CN113441094B - Boron alkene-graphene composite aerogel and preparation and application thereof - Google Patents
Boron alkene-graphene composite aerogel and preparation and application thereof Download PDFInfo
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
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- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/12—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in capacitance, i.e. electric circuits therefor
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Abstract
The invention discloses a preparation method of a boron alkene-graphene composite aerogel and application of a pressure sensor thereof, and belongs to the technical field of sensors. The preparation method comprises the following steps: 1) Preparing boron alkene; 2) Preparing a boron alkene-graphene composite hydrogel; 3) Dialysis of the boron alkene-graphene composite hydrogel; 4) Freeze drying of the boron alkene-graphene composite hydrogel; 5) Preparing a boron alkene-graphene composite aerogel; 5) And packaging the pressure sensor. The boron alkene-graphene composite aerogel has a porous structure and excellent mechanical properties, can be used as an elastic dielectric layer, and is applied to research and development of high-sensitivity capacitance pressure sensors. The capacitance pressure sensor has a capacitance pressure of 0.89kPa in the range of 0 to 3kPa ‑1 A minimum detection force of 8.7Pa, and a response time of 110 ms. The whole preparation process of the boron alkene-graphene composite aerogel disclosed by the invention is simple, has multiple functions, and has a good application prospect in the field of pressure sensors.
Description
Technical Field
The invention relates to a boron alkene-graphene composite aerogel, a preparation method and application thereof, and belongs to the field of electronic material devices.
Background
Graphene is a two-dimensional material which is stripped from graphite and has single-atom thickness composed of carbon atoms, has good elasticity and good conductivity, and a mechanical device based on graphene has high sensitivity, so that the graphene material is widely applied to various flexible mechanical devices by scientists. The graphene aerogel has the characteristics of small density, high elasticity, strong adsorption and porous material, so that the graphene aerogel has a great application prospect in the aspects of mechanics and adsorption. The boron alkene is a new material which is more flexible, lighter, more stable and wider in application range than the graphene, has potential to combine with the graphene, and improves the electrical and mechanical stability.
The pressure sensor is the most commonly used sensor in industrial practice, is widely applied to various industrial self-control environments, and relates to various industries such as water conservancy and hydropower, railway traffic, intelligent building, production self-control, aerospace, military industry, petrochemical industry, oil well, electric power, ships, machine tools, pipelines and the like. The conventional pressure sensor mainly comprises a capacitive pressure sensor and a piezoresistive pressure sensor, and compared with the piezoresistive pressure sensor, the capacitive pressure sensor has the advantages of short response time, wide temperature range and the like. The capacitance pressure sensor also comprises a polar distance variable type and an area variable type, and compared with the area variable type, the polar distance variable type capacitance pressure sensor has small influence on a tested system and high sensitivity.
The existing Chinese patent 'a preparation method of three-dimensional nitrogen-boron co-doped graphene aerogel' (publication No. CN 160829929B) uses boron nitride as a nitrogen source and a boron source, adopts a hydrothermal method and freeze drying to prepare the graphene aerogel with higher adsorption performance, but the boron nitride does not have good elasticity, so that the aerogel elasticity is reduced. In addition, there is a chinese patent "a graphene pressure sensor and its structure and preparation method" (publication No. CN110207867 a), the sensor is composed of an interdigital electrode layer, a graphene-embedded elastic substrate layer, and a flexible encapsulation layer. The preparation process is complex, and excellent mechanical properties of the graphene are not fully exerted, so that the sensitivity of the sensor is low.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a preparation method of a boron alkene-graphene composite aerogel and application of a pressure sensor thereof. According to the invention, a liquid phase stripping method is adopted, the borane is prepared through ultrasonic grinding, and the composite aerogel is prepared through a hydrothermal method, so that the preparation process is simpler. In the invention, ammonia water and boron are used as nitrogen sources and boron sources, wherein the ammonia water also plays a role in reduction, and graphene oxide is reduced. The obtained aerogel has better conductivity and a porous honeycomb structure, greatly improves the elasticity of the aerogel, and simultaneously adopts a freeze-drying method to ensure that the aerogel is more stable, has simpler preparation process and is suitable for being used as a pressure sensor.
