CN111044086B - Sensor for monitoring composite material liquid forming process and preparation method - Google Patents
Sensor for monitoring composite material liquid forming process and preparation method Download PDFInfo
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- CN111044086B CN111044086B CN201911336931.8A CN201911336931A CN111044086B CN 111044086 B CN111044086 B CN 111044086B CN 201911336931 A CN201911336931 A CN 201911336931A CN 111044086 B CN111044086 B CN 111044086B
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- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D5/00—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable
- G01D5/12—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable using electric or magnetic means
- G01D5/14—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable using electric or magnetic means influencing the magnitude of a current or voltage
- G01D5/18—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable using electric or magnetic means influencing the magnitude of a current or voltage by varying effective impedance of discharge tubes or semiconductor devices
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
Abstract
A sensor for monitoring a composite material liquid molding process and a preparation method thereof are characterized in that the preparation method comprises the following steps: (1) adding MXene powder into deionized water, and ultrasonically stripping to obtain an MXene lamellar monodisperse aqueous solution; (2) spraying the MXene lamellar monodisperse aqueous solution on the PU film, and drying in vacuum to obtain an MXene matrix film; (3) spraying the CNT monodisperse aqueous solution on the MXene matrix film, and drying in vacuum to obtain an MXene-CNT composite matrix film; (4) spraying the MXene lamellar monodisperse aqueous solution on the MXene-CNT composite matrix film, and drying in vacuum to obtain the MXene-CNT-MXene sandwich structure film; (5) and peeling the MXene-CNT-MXene sandwich structure film from the PU film, cutting the film into a circle, and arranging electrodes at two ends of the diameter to obtain the MXene/CNT sensor. The MXene/CNT sensor prepared by the method can be distributed and controlled at different positions of the composite material preformed body with any shape, and the real-time online monitoring of the LCM process mold filling process is carried out.
Description
Technical Field
The invention belongs to the field of nano composite materials, and particularly relates to a sandwich-structured MXene/CNT high-sensitivity sensor for monitoring a composite material liquid forming process and a preparation method thereof.
Background
The liquid molding (LCM) process of the composite material is suitable for manufacturing composite material structures with large sizes and complex shapes, has the advantages of strong designability, low cost and the like, and is widely applied to the fields of aerospace, ship industry, transportation and the like. The performance of LCM parts depends on the mold filling process of matrix resin to a great extent, and insufficient mold filling and impregnation can cause matrix defects of the composite material, so that the parts have the problems of layering, warping, poor mechanical properties and the like. Although a composite manufacturer will provide a "standard" process regime, this process regime is typically tailored to an ideal situation and does not necessarily suit the actual manufacturing process of the composite structure in the project. In order to ensure the quality of LCM products, the mold filling information of the resin in the manufacturing process needs to be accurately and effectively monitored on line in real time.
At present, the on-line monitoring technology for manufacturing the composite material mainly comprises a direct current method, a dielectric method, a piezoelectric method, an ultrasonic detection method and a fiber grating monitoring method. The fiber grating sensor has the characteristics of small size, high precision, good stability and the like, is considered to be most suitable for monitoring the manufacturing process of the composite material, but the size of the fiber grating sensor is still nearly two orders of magnitude larger than the diameter of the fiber, and when the fiber grating sensor is used as a sensing element and is embedded into the composite material, the defect is equivalently introduced into the composite material. Meanwhile, the fiber grating sensor has the defects of high cost, limited monitoring area and the like, which are all unfavorable factors for limiting the application of the fiber grating sensor in engineering. Although the Carbon Nanotube (CNT) sensor developed recently solves the internal defect of the composite material caused by the scale magnitude of the fiber grating sensor, and accurately monitors the impregnation process of resin to fibers in the prepreg forming process of the composite material, for LCM monitoring, as the resin flow in a larger degree erodes the carbon nanotube network, part of the carbon nanotubes leave the network and enter the fiber net rack, so that the overall stability of the sensor is damaged, and the high-precision monitoring of the whole process of filling the mold of the composite material cannot be ensured.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a novel transition metal carbide (MXene)/Carbon Nanotube (CNT) micro-nano sensor with a sandwich structure, which has high sensitivity, can be distributed and controlled on a curved surface, can be integrally formed with a composite material, is low in cost, is used for monitoring the liquid forming process of the composite material in real time, improving the problem of incomplete mold filling of a composite material component, providing beneficial guidance for material design, mold filling pressure regulation and process system formulation in the production of the composite material, and has important application value in practical engineering.
