CN113353924A - Preparation method and application of fluorinated graphene photo-thermal conversion film for laser ignition - Google Patents
Preparation method and application of fluorinated graphene photo-thermal conversion film for laser ignition Download PDFInfo
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- CN113353924A CN113353924A CN202110864984.8A CN202110864984A CN113353924A CN 113353924 A CN113353924 A CN 113353924A CN 202110864984 A CN202110864984 A CN 202110864984A CN 113353924 A CN113353924 A CN 113353924A
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Abstract
The invention discloses a preparation method and application of a fluorinated graphene photo-thermal conversion film for laser ignition, which comprises the following steps: carrying out vacuum filtration on the graphene oxide solution to form a film so as to obtain a graphene oxide film; mixing the graphene oxide film with a fluoride solution, stirring, placing the mixture in a hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and carrying out a fluorination reaction to obtain a fluorinated graphene film; and cleaning and drying the fluorinated graphene film to obtain the fluorinated graphene photo-thermal conversion film for laser ignition. The invention solves the technical problem that the fluorinated graphene is difficult to form a film under simple conditions; compared with other photo-thermal materials, the fluorinated graphene has higher heat energy output under the illumination condition; the fluorinated graphene has excellent stability and excellent storage characteristics for energetic materials and devices. The fluorinated graphene film prepared by the method can realize laser ignition of energetic materials; the preparation steps are simple and easy to popularize.
Description
Technical Field
The invention belongs to the technical field of laser ignition, and particularly relates to a preparation method of a fluorinated graphene photo-thermal conversion film for laser ignition and application of the fluorinated graphene photo-thermal conversion film in laser ignition.
Background
Ignition and detonation of energetic materials are key to the proper functioning of the weapon system. With the development of the times, the reliability and safety of the ignition mode begin to receive attention. At present, the detonation technology of energetic materials realizes ignition mainly by energy in the forms of electric energy generation fragments, plasma, high temperature and the like reaching the ignition threshold value of the energetic materials. However, the safety of the ignition technology of the electric detonator is challenged due to the existence of static electricity, and a safe and reliable ignition mode needs to be developed.
The laser ignition is a technology for realizing the ignition of the energetic material by directly irradiating the energetic material by laser or irradiating the photo-thermal conversion material through a photo-thermal hot spot. The method has the advantages of high reliability, strong operability, high safety and the like, and is widely researched. However, the photothermal conversion material generally has the disadvantages of poor stability, poor photothermal conversion capability, poor storage performance and the like, so that the development of a photothermal material with high storage capability, high photothermal conversion capability and good stability is of great significance for the design of advanced laser ignition devices and systems.
Based on the above, the photo-thermal conversion film with the fluorinated graphene film for laser ignition is selected, so that on one hand, the fluorinated graphene has excellent photo-thermal conversion characteristics, storage property and stability, and meanwhile, the fluorinated graphene has better conductivity, and the sensitivity of an energetic material can be effectively reduced, which is of great significance for the design and application of advanced initiating explosive devices.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing a fluorinated graphene photo-thermal conversion film for laser ignition, comprising the steps of:
step one, carrying out vacuum filtration on a graphene oxide solution to form a film so as to obtain a graphene oxide film;
mixing the graphene oxide film with a fluoride solution, stirring, placing the mixture in a hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and carrying out fluorination reaction to obtain a fluorinated graphene film;
and step three, cleaning and drying the fluorinated graphene film to obtain the fluorinated graphene photo-thermal conversion film for laser ignition.
Preferably, the concentration of the graphene oxide solution is 0.1mg/mL-20 mg/mL.
Preferably, the fluoride solution is one or more of a hydrofluoric acid solution, an ammonium fluoride solution, a lithium fluoride solution, a sodium fluoride solution and a potassium fluoride solution.
Preferably, the fluoride solution has a concentration of 1 wt% to 40 wt%.
Preferably, in the second step, the stirring time is 30-45 min; the temperature of the fluorination reaction is 150-250 ℃ and the time is 12-96 h.
Preferably, the volume ratio of the graphene oxide solution to the fluoride solution is 1: 3.
