetrahydrofuran solution containing nanowires, and stir Uniform coupling agent treatment solution, in the coupling agent treatment solution, the nanowires and the inorganic reactive groups of the coupling agent unite to form a strong chemical bond;

Step 3: Inject 2.8g of E-44 epoxy resin into the coupling agent treatment solution and stir for 5 minutes to completely dissolve the E-44 epoxy resin; then inject 2.8g of 650# polyamide resin into it and stir Completely dissolve the polyamide resin to obtain nanowire suspension, the whole process is carried out in a water bath at 35°C; the weight ratio of epoxy resin to polyamide resin is 1:1;

Step 4: Put the suspension of nanowires dissolved in epoxy resin E-44 and polyamide resin 650# into a water bath, set the temperature of the water bath to 35°C, and the water bath time to 16 hours, and ensure that the test tube is sealed Good, prevent tetrahydrofuran from volatilizing; Stir every half an hour to make the resin and the organic reactive group of the coupling agent unite to form a strong chemical bond, and slowly solidify to make the viscosity reach 15-25Pa.s;

Step 5: Slowly pull the viscous solution with a comb-shaped mold, and keep it in the air for about 1 minute to form a resin film. The nanowires are regularly arranged in the resin film along the direction of gravity, and then the resin film is transferred to the place in step 1. On the prepared silicon wafer, well-dispersed CdS nanowires were obtained.

FIG. 4 is a microscope photo magnified 500 times of CdS nanowires dispersed on a silicon wafer in Example 4. FIG. Fig. 4 shows that according to the method of this embodiment, a regularly arranged CdS nanowire array can be obtained by dispersing.

Claims (2)

1. a method based on epoxy resin drawing film dispersion nanowire, it is characterized in that operate as follows: a. Pretreatment Dispersing the nanowires in a tetrahydrofuran solution, injecting a silicon coupling agent into the tetrahydrofuran solution containing the nanowires, and stirring evenly to obtain a coupling agent treatment solution; b. Preparation of resin solution Inject epoxy resin into the coupling agent treatment solution, stir to dissolve it; then inject polyamide resin, stir again to dissolve it into a nanowire suspension; place the nanowire suspension in a water bath at 25-35°C , and slowly solidify to make the viscosity reach 12-25Pa.s; c. Pulling film Pulling the nanowire suspension treated in the water bath in the step b into a resin film with a mold, and transferring the resin film to a silicon wafer or a glass substrate to realize dispersion of the nanowires; The step a is to disperse 3-4mg of nanowires into 4ml of tetrahydrofuran solution with ultrasound at room temperature, and the amount of the silicon coupling agent is 0.4-0.7ml; The amount of epoxy resin in the step b is 2.8-3.2g, the amount of polyamide resin is 2.0-2.8g; the nanowires are CdS nanowires. 2. The method for drawing and dispersing nanowires based on epoxy resin according to claim 1, characterized in that the silicon coupling agent is KH560; the epoxy resin is E-44, and the polyamide resin is 650#.

Images