The invention discloses a preparation method of a sensor for monitoring a composite material liquid molding process, which comprises the following steps of:
(1) adding a certain amount of MXene powder into a certain amount of deionized water, and carrying out ultrasonic stripping to obtain an MXene lamella monodisperse aqueous solution; wherein the mass volume ratio of MXene powder to deionized water is 1: 2.67;
(2) spraying the MXene lamellar monodisperse aqueous solution on the treated Polyurethane (PU) film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene matrix film with the thickness of a; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 80-100 ℃, and the drying time is 1-2 h; the PU film is treated by repeatedly cleaning for 3-5 times with acetone, ethanol and deionized water;
(3) spraying the prepared CNT monodisperse aqueous solution on the obtained MXene matrix film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene-CNT composite matrix film with the thickness of b; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 80-100 ℃, and the drying time is 1-2 h;
(4) spraying the MXene lamellar monodisperse aqueous solution on the obtained MXene-CNT composite matrix film by using a high-pressure spray gun again, and drying in vacuum to obtain an MXene-CNT-MXene sandwich structure film with the thickness of c; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 80-100 ℃, and the drying time is 1-2 h;
(5) and peeling the MXene-CNT-MXene sandwich structure film from the PU film, cutting the film into a circle with the diameter of 2-10 mm, and arranging electrodes at two ends of the diameter of the circle film to obtain the MXene/CNT sensor.
The MXene/CNT sensor is arrayed in the composite material preforming body in a pre-buried mode, resin flows and is soaked into the sensor along with the progress of an LCM process, the resistance value of the sensor changes in real time, and the resin mold filling state is obtained through the resistance change rate-time response curve of the sensor.
The preparation method of the sensor for monitoring the composite material liquid molding process is as follows:
in the step (1), the transition metal carbide (MXene) is Ti3C2。
In the steps (2) to (4), the thickness a of the obtained MXene matrix film is 5-10 μm, the thickness b of the obtained MXene-CNT composite matrix film is 10-20 μm, and the thickness c of the obtained MXene-CNT-MXene sandwich structure film is 15-30 μm, wherein a < b < c.
In the step (3), the method for preparing the CNT monodisperse aqueous solution is a preparation method in patent CN2012104391772 (a method for preparing a temperature sensor based on a carbon nanotube three-dimensional network thin film).
In the step (5), the electrodes are arranged at two ends of the diameter of the circular film, namely, the metal copper wires are arranged at the edges of two ends of any diameter of the surface of the film through conductive silver paste.
Compared with the prior art, the invention has the advantages and beneficial effects that:
(1) the segment cross-linked reticular structure in the MXene/CNT sensor prepared by the method greatly increases the effective contact area between the conductive network and the composite material resin matrix, greatly improves the sensitivity of the sensor, and solves the problem of insufficient monitoring sensitivity of the existing sensing technology in a specific area and under specific conditions. And an MXene sheet layer in the MXene/CNT sensor can be laid in a direction parallel to the flowing direction of resin, so that the scouring force of the rapidly flowing resin on a CNT network in the sensor is reduced, the sensitivity and the overall stability of the sensor are ensured, the full impregnation process of a resin matrix on the reinforced fibers can be accurately responded, and the method is suitable for high-precision monitoring of the LCM process mold filling process of the fiber reinforced resin matrix composite material.
(2) The MXene/CNT sensor prepared by the method can be distributed and controlled at different positions of the composite material preformed body with any shape, the real-time online monitoring of the LCM process mold filling process is carried out, the precision and operability are very high, the method is safe and environment-friendly, the production efficiency is high, the cost of the sensor and a sensing signal demodulation system is low, and the popularization and the application are facilitated.
Drawings
FIG. 1 is a schematic microstructure diagram of an MXene-CNT-MXene sandwich structure film prepared by the method of the present invention; wherein, 1: an MXene layer; 2: a CNT layer; 3: and a PU layer.
FIG. 2 is a graph of resistance change rate versus time of an MXene/CNT sensor monitoring a resin mold filling process of a VARI process of a composite material in example 1 of the present invention.
Detailed Description
The invention is described in more detail below by way of example with reference to the accompanying drawings.
Fig. 1 shows the microstructure of the MXene-CNT-MXene sandwich structure film prepared in embodiments 1 to 4 of the present invention.