The invention also provides a preparation method of the boron alkene-graphene composite aerogel and application of the boron alkene-graphene composite aerogel in a pressure sensor, wherein the preparation method comprises the steps of preparing boron alkene, preparing boron alkene-graphene composite hydrogel, dialyzing the boron alkene-graphene composite hydrogel, preparing the boron alkene-graphene composite aerogel and application of the boron alkene-graphene composite aerogel in the field of the pressure sensor.
The invention relates to a boron alkene-graphene composite aerogel, which is mainly formed by compositing boron alkene and graphene, wherein two-dimensional boron alkene and graphene form a three-dimensional reticular aerogel structure together, and the atomic percentage ranges of C, O, N, B elements are 68% -70%, 10% -12%, 16% -18% and 4% -5% respectively.
The preparation method of the boron alkene-graphene composite aerogel provided by the invention can adopt the following steps:
1) Preparing a boron alkene-graphene mixed precursor solution: 5-15 mg of amorphous boron powder is ultrasonically crushed in 10-30 ml of DMF (N, N-dimethylformamide) solution for 3-5 hours at normal temperature, and centrifuged for 20-40 minutes at 3000-5000 rpm, and supernatant fluid is taken to obtain DMF solution dispersed with borane; adding graphene oxide into deionized water solution and continuously performing ultrasonic treatment to obtain a dispersion solution; preparing a mixed precursor solution, wherein the mass ratio of graphene oxide to ammonia water to DMF solution dispersed with the boron alkene to deionized water is (15-30): (600-700): (1800-1900). The preparation of the mixed precursor solution is to uniformly mix ammonia water, DMF solution dispersed with the boron alkene and the dispersion solution of the graphene oxide. The ammonia water is common ammonia water with the concentration of 25-28 percent (mass).
2) Preparation of a boron alkene-graphene composite hydrogel: adding the mixed precursor solution into a reaction kettle, and placing the reaction kettle into a baking oven to perform a hydrothermal reaction, wherein the temperature of the baking oven is 90-140 ℃ during the hydrothermal reaction, and the boron alkene-graphene composite hydrogel can be obtained after 8-10 hours of hydrothermal reaction; then mixing absolute ethanol and water with 1: preparing mixed dialysate according to the volume ratio of (90-110), and finally immersing the boron alkene-graphene composite hydrogel into the dialysate for dialysis, wherein the temperature is kept between 15-25 ℃ and the dialysis is carried out for 5-8 hours;
3) Preparation of a boron alkene-graphene composite aerogel: freezing the hydrogel obtained in the step 2) at-10 to-20 ℃ for 6 to 14 hours. Then freeze-drying is carried out under vacuum, the freeze-drying temperature is-40 ℃ to-30 ℃, and the boron alkene-graphene composite aerogel is obtained after drying for 18-24 hours;
the preparation method of the pressure sensor provided by the invention specifically comprises the following steps:
1) Pretreatment of the electrode; cleaning the electrode to remove impurities and greasy dirt on the surface of the electrode;
2) Preparation of gel electrolyte: preparing PVA solid powder and concentrated sulfuric acid into an aqueous solution, wherein the mass percentage ranges of PVA, concentrated sulfuric acid and deionized water are respectively (5-10): (1-2): (50-80), and heating and stirring in a water bath kettle at the temperature of 90-100 ℃ for 1-2 hours;
3) Preparation of a pressure sensor: brushing the gel electrolyte prepared in the step 2) on the electrode prepared in the step 1) to form a PVA adhesive film, soaking the boron alkene-graphene composite aerogel in the gel electrolyte for 5-15 min, and finally fixing the gel electrolyte on a metal sheet electrode through the PVA adhesive film to assemble the gel electrolyte into the metal sheet electrode: and (3) the electrode/PVA film/boron alkene-graphene composite aerogel/PVA film/electrode structure is placed in an oven for drying, the drying temperature is 30-50 ℃, and the drying time is 18-24 hours.
