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    • 专利摘要:
    A layer-by-layer sample preparation method for aligning carbon nanotubes by utilizing an ultra-thin monolayer is provided in this invention, comprising the following steps: preparing a carbon nanotube solution by using the carbon nanotubes and a solvent; adding a matriX material solution to prepare a mixed solution with carbon nanotubes evenly dispersed; preparing a substrate; taking out a certain amount of the mixed solution to form an ultra-thin composite film of micron thickness on the substrate; annealing the thin film; and repeating the preparation of the ultra-thin composite film to obtain a carbon nanotube composite material composed of the multi-layer ultra-thin composite film. The method has; among others; the advantages that the carbon nanotubes are aligned and well dispersed in the composite material; and no dispersant is added in the preparation process; ensuring the purity of the composite material.
    公开号:NL2028543A
    申请号:NL2028543
    申请日:2021-06-25
    公开日:2022-02-28
    发明作者:Liu Qicheng；He Chunqing；Yin Chongshan
    申请人:Univ Changsha Science & Tech；
    IPC主号:
    专利说明:

    LAYER-BY-LAYER SAMPLE PREPARATION METHOD FOR ALIGNING CARBON NANOTUBES BY USING ULTRA-THIN MONOLAYER Field of the invention The invention relates to the technical field of carbon nanotube composite materials, in particular to a layer-by-layer sample preparation method for aligning carbon nanotubes by using an ultra-thin monolayer. Background of the invention Since the discovery of carbon nanotubes, scientists have attracted great attention because of their excellent physical properties, stable chemical properties, and special geometric shapes. Researchers often use pure carbon nanotubes or chemically modified carbon nanotubes as modified materials and dope into other materials to synthesize composite materials with excellent properties. Over the years, countless high-performance carbon nanotube composite materials have been developed. These composite materials have shown promising application prospects in many industries such as physics, chemistry, biology, aviation, construction, and machinery. With the progress of industrial technology, a variety of carbon nanotube composite materials have gradually entered the civilian field. So far, how to further improve the performance of carbon nanotubes and the development of new carbon nanotube composite materials are still extremely popular research fields in the world.
    In the development process of carbon nanotube composite materials, there are many types of doping methods of carbon nanotube, each with its own advantages and disadvantages. However, the dispersion and orientation of carbon nanotubes in materials has always been one of the most difficult points in the material preparation process. The first is the dispersion of carbon nanotubes. Carbon nanotubes have a special geometric shape. The radial dimension is on the order of nanometers and the axial dimension is on the order of micrometers. Whether it is a single-walled carbon nanotube or a multi-walled carbon nanotube, its length is much greater than its diameter. Therefore, under the action of thermal movement, carbon nanotubes are easily entangled with each other to form carbon nanotube clusters, and the formation of these clusters is almost inevitable. The formation of carbon nanotube clusters reduces the advantages of the special geometry of carbon nanotubes, and is not conducive to the uniformity of carbon nanotube composites. Clusters usually have a certain negative impact on the structure and overall performance of the material. In order to increase the dispersibility of carbon nanotubes in materials, people have come up with a variety of traditional methods for dispersing carbon nanotubes, which generally include mechanical stirring, ultrasonic treatment, adding dispersants, chemically modifying carbon nanotubes, etc.
    These methods can all play the role of dispersing carbon nanotubes, but there are some limitations.
    Then there is the problem of the orientation of carbon nanotubes.
    Also due to thermal movement, carbon nanotubes usually present a random arrangement and disordered orientation in the material, that is, an isotropic distribution.
    In some specific materials, such as films, ropes, etc., if the carbon nanotubes can be oriented and arranged, the material properties can be further improved (for example, the arrangement parallel to the rope in a rope-like material, it will be beneficial to the tensile strength of the rope). Therefore, in recent years, many people have begun to study the orientation method of carbon nanotubes.
    Common orientation methods of carbon nanotubes mainly include magnetic field orientation, electric field orientation, stretch modulation orientation, rubbing orientation, polymer extrusion orientation, etc.