Example 1
The MXene powder in the examples of the present invention is Ti with a particle size of 200 mesh produced by Fusmann technologies (Beijing) Co., Ltd3C2The carbon nano tube is a multi-wall carbon nano tube with the diameter of 8-15 nm and the length of 50 mu m produced by Zhongkenao times Limited, the conductive silver paste is produced by Shenzhen Nabo electronic material Limited, the ethanol and the acetone are produced by Xinhe medicine group reagent company, the PU film is produced by Bairong medical material Limited, the composite material reinforcement is a single-layer 0.4 mm-thick unidirectional continuous glass fiber cloth produced by Yixing Fuxing glass fiber Limited, and the composite material matrix is T-158 type vinyl resin produced by Jinnan Changhua resin chemical industry Limited. The monitoring object is the resin filling process of a typical Vacuum Assisted Resin Infusion (VARI) process in LCM.
A preparation method of a sensor for monitoring a composite material liquid molding process comprises the following steps:
(1) adding 150mg of MXene powder into 400ml of deionized water, and carrying out ultrasonic treatment for 40min at the ultrasonic power of 80W to obtain a monodisperse aqueous solution of the MXene sheet layer;
(2) spraying the MXene lamellar monodisperse aqueous solution on the treated PU film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene matrix film with the thickness of 7 mu m; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 90 ℃, and the drying time is 1.5 h; the size of the PU film is 20mm multiplied by 50mm, and the PU film is processed in a way that acetone, ethanol and deionized water are repeatedly washed for 4 times;
(3) spraying the CNT monodisperse aqueous solution on the obtained MXene matrix film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene-CNT composite matrix film with the thickness of 14 mu m; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 90 ℃, and the drying time is 1.5 h; the preparation method of the CNT monodisperse aqueous solution refers to the method in patent CN 2012104391772;
(4) spraying the MXene lamellar monodisperse aqueous solution on the MXene-CNT composite matrix film by using a high-pressure spray gun, and drying in vacuum to prepare the MXene-CNT-MXene sandwich structure film with the thickness of 21 μm shown in figure 1; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 90 ℃, and the drying time is 1.5 h;
(5) peeling the MXene-CNT-MXene sandwich structure film from the PU film, cutting the film into a 5mm circle, and arranging a metal copper conductor at the edges of two ends of any diameter of the surface of the circular film through conductive silver paste, so as to arrange electrodes on the film, and obtain the MXene/CNT sensor.
The thickness of the MXene matrix film, the MXene-CNT composite matrix film and the MXene-CNT-MXene sandwich structure film prepared by the preparation method in this embodiment show an increasing relationship.
The MXene/CNT sensors obtained in the embodiment are arrayed between glass reinforced fiber layering layers of a composite material preforming body in a pre-buried mode, along with the progress of a VARI process, resin is poured into a vacuum mold, flows and is soaked into the sensors, the electronic tunneling effect of the sensors is changed, so that the resistance value of the MXene/CNT sensors is changed in real time, and the mold filling state of the resin in the process of preparing the continuous glass fiber reinforced vinyl composite material by using the VARI process is obtained through a sensor resistance change rate-time response curve shown in fig. 2. Wherein, starting from 0s, the rate of change of the sensor resistance Δ R/R0Holding the value at 0 indicates that the resin is not impregnated into the reinforcing fibers at the sensor monitor; at 54s, the rate of change of the sensor resistance Δ R/R0An abrupt change occurs, indicating an enhancement of the initial impregnation of the resin into the sensor site at that pointFibers; within the time period of 54-426 s, the resistance change rate delta R/R of the sensor0A continuous increase, indicating that the resin is continuously impregnating the reinforcing fibers where the sensor is monitoring; from 426s, the rate of change of the sensor resistance Δ R/R0A stable value is maintained substantially indicating that the reinforcing fibers at the sensor monitor have been fully impregnated with resin. The results monitored by the sensors are completely consistent with the comparative experimental results obtained by a direct observation method in the mold filling stage.
Example 2
The MXene powder in the examples of the present invention is Ti produced by Fusmann technologies (Beijing) Co., Ltd., having a particle size of 300 mesh3C2The carbon nano tube is a multi-wall carbon nano tube with the diameter of 8-15 nm and the length of 50 mu m produced by Zhongkenai Mingmo, the conductive silver paste is produced by Shenzhen Nabo electronic material, the ethanol and the acetone are produced by Xinhe medicine group reagent, the PU film is produced by Bairong medical material, the composite material reinforcement is woven basalt fiber cloth with the single-layer thickness of 0.6mm produced by Sichuan Tuxin research institute, and the composite material matrix is T-158 type vinyl resin produced by Jinan Changhua resin chemical industry, Inc. The monitoring object is the resin filling process of a typical Vacuum Assisted Resin Infusion (VARI) process in LCM.