Preparation of a boron alkene-graphene composite aerogel and application principles of a pressure sensor thereof: the composite graphene aerogel is prepared from materials such as boron alkene, graphene and the like by a composite hydrothermal method, and two-dimensional boron alkene and two-dimensional graphene jointly form a boron alkene-graphene composite aerogel with a three-dimensional reticular aerogel structure. The two-dimensional boron alkene has good mechanical properties and electrical properties, has strengthened the mechanical stability of graphite alkene structure, has strengthened the electrical activity of graphite alkene. Therefore, compared with pure graphene aerogel, the boron alkene-graphene composite aerogel has more porous structures and better mechanical properties.
Compared with the prior art, the boron alkene-graphene composite aerogel has a porous honeycomb structure, has strong mechanical elasticity and stability, is simple in manufacturing process, and has good prospect in the application field of pressure sensing.
Drawings
FIG. 1 is an SEM image of a composite aerogel of a boron alkene and graphene in samples 1, 2 and 3 prepared in examples 1 and 2 of the present invention;
fig. 2 is a block diagram of a pressure sensor made in accordance with the present invention. Wherein 1 is an electrode; 2 is a boron alkene-graphene composite aerogel dielectric layer; 3 is a PVA film.
FIG. 3 is a graph of test results and sensitivity graphs of a pressure sensor assembled from the graphene-graphene composite aerogel prepared based on sample 1 of example 3;
FIG. 4 is a graph of test results and sensitivity graphs of a pressure sensor assembled from the graphene-graphene composite aerogel prepared based on sample 2 of example 3;
FIG. 5 is a graph of test results and sensitivity graphs of a pressure sensor assembled from the graphene-graphene composite aerogel prepared based on sample 3 of example 4;
FIG. 6 is a response time test plot of a pressure sensor assembled from a boron alkene-graphene composite aerogel prepared based on sample 3 of example 4;
FIG. 7 is a graph of the minimum pressure detection of a pressure sensor assembled from the boron alkene-graphene composite aerogel prepared based on sample 3 of example 4;
Detailed Description
The present invention will be described in further detail below in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be noted, however, that the detailed description herein is for the purpose of illustrating the invention only and is not intended to limit the scope of the invention. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as the terms of the art, and the terms used herein in the description of this invention are intended to be used only to describe specific embodiments and are not intended to limit the invention.
Example 1 preparation of a boron alkene-graphene composite aerogel
1) Preparing a boron alkene-graphene mixed precursor solution: ultrasonic pulverizing 10mg amorphous boron powder in 20ml DMF solution at normal temperature for 4 hours by a cell pulverizer, centrifuging at 4000rpm for 30 minutes, and collecting supernatant to obtain DMF solution dispersed with borane; adding graphene oxide into deionized water solution and continuously performing ultrasonic treatment to obtain a dispersion solution; preparing a mixed precursor solution sample 1 and a mixed precursor solution sample 2, wherein the mixed precursor solution sample 1 is as follows: the mass ratio range of graphene oxide, ammonia water and deionized water is 20:80:1800. as a comparative sample, sample 1 was not added with a DMF solution in which the borane was dispersed. Sample 2: the mass ratio of graphene oxide to ammonia water to DMF solution dispersed with the boron alkene to deionized water is 20:80:600:1800.
2) Preparation of a boron alkene-graphene composite hydrogel: adding the mixed precursor solution of the samples 1 and 2 into a reaction kettle, and placing the reaction kettle into an oven to perform hydrothermal reaction, wherein the temperature of the oven is 120 ℃ and the hydrothermal time is 10 hours during the hydrothermal reaction to obtain the boron alkene-graphene hydrogel; then mixing absolute ethanol and water with 1: preparing a mixed dialysate according to the volume ratio of 100, immersing the boron alkene-graphene composite hydrogel into the dialysate for dialysis, and keeping the temperature at 25 ℃ for 7 hours;
3) Preparation of a boron alkene-graphene composite aerogel: freezing the sample 1, 2 boron alkene-graphene composite hydrogel obtained in the step 2) at the temperature of minus 10 ℃ for 12 hours, and then carrying out vacuum freeze drying at the temperature of minus 30 ℃ for 24 hours to obtain sample 1, 2 boron alkene-graphene composite aerogel; sample 1 is actually a graphene aerogel.