    These methods can all play a role in aligning carbon nanotubes to a certain extent, but there are some limitations. 13 Prior art 1 First, a solution of carbon nanotubes and matrix material is prepared, that is, a mixed solution containing solvent, matrix material and carbon nanotubes.
    After preparing the required solution, first disperse the carbon nanotubes in the solution.
    The dispersion method is usually to add a dispersant and at the same time use physical dispersion method to maximize the dispersibility of the carbon nanotubes.
    For example, after adding a suitable carbon nanotube dispersant to the solution, the solution is mechanically stirred and ultrasonically treated for a period of time to obtain a mixed solution with uniformly dispersed carbon nanotubes.
    The orientation method of carbon nanotubes in solution usually adopts the technical method of applying an external field (magnetic field, electric field). Studies have shown that under certain temperature conditions, carbon nanotubes that can move freely in a strong magnetic or electric field tend to be aligned along the direction of the strong magnetic or electric field.
    Therefore, after applying a strong magnetic field or a strong electric field, the carbon nanotubes in the solution tend to be aligned parallel to the direction of the external field.
    Therefore, a mixed solution with aligned carbon nanotubes can be obtained by applying a strong magnetic field or a strong electric field.
    Finally, the external field is continuously applied, while the solvent in the mixed solution 1s volatilized (heating, blowing, standing, etc.), and finally a composite material with aligned carbon nanotubes inside is obtained.
    Disadvantages of prior art 1
    1. The carbon nanotube dispersant needs to be added to the mixed solution, and the residual dispersant in the composite material will have a certain impact on the material.
    2. A strong magnetic field or a strong electric field requires special equipment, so there are certain restrictions on using this method.
    3. The degree of orientation of carbon nanotubes by a strong magnetic field or a strong electric field is related to the size of the magnetic field or electric field, the viscosity of the solution, the orientation time, the length and diameter of the carbon nanotubes, etc. There are many influencing factors and restrictions.
    4. A strong magnetic field or a strong electric field may have some adverse effects on the matrix material.
    5. The solvent volatilization time of the mixed solution is long. During the solvent volatilization process, some carbon nanotubes are easy to agglomerate together due to thermal movement, and the dispersion degree decreases.
    13 Prior art 2 First, the carbon nanotube-doped composite material is prepared by traditional methods. The arrangement of carbon nanotubes in this composite material does not have orientation. Then use physical and mechanical methods to guide the arrangement of carbon nanotubes in the material. Commonly used mechanical modulation methods include: stretching (that is, stretching the composite material), friction (that is, rubbing the surface of the composite material in a fixed direction), extrusion (that is, squeezing the composite material out of the hole), and cutting (that is, cutting into the composite material in a fixed direction) and other methods. The common feature of the mechanical modulation method is that the carbon nanotubes tend to be aligned along the direction of the applied force due to mechanical action. For example, the orientation direction of the carbon nanotubes by stretching modulation is the stretching direction. Therefore, the mechanical modulation method can achieve the purpose of aligning carbon nanotubes within the influence range of force.
    Disadvantages of prior art 2
    1. The mechanical orientation process usually damages the composite material or changes the structure of the composite material.
    2. The carbon nanotubes outside the influence range of the force are not affected, and the uniformity of the prepared composite material is easily affected.
    Summary of the invention Aiming at the defects of the prior art, the present invention provides a layer-by-layer sample preparation method for aligning the carbon nanotubes by using an ultra-thin monolayer without adding a dispersant. When the length of the carbon nanotubes exceeds the thickness of the layer, limited by physical space, the carbon nanotubes in the ultra-thin monolayer tend to be aligned in the direction parallel to the monolayer. Taking advantage of this feature of ultra- thin monolayer, a special layer-by-layer sample preparation method is used to prepare a composite material with carbon nanotubes aligned and well dispersed.