The preparation method of the sandwich structure sensor for monitoring the composite material liquid forming process comprises the following steps:
(1) adding 300mg of MXene powder into 800ml of deionized water, and carrying out ultrasonic treatment for 1h at the ultrasonic power of 80W to obtain a monodisperse aqueous solution of the MXene sheet layer;
(2) spraying the MXene lamellar monodisperse aqueous solution on the treated PU film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene matrix film with the thickness of 10 mu m; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 100 ℃, and the drying time is 1 h; the size of the PU film is 20mm multiplied by 50mm, and the PU film is processed by repeatedly cleaning acetone, ethanol and deionized water for 5 times;
(3) spraying the CNT monodisperse aqueous solution on the obtained MXene matrix film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene-CNT composite matrix film with the thickness of 20 mu m; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 100 ℃, and the drying time is 1 h; the preparation method of the CNT monodisperse aqueous solution refers to the method in patent CN 2012104391772;
(4) spraying the MXene lamellar monodisperse aqueous solution on the MXene-CNT composite matrix film by using a high-pressure spray gun, and drying in vacuum to prepare the MXene-CNT-MXene sandwich structure film with the thickness of 30 μm shown in figure 1; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 100 ℃, and the drying time is 1 h;
(5) peeling the MXene-CNT-MXene sandwich structure film from the PU film, cutting the film into a 10mm circle, and arranging a metal copper conductor at the edges of two ends of any diameter of the surface of the circular film through conductive silver paste so as to arrange electrodes on the film, thus obtaining the MXene/CNT sensor.
The thickness of the MXene matrix film, the MXene-CNT composite matrix film and the MXene-CNT-MXene sandwich structure film prepared by the preparation method in this embodiment show an increasing relationship.
The MXene/CNT sensor obtained in the embodiment is arrayed between basalt reinforced fiber layering layers of a composite material pre-forming body in a pre-buried mode, along with the progress of a VARI process, resin is poured into a vacuum mould, flows and is soaked into the sensor, the electronic tunneling effect of the sensor is changed, and therefore the resistance value of the MXene/CNT sensor is changed in real time. And obtaining the mold filling state of the resin in the process of preparing the continuous basalt fiber reinforced vinyl composite material by utilizing the VARI process by monitoring the resistance change rate-time response curve of the sensor. Wherein the rate of change of the sensor resistance Δ R/R0Holding the value at 0 indicates that the resin is not impregnated into the reinforcing fibers at the sensor monitor; rate of change of resistance Δ R/R of subsequent sensor0A sudden change occurs, indicating that the resin begins to impregnate the reinforcing fibers at the sensor monitoring site; and then the rate of change of the resistance of the sensor is delta R/R0A continuous increase, indicating that the resin is continuously impregnating the reinforcing fibers where the sensor is monitoring; last sensor resistance change rate delta R/R0Substantially maintain a stable value, indicating sensing at that timeThe reinforcing fibers where the machine monitors have been fully impregnated with resin.
Example 3
The MXene powder in the examples of the present invention is Ti with a particle size of 200 mesh produced by Fusmann technologies (Beijing) Co., Ltd3C2The carbon nano tube is a multi-walled carbon nano tube with the diameter of 8-15 nm and the length of 50 microns, which is produced by Zhongkenao times Limited, the conductive silver paste is produced by Shenzhen Nabo electronic material Limited, the ethanol and the acetone are produced by Xinhe medicine group reagent company, the PU film is produced by Bairong medical material Limited, the composite material reinforcement is a single-layer unidirectional continuous glass fiber cloth with the thickness of 0.4mm, which is produced by Yixing Fuxing glass fiber Limited, and the composite material matrix is WS-105 type epoxy resin produced by Qingdao good innovative material Limited. The monitoring object is a resin filling process of a typical Resin Transfer Molding (RTM) process in LCM.