Preferably, the process of the second step is replaced by: mixing the graphene oxide film with a fluoride solution, stirring, filling the mixture into a high-pressure-resistant polyvinyl chloride bag, putting the polyvinyl chloride bag into high-static-pressure treatment equipment, pressurizing to perform high-static-pressure treatment, then putting the polyvinyl chloride bag into a hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and performing fluorination reaction to obtain a fluorinated graphene film; and applying dual-frequency ultrasound while carrying out fluorination reaction in the hydrothermal reaction kettle.
Preferably, the fluoride solution is one or more of hydrofluoric acid solution, ammonium fluoride solution, lithium fluoride solution, sodium fluoride solution and potassium fluoride solution; the concentration of the fluoride solution is 1-40 wt%; the stirring time is 30-45 min; the temperature of the fluorination reaction is 150-250 ℃, and the time is 12-96 h; the alternating frequency of the double-frequency ultrasound is 30-45 kHz and 125-145 kHz, the time of the alternating processing of the double-frequency ultrasound is 60-120 s, and the power of the double-frequency ultrasound is 600-800W.
Preferably, in the third step, the obtained fluorinated graphene photothermal conversion film is placed in a low-temperature plasma processor for processing for 15-30 min, and the low-temperature plasma processor stops for 1-2 min after discharging for 1-2 min; the atmosphere of the low-temperature plasma processor is CF4(ii) a The frequency of the low-temperature plasma treatment instrument is 35-55 KHz, the power is 65-125W, and the pressure of the atmosphere is 30-60 Pa.
The invention also provides application of the fluorinated graphene photo-thermal conversion film for laser ignition in laser ignition.
The invention at least comprises the following beneficial effects: the technical scheme of the invention has the following advantages: the technical problem that the fluorinated graphene is difficult to form a film under simple conditions is solved; compared with other photo-thermal materials, the fluorinated graphene has higher heat energy output under the illumination condition; the fluorinated graphene has excellent stability and excellent storage characteristics for energetic materials and devices. The fluorinated graphene film prepared by the method can realize laser ignition of energetic materials; the preparation steps are simple and easy to popularize.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
fig. 1 is a raman spectrum of a fluorinated graphene photo-thermal conversion film prepared in example 1 of the present invention;
FIG. 2 is a transient high temperature curve diagram of a fluorinated graphene photo-thermal conversion film prepared in embodiments 1-5 of the present invention;
FIG. 3 is a transient high temperature curve diagram of a fluorinated graphene photo-thermal conversion film prepared in embodiments 1, 5-8 of the present invention;
fig. 4 is a laser ignition photograph of the fluorinated graphene photo-thermal conversion film prepared in example 1 of the present invention.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
a preparation method of a fluorinated graphene photo-thermal conversion film for laser ignition comprises the following steps:
step one, carrying out vacuum filtration on 5mL of 10mg/mL graphene oxide solution to form a film so as to obtain a graphene oxide film;
step two, mixing the graphene oxide film with 5mL of hydrofluoric acid with the concentration of 10 wt%, stirring, placing the mixture in a 50mL hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and carrying out fluorination reaction at the temperature of 200 ℃ for 48 hours; obtaining a fluorinated graphene film;
and step three, centrifuging, cleaning and drying the fluorinated graphene film to obtain the fluorinated graphene photo-thermal conversion film for laser ignition.
Example 2:
a preparation method of a fluorinated graphene photo-thermal conversion film for laser ignition comprises the following steps:
step one, carrying out vacuum filtration on 5mL of 10mg/mL graphene oxide solution to form a film so as to obtain a graphene oxide film;
step two, mixing the graphene oxide film with 10mL of hydrofluoric acid with the concentration of 10 wt%, stirring, placing the mixture into a 50mL hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and carrying out fluorination reaction at the temperature of 200 ℃ for 48 hours; obtaining a fluorinated graphene film;
and step three, centrifuging, cleaning and drying the fluorinated graphene film to obtain the fluorinated graphene photo-thermal conversion film for laser ignition.
Example 3:
a preparation method of a fluorinated graphene photo-thermal conversion film for laser ignition comprises the following steps:
step one, carrying out vacuum filtration on 5mL of 10mg/mL graphene oxide solution to form a film so as to obtain a graphene oxide film;
step two, mixing the graphene oxide film with 15mL of hydrofluoric acid with the concentration of 10 wt%, stirring, placing the mixture into a 50mL hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and carrying out fluorination reaction at the temperature of 200 ℃ for 48 hours; obtaining a fluorinated graphene film;
and step three, centrifuging, cleaning and drying the fluorinated graphene film to obtain the fluorinated graphene photo-thermal conversion film for laser ignition.