    In order to achieve the above objectives, the technical solutions adopted by the present invention are as follows: A layer-by-layer sample preparation method for aligning carbon nanotubes by using an ultra-thin monolayer, characterized in that it comprises the following steps:
    1. Preparing a certain amount of carbon nanotubes and adding them to a solvent that is stable in nature and does not damage the structure of carbon nanotubes, and has a low boiling point, the solvent comprises water, ethanol, propanol and tetrahydrofuran, magnetically stirring for 2 hours, and ultrasonically dispersing for 4 hours to obtain a carbon nanotube solution;
    2. Preparing a certain amount of matrix material solution, the matrix material solution comprises Nafion solution, doping into the carbon nanotube solution; the doping amount of the carbon nanotube solution is not more than 20% of the matrix material solution to ensure good dispersion of carbon nanotubes; Dispersing the carbon nanotubes in a dispersion solution using mechanical stirring or ultrasonic treatment to obtain a mixed solution with carbon nanotubes evenly dispersed;
    3. Preparing a substrate of sufficient size and placing it horizontally, the substrate material comprises silicon wafer and quartz wafer;
    4. Taking out a certain amount of mixed solution according to the content of the matrix material and carbon nanotubes in the mixed solution; the mixed solution taken out should be just enough to form a micron-sized ultra-thin composite film on the substrate; The specific thickness is adjusted according to the length of the carbon nanotubes used, the thickness is required to be less than the length of the carbon nanotubes used, and the thickness is in the range of 0.5-50um;
    5. Applying evenly the mixed solution taken out on the substrate using a spreader and standing to form a film; and controlling the temperature, humidity and blast conditions during the film formation process as needed,
    6. Obtaining a micron-sized ultra-thin composite film; and annealing the film to stabilize the structure of the film;
    7. Repeating steps 4-6, the amount of mixed solution taken is equal each time;
    8. After repeating a certain number of times, a carbon nanotube composite material composed of multiple ultra-thin composite films is obtained.
    5 Preferably, the thickness of one composite film in step 4 is 1. lum, and the carbon nanotube composite material obtained by repeating 35 times in step 8 is 35 layers Preferably, the thickness of one composite film in step 4 is 0.8um, and the carbon nanotube composite material obtained by repeating 50 times in step 8 is 50 layers.
    Preferably, the thickness of one composite film in step 4 is 0.5um, and the carbon nanotube composite material obtained by repeating 80 times in step 8 is 80 layers.
    Compared with the prior art, the advantages of the present invention are as follows:
    1. The carbon nanotubes are aligned and well dispersed in the composite material.
    2. No dispersant is added during the preparation process, ensuring the purity of the composite material.
    3. The formation time of each monolayer is short, and the thermal movement time of carbon nanotubes is short, which weakens the agglomeration of carbon nanotubes and facilitates the dispersion of carbon nanotubes.
    4. The preparation is simple, no special large-scale equipment is needed, and the cost is low.
    Brief description of the drawings FIG. 1 is a flow chart of the preparation method of the carbon nanotube composite material in the embodiment of the present invention; FIG. 2 is a schematic diagram of the physical orientation mechanism of the ultra-thin monolayer to carbon nanotubes in the embodiment of the present invention; FIG. 3 is the surface topography of the carbon nanotube composite material in Example 1 of the present invention; FIG. 4 is the surface topography of the carbon nanotube composite material in Example 2 of the present invention; FIG. 5 is the surface topography of the carbon nanotube composite material in Example 3 of the present invention.
    Detailed description of the embodiments In order to make the objectives, technical solutions, and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and examples. As shown in FIG. 1, a layer-by-layer sample preparation method for aligning carbon nanotubes by using an ultra-thin monolayer, characterized in that it comprises the following steps:
    1. Preparing a solution of carbon nanotubes and matrix material, that is, a mixed solution containing a solvent, matrix material and carbon nanotubes.
    2. Dispersing the carbon nanotubes in the solution using physical methods, such as mechanical stirring and ultrasonic treatment, to obtain a mixed solution with carbon nanotubes well dispersed.