The prepared boron alkene-graphene composite aerogel is formed by compositing materials such as boron alkene and graphene, and two-dimensional boron alkene and two-dimensional graphene form a three-dimensional reticular aerogel structure in a space, wherein atomic percentages of elements C, O, N of the sample 1 boron alkene-graphene composite aerogel are 70%, 12% and 18% respectively; the atomic percentages of the elements of the sample 2 boron alkene-graphene composite aerogel C, O, N, B are 69%, 10%, 17% and 4%, respectively. In fig. 1, (a) and (b) are SEM images of the sample 1 and 2, respectively, the graphene-graphene composite aerogel, it can be found that the interior is a three-dimensional network structure, and the sample 2 has a denser three-dimensional mesh than the interior of the sample 1.
Example 2 preparation of a boron alkene-graphene composite aerogel
1) Preparing a boron alkene-graphene mixed precursor solution: ultrasonic pulverizing 10mg of amorphous boron powder in 20ml of DMF solution at normal temperature for 4 hours, centrifuging at 4000rpm for 30 minutes, and collecting supernatant to obtain DMF solution dispersed with boron alkene; adding graphene oxide into an aqueous solution and continuously performing ultrasonic treatment to obtain a dispersion solution; preparing a mixed precursor solution sample 3, wherein the mass ratio of graphene, ammonia water, DMF solution dispersed with the boron alkene and deionized water in the sample 3 is 20:80:700:1800.
2) Preparation of a boron alkene-graphene composite hydrogel: adding the mixed precursor solution of the sample 3 into a reaction kettle, and placing the reaction kettle into an oven to perform hydrothermal reaction, wherein the temperature of the oven is 120 ℃ during the hydrothermal reaction, and the boron alkene-graphene hydrogel is obtained after 10 hours of hydrothermal reaction; absolute ethanol and water were mixed according to 1: preparing a mixed dialysate by volume ratio of 100, immersing the boron alkene-graphene hydrogel into the dialysate for dialysis, and keeping the temperature at 25 ℃ for 7 hours;
3) Preparation of a boron alkene-graphene composite aerogel: freezing the sample 3 boron alkene-graphene composite hydrogel obtained in the step 2) at the temperature of minus 10 ℃ for 12 hours, and then carrying out vacuum freeze drying at the temperature of minus 30 ℃ for 24 hours to obtain sample 3 boron alkene-graphene composite aerogel;
the boron alkene-graphene composite aerogel is formed by compositing boron alkene, graphene and the like, and the two-dimensional boron alkene and the two-dimensional graphene jointly form a three-dimensional reticular aerogel structure, and the atomic percentages of the C, O, N, B elements of the sample 3 boron alkene-graphene composite aerogel are 68%, 11%, 16% and 5% respectively. In fig. 1 (c), SEM images of the sample 3-graphene composite aerogel are shown, and it can be found that the interior is a three-dimensional network structure, and that the sample 3 has a denser three-dimensional mesh than the interior of samples 1 and 2.
Taken together with the comparison of examples 1, 2, and 3, it can be found that the sample 3-borane-graphene composite aerogel has denser three-dimensional meshes inside.