Example 4:
a preparation method of a fluorinated graphene photo-thermal conversion film for laser ignition comprises the following steps:
step one, carrying out vacuum filtration on 5mL of 10mg/mL graphene oxide solution to form a film so as to obtain a graphene oxide film;
mixing the graphene oxide film with 20mL of hydrofluoric acid with the concentration of 10 wt%, stirring, placing the mixture in a 50mL hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and carrying out a fluorination reaction at the temperature of 200 ℃ for 48 hours; obtaining a fluorinated graphene film;
and step three, centrifuging, cleaning and drying the fluorinated graphene film to obtain the fluorinated graphene photo-thermal conversion film for laser ignition.
Example 5:
a preparation method of a fluorinated graphene photo-thermal conversion film for laser ignition comprises the following steps:
step one, carrying out vacuum filtration on 5mL of 10mg/mL graphene oxide solution to form a film so as to obtain a graphene oxide film;
placing the graphene oxide film in a 50mL hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and reacting at the temperature of 200 ℃ for 48 hours; obtaining a graphene oxide film;
and step three, centrifuging, cleaning and drying the graphene oxide film to obtain the graphene oxide photo-thermal conversion film for laser ignition.
Example 6:
a preparation method of a fluorinated graphene photo-thermal conversion film for laser ignition comprises the following steps:
step one, carrying out vacuum filtration on 5mL of 10mg/mL graphene oxide solution to form a film so as to obtain a graphene oxide film;
mixing the graphene oxide film with 5mL of hydrofluoric acid with the concentration of 10 wt%, stirring, putting the mixture into a high-pressure-resistant polyvinyl chloride bag, putting the polyvinyl chloride bag into high-static-pressure treatment equipment, pressurizing to perform high-static-pressure treatment, putting the polyvinyl chloride bag into a 50mL hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and performing fluorination reaction to obtain a fluorinated graphene film; and applying dual-frequency ultrasound while carrying out fluorination reaction in the hydrothermal reaction kettle; the temperature of the fluorination reaction is 200 ℃, and the reaction time is 48 h; obtaining a fluorinated graphene film; the alternating frequency of the double-frequency ultrasound is 45kHz and 135kHz, the alternating processing time of the double-frequency ultrasound is 120s, and the power of the double-frequency ultrasound is 600W;
and step three, centrifuging, cleaning and drying the fluorinated graphene film to obtain the fluorinated graphene photo-thermal conversion film for laser ignition.
Example 7:
a preparation method of a fluorinated graphene photo-thermal conversion film for laser ignition comprises the following steps:
step one, carrying out vacuum filtration on 5mL of 10mg/mL graphene oxide solution to form a film so as to obtain a graphene oxide film;
step two, mixing the graphene oxide film with 5mL of hydrofluoric acid with the concentration of 10 wt%, stirring, placing the mixture in a 50mL hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and carrying out fluorination reaction at the temperature of 200 ℃ for 48 hours; obtaining a fluorinated graphene film;
step three, centrifuging, cleaning and drying the fluorinated graphene film to obtain the fluorinated graphene film for laserA fired fluorographene photo-thermal conversion film; placing the obtained fluorinated graphene photo-thermal conversion film in a low-temperature plasma processor for processing for 20min, and stopping the low-temperature plasma processor for 1 min after discharging for 1 min; the atmosphere of the low-temperature plasma processor is CF4(ii) a The frequency of the low-temperature plasma processor is 45KHz, the power is 120W, and the pressure of the atmosphere is 50 Pa;
example 8:
a preparation method of a fluorinated graphene photo-thermal conversion film for laser ignition comprises the following steps:
step one, carrying out vacuum filtration on 5mL of 10mg/mL graphene oxide solution to form a film so as to obtain a graphene oxide film;
mixing the graphene oxide film with 5mL of hydrofluoric acid with the concentration of 10 wt%, stirring, putting the mixture into a high-pressure-resistant polyvinyl chloride bag, putting the polyvinyl chloride bag into high-static-pressure treatment equipment, pressurizing to perform high-static-pressure treatment, putting the polyvinyl chloride bag into a 50mL hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and performing fluorination reaction to obtain a fluorinated graphene film; and applying dual-frequency ultrasound while carrying out fluorination reaction in the hydrothermal reaction kettle; the temperature of the fluorination reaction is 200 ℃, and the reaction time is 48 h; obtaining a fluorinated graphene film; the alternating frequency of the double-frequency ultrasound is 45kHz and 135kHz, the alternating processing time of the double-frequency ultrasound is 120s, and the power of the double-frequency ultrasound is 600W;