    3. Preparing a substrate of sufficient size (such as silicon wafer, quartz wafer, etc.) and placing it horizontally.
    4. Taking out a certain amount of mixed solution according to the content of the matrix material and carbon nanotubes in the mixed solution; the mixed solution taken out should be just enough to form a micron-sized ultra-thin composite film on the substrate; The specific thickness is adjusted according to the length of the carbon nanotubes used, the thickness is required to be less than the length of the carbon nanotubes used, and the thickness is in the range of 0.5-50um;
    5. Applying evenly the mixed solution taken out on the substrate using a spreader and standing to form a film; and controlling the temperature, humidity and blast conditions during the film formation process as needed;
    6. Obtaining a micron-sized ultra-thin composite film; and annealing the film to stabilize the structure of the film;
    7. Repeating steps 4-0, the amount of mixed solution taken is equal each time; and
    8. After repeating a certain number of times, a carbon nanotube composite material composed of multiple ultra-thin composite films is obtained. The material preparation steps are shown in FIG.1. The prepared carbon nanotube composite material is composed of multiple ultra-thin composite films. Since the length of the carbon nanotubes exceeds the thickness of the layer, the carbon nanotubes in the ultra-thin monolayer tend to be aligned 1n the direction parallel to the monolayer due to the limitation of physical space. Therefore, the carbon nanotubes in the composite material prepared by this method have the property of being aligned in the direction parallel to the ultra-thin monolayer. The schematic diagram is shown in FIG.2. Example 1
    21 mg of multi-walled carbon nanotubes (about 2um in length and 10-20 nm in diameter) was prepared, and added to 35 ml of tetrahydrofuran solvent, magnetically stirred for 2 hours, and ultrasonically dispersed for 4 hours to obtain a solution with carbon nanotubes well dispersed. 9ml of Nafion solution (DuPont, DE-520, EW 1100, perfluorosulfonic acid resin content of Swt%) was prepared, and doped into the carbon nanotube solution. The mixed solution was stirred and ultrasonically dispersed. The mixed solution was evaporated slightly during the ultrasonic treatment, and the final total volume was about 40ml. The mixed solution was evenly divided into 35 equal parts using a pipette.
    1. A portion of the mixed solution was taken and evenly coated on a quartz glass substrate (9cmx9cm), and the substrate was placed horizontally.
    2. The mixed solution was volatilized to form a film under normal temperature and humidity conditions.
    3. The mixed solution was formed a composite film with a thickness of about 1.1um on the substrate, and the film was vacuum annealed at 140°C for 1 hour.
    4. Steps 1-3 were repeated to prepare a carbon nanotubes/Nafion composite film composed of 35 ultra-thin monolayers.
    Due to the limitation of physical space, the carbon nanotubes in the ultra-thin monolayer (about 1.1 um) with a length on the order of micrometers tend to be aligned in the direction parallel to the monolayer. Therefore, the carbon nanotubes in the obtained composite material have the properties of oriented arrangement. The surface morphology of the prepared film is shown in FIG.3, the carbon nanotubes have good dispersibility, no obvious agglomeration, and tend to be distributed in the direction parallel to the surface of the ultra- thin monolayer.
    Example 2 21 mg of carbon nanotubes (about um in length and 10-20 nm in diameter) was prepared, and added to 35 ml of tetrahydrofuran solvent, magnetically stirred for 2 hours, and ultrasonically dispersed for 4 hours to obtain a uniformly dispersed solution of carbon nanotubes. 9ml of Nafion solution (DuPont, DE-520, EW 1100, perfluorosulfonic acid resin content of 5wt%) was prepared, and doped into the carbon nanotube solution. The mixed solution was stirred and ultrasonically dispersed. The mixed solution was evaporated slightly during the ultrasonic treatment, and the final total volume was about 40ml. The mixed solution was evenly divided into 50 equal parts using a pipette.
    1. A portion of the mixed solution was taken and evenly coated on a quartz glass substrate (9cm*9cm)}, and the substrate was placed horizontally.
    2. The mixed solution was volatilized to form a film under normal temperature and humidity conditions.
    3. The mixed solution was formed a composite film with a thickness of about 0.8um on the substrate, and the film was vacuum annealed at 140°C for 1 hour.