The preparation method of the sandwich structure sensor for monitoring the composite material liquid forming process comprises the following steps:
(1) adding 75mg of MXene powder into 200ml of deionized water, and carrying out ultrasonic treatment for 30min at the ultrasonic power of 80W to obtain a monodisperse aqueous solution of the MXene sheet layer;
(2) spraying the MXene lamellar monodisperse aqueous solution on the treated PU film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene matrix film with the thickness of 5 mu m; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 80 ℃, and the drying time is 2 h; the size of the PU film is 20mm multiplied by 50mm, and the PU film is processed in a mode of repeatedly cleaning for 3 times by acetone, ethanol and deionized water;
(3) spraying the CNT monodisperse aqueous solution on the obtained MXene matrix film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene-CNT composite matrix film with the thickness of 10 microns; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 80 ℃, and the drying time is 2 h; the preparation method of the CNT monodisperse aqueous solution refers to the method in patent CN 2012104391772;
(4) spraying the MXene lamellar monodisperse aqueous solution on the MXene-CNT composite matrix film by using a high-pressure spray gun, and drying in vacuum to prepare the MXene-CNT-MXene sandwich structure film with the thickness of 15 μm shown in figure 1; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 80 ℃, and the drying time is 2 h;
(5) peeling the MXene-CNT-MXene sandwich structure film from the PU film, cutting the film into a 2mm circle, and arranging a metal copper conductor at the edges of two ends of any diameter of the surface of the circular film through conductive silver paste, so as to arrange electrodes on the film, and obtain the MXene/CNT sensor.
The thickness of the MXene matrix film, the MXene-CNT composite matrix film and the MXene-CNT-MXene sandwich structure film prepared by the preparation method in this embodiment show an increasing relationship.
The MXene/CNT sensor obtained in the embodiment is arrayed between glass reinforced fiber layering layers of a composite material preforming body in a pre-buried mode, resin is poured into a mould along with the progress of an RTM (resin transfer molding) process, the resin flows and is soaked into the sensor, the electronic tunneling effect of the sensor is changed, and therefore the resistance value of the MXene/CNT sensor is changed in real time. And (3) obtaining the mold filling state of the resin in the process of preparing the continuous glass fiber reinforced epoxy composite material by using the RTM process by monitoring the resistance change rate-time response curve of the sensor. Wherein the rate of change of the sensor resistance Δ R/R0Holding the value at 0 indicates that the resin is not impregnated into the reinforcing fibers at the sensor monitor; rate of change of resistance Δ R/R of subsequent sensor0A sudden change occurs, indicating that the resin begins to impregnate the reinforcing fibers at the sensor monitoring site; and then the rate of change of the resistance of the sensor is delta R/R0A continuous increase, indicating that the resin is continuously impregnating the reinforcing fibers where the sensor is monitoring; last sensor resistance change rate delta R/R0A stable value is maintained substantially indicating that the reinforcing fibers at the sensor monitor have been fully impregnated with resin.
Example 4
The MXene powder in the examples of the present invention is Ti produced by Fusmann technologies (Beijing) Co., Ltd., having a particle size of 300 mesh3C2The carbon nanotube is a multiwalled carbon nanotube with a diameter of 8-15 nm and a length of 50 μm, which is produced by the China Ke nanometer time Co., LtdThe conductive silver paste is produced by Shenzhen Nambo electronic material Co., Ltd, the ethanol and the acetone are produced by Xinhe medicine group reagent Co., Ltd, the PU film is produced by Bairong medical material Co., Ltd, the composite material reinforcement is woven basalt fiber cloth with a single layer thickness of 0.6mm produced by Sichuan Tuoxin research institute, and the composite material matrix is WS-105 type epoxy resin produced by Qingdao Innovative material Co., Ltd. The monitoring object is a resin filling process of a typical Resin Transfer Molding (RTM) process in LCM.
The preparation method of the sandwich structure sensor for monitoring the composite material liquid forming process comprises the following steps:
(1) adding 225mg of MXene powder into 600ml of deionized water, and carrying out ultrasonic treatment for 50min at the ultrasonic power of 80W to obtain a monodisperse aqueous solution of the MXene sheet layer;
(2) spraying the MXene lamellar monodisperse aqueous solution on the treated PU film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene matrix film with the thickness of 8 mu m; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 100 ℃, and the drying time is 1.5 h; the size of the PU film is 20mm multiplied by 50mm, and the PU film is processed by repeatedly cleaning acetone, ethanol and deionized water for 5 times;
(3) spraying the CNT monodisperse aqueous solution on the obtained MXene matrix film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene-CNT composite matrix film with the thickness of 16 mu m; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 100 ℃, and the drying time is 1.5 h; the preparation method of the CNT monodisperse aqueous solution refers to the method in patent CN 2012104391772;
(4) spraying the MXene lamellar monodisperse aqueous solution on the MXene-CNT composite matrix film by using a high-pressure spray gun, and drying in vacuum to prepare the MXene-CNT-MXene sandwich structure film with the thickness of 24 μm shown in figure 1; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 100 ℃, and the drying time is 1.5 h;
(5) peeling the MXene-CNT-MXene sandwich structure film from the PU film, cutting the film into a circle of 8mm, and arranging a metal copper conductor at the edges of two ends of any diameter of the surface of the circular film through conductive silver paste so as to arrange electrodes on the film, thus obtaining the MXene/CNT sensor.