Example 3 preparation of pressure sensor
1) Pretreatment of the electrode: sequentially cleaning a sample by using distilled water, ethanol and acetone by taking a titanium sheet as an electrode to remove impurities and greasy dirt on the surface of the sample;
2) Preparation of gel electrolyte: preparing PVA solid powder and concentrated sulfuric acid into an aqueous solution, wherein the mass ratio of PVA to sulfuric acid to deionized water is 8:2:70, and heating and stirring in a water bath kettle at 90 ℃ for 1 hour;
3) Preparation of a pressure sensor: and (3) brushing the gel electrolyte prepared in step (2) on the electrode prepared in step (1) to form a PVA adhesive film, soaking the sample 1 and 2 boron alkene-graphene composite aerogel prepared in step (1) in the gel electrolyte for 10min, fixing the sample on a metal sheet electrode through the PVA adhesive film, assembling the electrode/PVA film/boron alkene-graphene composite aerogel/PVA film/electrode structure, and placing the electrode/PVA film/electrode structure in an oven for drying at 50 ℃ for 24 hours to obtain the sample 1 and 2 pressure sensor.
The following FIG. 2 shows a structure of a pressure sensor, wherein 1 is an electrode, 2 is a boron alkene-graphene composite aerogel dielectric layer, and 3 is a PVA film. Fig. 3 shows a capacitance change curve and a sensitivity curve of a pressure sensor based on sample 1 under different forces, the sensitivity is s=0.54 KPa -1 The detection limit interval is 20-2000Pa, and the fitting degree is 0.99. Fig. 4 shows a capacitance change curve and a sensitivity curve of a pressure sensor based on sample 2 under different forces, the sensitivity is s=0.72 KPa -1 The detection limit interval is 18-2000Pa, and the fitting degree is 0.99. Data comparison found that sample 2 based pressure sensor compared to sample 1 pressure sensorThe detector has higher sensitivity, larger detection limit range and better performance.
Example 4 preparation of pressure sensor
1) Cleaning an electrode: sequentially cleaning a sample by using distilled water, ethanol and acetone by taking a titanium sheet as an electrode to remove impurities and greasy dirt on the surface of the sample;
2) Preparation of gel electrolyte: preparing PVA solid powder and concentrated sulfuric acid into an aqueous solution, wherein the mass percentages of PVA, sulfuric acid and deionized water are respectively 8:2:70, and heating and stirring in a water bath kettle at 90 ℃ for 1 hour;
3) Preparation of a pressure sensor: and (3) brushing the gel electrolyte prepared in the step (2) on the electrode prepared in the step (1) to form a PVA adhesive film, soaking the sample 3-boron alkene-graphene composite aerogel prepared in the step (2) in the gel electrolyte for 10min, fixing the sample on a metal sheet electrode through the PVA adhesive film, assembling the electrode/PVA film/boron alkene-graphene composite aerogel/PVA film/electrode structure, and placing the electrode/PVA film/electrode structure in an oven for drying at a drying temperature of 50 ℃ for 24 hours to obtain the sample 3 pressure sensor.
Fig. 5 is a graph showing the capacitance change curve and sensitivity curve of the pressure sensor based on sample 3 under different forces, the sensitivity is s=0.89 KPa -1 The detection limit interval is 8.7-3000Pa, and the fitting degree is 0.99.
By combining examples 3 and 4, based on the measurement data of the pressure sensor in table 1, compared with the pressure sensors based on samples 1, 2 and 3, it can be found that the pressure sensor based on sample 3 has higher sensitivity, larger detection limit range and best performance.
TABLE 1
Example 5 detection of response time and minimum pressure
Combining examples 3 and 4, the sample 3 based pressure sensor was tested for response time, minimum pressure, and higher sensitivity.
1) A force of 0.25kPa was applied to the sample 3 pressure sensor by a press to detect response time. As shown in fig. 6, the response time of the acquired capacitance signal during the application of the force of 0.25kPa was 110ms, while the recovery time of the acquired capacitance signal during the unloading of the force was 180ms. Indicating that the pressure sensor has a faster response and recovery time.
2) The capacitive response of the sample 3 pressure sensor was detected by applying a minute pressure of 8.7Pa thereto. As can be seen in fig. 7, the sensor can still exhibit a good capacitive response when the sensor is subjected to a slight pressure of 8.7Pa.
The pressure sensor has the sensitivity of 0.89kPa at the highest in the stress range of 0-3 kPa -1 The response time was 110ms and the minimum stress detection was 8.7Pa.