    4. Steps 1-3 were repeated to prepare a carbon nanotubes/Nafion composite film composed of 50 ultra-thin monolayers.
    Due to the limitation of physical space, the carbon nanotubes in the ultra-thin monolayer (about 0.8m) with a length on the order of micrometers tend to be aligned in the direction parallel to the monolayer. Therefore, the carbon nanotubes in the obtained composite material have the properties of oriented arrangement. The surface morphology of the prepared film is shown in FIG.4, the carbon nanotubes have good dispersibility, no obvious agglomeration, and tend to be distributed in the direction parallel to the surface of the ultra- thin monolayer.
    Example 3 21 mg of carbon nanotubes (about 2m in length and 10-20 nm in diameter) was prepared, and added to 35 ml of tetrahydrofuran solvent, magnetically stirred for 2 hours, and ultrasonically dispersed for 4 hours to obtain a uniformly dispersed solution of carbon nanotubes. 9ml of Nafion solution (DuPont, DE-520, EW 1100, perfluorosulfonic acid resin content of Swt%) was prepared, and doped into the carbon nanotube solution. The mixed solution was stirred and ultrasonically dispersed. The mixed solution was evaporated slightly during the ultrasonic treatment, and the final total volume was about 40ml. The mixed solution was evenly divided into 80 equal parts using a pipette.
    1. A portion of the mixed solution was taken and evenly coated on a quartz glass substrate (9cmx9cm)}, and the substrate was placed horizontally.
    2. The mixed solution was volatilized to form a film under normal temperature and humidity conditions.
    3. The mixed solution was formed a composite film with a thickness of about 0.54m on the substrate, and the film was vacuum annealed at 140°C for 1 hour.
    4. Steps 1-3 were repeated to prepare a carbon nanotubes/Nafion composite film composed of 80 ultra-thin monolayers.
    Due to the limitation of physical space, the carbon nanotubes in the ultra-thin monolayer (about 0.5um) with a length on the order of micrometers tend to be aligned in the direction parallel to the monolayer. Therefore, the carbon nanotubes in the obtained composite material have the properties of oriented arrangement. The surface morphology of the prepared film is shown in FIG5, the carbon nanotubes have good dispersibility, no obvious agglomeration, and tend to be distributed in the direction parallel to the surface of the ultra- thin monolayer. Those of ordinary skill in the art will realize that the embodiments described here are to help readers understand the implementation methods of the present invention, and it should be understood that the protection scope of the present invention is not limited to such special statements and embodiments. A person of ordinary skill in the art can make various other specific modifications and combinations without departing from the essence of the present invention based on the technical enlightenment disclosed in the present invention, and these modifications and combinations still fall within the protection scope of the present invention.
    Clause
    1. Alayer-by-layer sample preparation method for aligning carbon nanotubes by using an ultra-thin monolayer, characterized in that it comprises the following steps: a) Preparing a certain amount of carbon nanotubes and adding to a solvent, the solvent is stable in nature and does not damage the structure of carbon nanotubes, and has a low boiling point, the solvent comprises water, ethanol, propanol and tetrahydrofuran, magnetically stirring for 2 hours, and ultrasonically dispersing for 4 hours to obtain a solution of carbon nanotubes; b) Preparing a certain amount of matrix material solution, the matrix material solution comprises Nafion solution, mixing into the solution of carbon nanotubes; the doping amount of the solution of carbon nanotubes is not more than 20% of the matrix material solution to ensure good dispersion of carbon nanotubes, dispersing the carbon nanotubes in the dispersion solution using mechanical stirring or ultrasonic treatment to obtain a mixed solution with carbon nanotubes evenly dispersed; c) Preparing a substrate of sufficient size and placing horizontally, the substrate material comprises silicon wafer and quartz wafer; d) Taking out a certain amount of the mixed solution according to the content of the matrix material and carbon nanotubes in the mixed solution; the mixed solution taken out should be just enough to form a micron-sized ultra-thin composite film on the substrate; The specific thickness is adjusted according to the length of the carbon nanotubes used, the thickness is required to be less than the length of the carbon nanotubes used, and the thickness is in the range of 0.5-50um; e) Applying the mixed solution taken out evenly on the substrate using a spreader and standing to form a film; and controlling the temperature, humidity and blast conditions during the film formation process as needed; f) Obtaining a micron-sized ultra-thin composite film; and annealing the film to stabilize the structure of the film; g) Repeating steps 4-6, the amount of the mixed solution is equal each time; and h) After repeating a certain number of times, a carbon nanotube composite material composed of multiple ultra-thin composite films is obtained.