The thickness of the MXene matrix film, the MXene-CNT composite matrix film and the MXene-CNT-MXene sandwich structure film prepared by the preparation method in this embodiment show an increasing relationship.
The MXene/CNT sensor obtained in the embodiment is arrayed between basalt reinforced fiber layer layers of a composite material preforming body in a pre-buried mode, along with the progress of an RTM technological process, resin is poured into a mould, flows and is soaked into the sensor, the electronic tunneling effect of the sensor is changed, and therefore the resistance value of the MXene/CNT sensor is changed in real time. And (3) obtaining the mold filling state of the resin in the process of preparing the continuous basalt fiber reinforced epoxy composite material by using the RTM process by monitoring the resistance change rate-time response curve of the sensor. Wherein the rate of change of the sensor resistance Δ R/R0Holding the value at 0 indicates that the resin is not impregnated into the reinforcing fibers at the sensor monitor; rate of change of resistance Δ R/R of subsequent sensor0A sudden change occurs, indicating that the resin begins to impregnate the reinforcing fibers at the sensor monitoring site; and then the rate of change of the resistance of the sensor is delta R/R0A continuous increase, indicating that the resin is continuously impregnating the reinforcing fibers where the sensor is monitoring; last sensor resistance change rate delta R/R0A stable value is maintained substantially indicating that the reinforcing fibers at the sensor monitor have been fully impregnated with resin.
Claims (4)
1. The preparation method of the sensor for monitoring the composite material liquid forming process is characterized in that the sensor consists of a circular sandwich structure film and electrodes arranged at two ends of the diameter of the film, wherein the sandwich structure film consists of MXene-CNT-MXene sandwich structure film consisting of transition metal carbide and carbon nano tubes, and comprises the following steps of:
(1) adding a certain amount of transition metal carbide powder into a certain amount of deionized water, and carrying out ultrasonic stripping to obtain MXene lamella monodisperse aqueous solution; wherein the mass volume ratio of MXene powder to deionized water is 1: 2.67;
(2) spraying the MXene lamellar monodisperse aqueous solution on the treated PU film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene matrix film with the thickness of a; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 80-100 ℃, and the drying time is 1-2 h; the PU film is treated by repeatedly cleaning for 3-5 times with acetone, ethanol and deionized water;
(3) spraying the carbon nano tube monodisperse aqueous solution on the obtained MXene matrix film by using a high-pressure spray gun, and drying in vacuum to obtain an MXene-CNT composite matrix film with the thickness of b; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 80-100 ℃, and the drying time is 1-2 h;
(4) spraying the MXene lamellar monodisperse aqueous solution on the obtained MXene-CNT composite matrix film by using a high-pressure spray gun again, and drying in vacuum to obtain an MXene-CNT-MXene sandwich structure film with the thickness of c; wherein the vacuum degree of the vacuum drying oven is-0.06 MPa, the drying temperature is 80-100 ℃, and the drying time is 1-2 h;
(5) and peeling the MXene-CNT-MXene sandwich structure film from the PU film, cutting the film into a circle with the diameter of 2-10 mm, and arranging electrodes at two ends of the diameter of the circle film to obtain the MXene/CNT sensor.
2. The method of claim 1, wherein in step (1), the transition metal carbide is Ti3C2。
3. The method according to claim 1, wherein in the step, the thickness a of the obtained MXene matrix film is 5-10 μm, the thickness b of the MXene-CNT composite matrix film is 10-20 μm, and the thickness c of the MXene-CNT-MXene sandwich structure film is 15-30 μm, wherein a < b < c.
4. The method for preparing a sensor for monitoring a composite material liquid molding process according to claim 1, wherein in the step (5), the electrodes are arranged at two ends of the diameter of the circular film, and the metal copper wires are arranged at two end edges of any diameter of the surface of the film through conductive silver paste.
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