In summary, the invention provides a preparation method of a boron alkene-graphene composite aerogel and application of a pressure sensor thereof. The preparation method comprises the steps of preparing the boron alkene by ultrasonic liquid phase stripping, preparing the aerogel by a hydrothermal method, and applying the aerogel to the field of pressure sensors. It should be noted that the application of the invention is not limited to the examples described above, but that modifications or variations can be made by a person skilled in the art from the description above, all of which modifications and variations are intended to fall within the scope of the invention as defined in the appended claims.
Claims (3)
1. The pressure sensor is a capacitive pressure sensor and comprises a boron alkene-graphene composite aerogel, wherein the boron alkene-graphene composite aerogel is mainly formed by compositing boron alkene and graphene, and two-dimensional boron alkene and graphene form a dense three-dimensional reticular aerogel structure together, wherein atomic percentages of C, O, N, B elements are respectively 68% -70%, 10% -12%, 16% -18% and 4% -5%; the preparation method of the boron alkene-graphene composite aerogel comprises the following steps:
1) Preparing a boron alkene-graphene mixed precursor solution: ultrasonically crushing 5-15 mg of amorphous boron powder in 10-30 ml of DMF (dimethyl formamide) solution for 3-5 hours, centrifuging at 3000-5000 rpm for 20-40 minutes, and taking supernatant to obtain a DMF solution dispersed with borane; adding graphene oxide into deionized water solution and continuously performing ultrasonic treatment to obtain a dispersion solution; preparing a mixed precursor solution, wherein the mass ratio of graphene oxide to ammonia water to DMF solution dispersed with the boron alkene to deionized water is (15-30): (600-700): (1800-1900);
2) Preparation of a boron alkene-graphene composite hydrogel: adding the mixed precursor solution into a reaction kettle for hydrothermal reaction, wherein the hydrothermal reaction temperature is 90-140 ℃, and the boron alkene-graphene composite hydrogel can be obtained after 8-10 hours of hydrothermal reaction; then mixing absolute ethyl alcohol and water according to the ratio of 1: mixing (90-110) by volume ratio to prepare a dialysate, and finally immersing the boron alkene-graphene composite hydrogel into the dialysate for dialysis, keeping the temperature between 15 and 25 ℃ and dialyzing for 5-8 hours;
3) Preparation of a boron alkene-graphene composite aerogel: freezing the hydrogel obtained in the step 2) at the temperature of minus 10 ℃ to minus 20 ℃ for 6-14 hours; and then freeze-drying is carried out under vacuum, the freeze-drying temperature is-40 ℃ to-30 ℃, and the boron alkene-graphene composite aerogel is obtained after drying for 18-24 hours.
2. The pressure sensor of claim 1, comprising an electrode/PVA film/borene-graphene composite aerogel/PVA film/electrode structure in sequence.
3. A method of manufacturing a pressure sensor according to claim 2, comprising the steps of:
1) Pretreatment of the electrode; cleaning the electrode to remove impurities and greasy dirt on the surface of the electrode;
2) Preparation of gel electrolyte: preparing PVA solid powder and concentrated sulfuric acid into an aqueous solution, wherein the mass ratio of PVA to concentrated sulfuric acid to deionized water is (5-10): (1-2): (50-80), and heating and stirring in a water bath kettle at the temperature of 90-100 ℃ for 1-2 hours;
3) Preparation of a pressure sensor: brushing the gel electrolyte prepared in the step 2) on the electrode prepared in the step 1) to form a PVA adhesive film, soaking the boron alkene-graphene composite aerogel in the gel electrolyte for 5-15 min, and finally fixing the boron alkene-graphene composite aerogel on the metal sheet electrode through the PVA adhesive film to assemble the metal sheet electrode: and (3) placing the electrode/PVA film/boron alkene-graphene composite aerogel/PVA film/electrode structure in an oven for drying, wherein the drying temperature is 30-50 ℃, and the drying time is 18-24 hours.
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