    2. The layer-by-layer sample preparation method for aligning carbon nanotubes by using an ultra-thin monolayer according to claim 1, wherein the thickness of one composite film in step 4 is l.lum, and the carbon nanotube composite material obtained by repeating 35 times in step 8 has 35 layers.
    3. The layer-by-layer sample preparation method for aligning carbon nanotubes by using an ultra-thin monolayer according to claim 1, wherein the thickness of one composite film in step 4 is 0.8um, and the carbon nanotube composite material obtained by repeating 50 times in step 8 has 50 layers.
    4. The layer-by-layer sample preparation method for aligning carbon nanotubes by using an ultra-thin monolayer according to claim 1, wherein the thickness of one composite film in step 4 is 0.5um, and the carbon nanotube composite material obtained by repeating 80 times in step 8 has 80 layers.
    权利要求:
    Claims (4)
    [1]
    A layer-by-layer sample preparation method for aligning carbon nanotubes using an ultra-thin monolayer, characterized in that the method comprises the following steps: a) Preparing a certain amount of carbon nanotubes and adding it to a solvent, wherein the solvent is naturally stable, does not damage the structure of the carbon nanotubes and has a low boiling point, and wherein the solvent comprises water, ethanol, propanol and tetrahydrofuran, magnetic stirring for two hours, and ultrasonic dispersing for four hours to form a solution from carbon nanotubes; b) preparing a predetermined amount of matrix material solution, wherein the matrix material solution comprises a Nafion solution, mixing with the solution of carbon nanotubes; wherein the doping amount of the solution of carbon nanotubes is not more than 20% of the matrix material solution to ensure good dispersion of carbon nanotubes; dispersing the carbon nanotubes in the dispersion solution by mechanical stirring or ultrasonic treatment to obtain a mixed solution with evenly dispersed carbon nanotubes; c) Preparing and horizontally placing a substrate of sufficient size, wherein the substrate material comprises silicon wafer and quartz wafer; d) Taking out a certain amount of a mixed solution depending on the amount of matrix material and carbon nanotubes in the mixed solution; wherein the taken out mixed solution must be just enough to form an ultrathin micron-sized composite film on the substrate; wherein the specific thickness is adapted to the length of the carbon nanotubes used, the thickness being less than the length of the carbon nanotubes used, and the thickness being between 0.5-50 µm; e) Evenly applying the extracted mixed solution to the substrate using a spreading element and allowing it to stand to form a film; and controlling the temperature, humidity and conditioning during the film forming process as needed; f) Obtaining an ultrathin micron size composite film; and controlled cooling of the film to stabilize the structure of the film;
    g) Repeating steps (d)-(f), the amount of the mixed solution being the same each time; and h) After a certain number of repetitions, obtaining a composite material of carbon nanotubes that is composed of a plurality of ultra-thin composite films.
    [2]
    The layer-by-layer sample preparation method for aligning carbon nanotubes using an ultra-thin monolayer according to claim 1, wherein the thickness of a composite film in step (d) is 1.1 µm, and wherein the composite material of carbon nanotubes is obtained by Repeat 35 times so that at step (h) the composite material has 35 layers.
    [3]
    The layer-by-layer sample preparation method for aligning carbon nanotubes using an ultra-thin monolayer according to claim 1, wherein the thickness of a composite film in step (d) is 0.8 µm, and the composite material of carbon nanotubes is obtained by 50 times iteration so that at step (h) the composite material has 50 layers.
    [4]
    The layer-by-layer sample preparation method for aligning carbon nanotubes using an ultra-thin monolayer according to claim 1, wherein the thickness of a composite film in step (d) is 0.5 µm, and the composite material of carbon nanotubes is obtained by 80 times iteration so that at step (h) the composite material has 80 layers.
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    同族专利:
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    引用文献:
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