centrifuging, cleaning and drying the fluorinated graphene film to obtain a fluorinated graphene photo-thermal conversion film for laser ignition; placing the obtained fluorinated graphene photo-thermal conversion film in a low-temperature plasma processor for processing for 20min, and stopping the low-temperature plasma processor for 1 min after discharging for 1 min; the atmosphere of the low-temperature plasma processor is CF4(ii) a The frequency of the low-temperature plasma processor is 45KHz, the power is 120W, and the pressure of the atmosphere is 50 Pa;
testing the transient high temperature of the fluorinated graphene film prepared in the embodiment 1-8 by using an infrared testing system, placing the fluorinated graphene film on a laboratory bench, and then converging the light paths of the laser and the infrared temperature measuring system to one point; starting an infrared temperature measurement system to record real-time temperature, then starting laser irradiation for 100ms, and recording temperature pulse under the laser irradiation; as shown in fig. 2 to 3, the higher the transient high temperature (the higher the peak value), the better the laser ignition performance of the fluorinated graphene film, and the more favorable the laser ignition.
Testing laser ignition of the fluorinated graphene film prepared in example 1 by using an infrared test system, placing an energetic material (CL-20) below the fluorinated graphene film, and converging light paths of a laser and an infrared temperature measurement system to one point; the infrared temperature measurement system is started to record real-time temperature, then laser irradiation is started, the high-speed camera is started to record after the infrared temperature measurement system is started, then the picture is captured frame by frame, the result is shown in figure 4, and the fluorinated graphene film realizes laser ignition.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (10)
1. A preparation method of a fluorinated graphene photo-thermal conversion film for laser ignition is characterized by comprising the following steps:
step one, carrying out vacuum filtration on a graphene oxide solution to form a film so as to obtain a graphene oxide film;
mixing the graphene oxide film with a fluoride solution, stirring, placing the mixture in a hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and carrying out fluorination reaction to obtain a fluorinated graphene film;
and step three, cleaning and drying the fluorinated graphene film to obtain the fluorinated graphene photo-thermal conversion film for laser ignition.
2. The method for preparing a fluorinated graphene photothermal conversion film for laser ignition according to claim 1, wherein the concentration of the graphene oxide solution is 0.1mg/mL to 20 mg/mL.
3. The method for producing a fluorinated graphene photothermal conversion film for laser ignition according to claim 1, wherein the fluoride solution is one or more of a hydrofluoric acid solution, an ammonium fluoride solution, a lithium fluoride solution, a sodium fluoride solution, and a potassium fluoride solution.
4. The method for preparing a fluorinated graphene photo-thermal conversion film for laser ignition according to claim 1, wherein the concentration of the fluoride solution is 1 wt% to 40 wt%.
5. The preparation method of the fluorinated graphene photothermal conversion film for laser ignition according to claim 1, wherein in the second step, the stirring time is 30 to 45 min; the temperature of the fluorination reaction is 150-250 ℃ and the time is 12-96 h.
6. The method for producing a fluorinated graphene photo-thermal conversion film for laser ignition according to claim 1, wherein the volume ratio of the graphene oxide solution to the fluoride solution is 1: 3.
7. The method for preparing a fluorinated graphene photothermal conversion film for laser ignition according to claim 1, wherein the process of the second step is replaced by: mixing the graphene oxide film with a fluoride solution, stirring, filling the mixture into a high-pressure-resistant polyvinyl chloride bag, putting the polyvinyl chloride bag into high-static-pressure treatment equipment, pressurizing to perform high-static-pressure treatment, then putting the polyvinyl chloride bag into a hydrothermal reaction kettle, adding water to enable the filling rate of the hydrothermal reaction kettle to be 80%, and performing fluorination reaction to obtain a fluorinated graphene film; and applying dual-frequency ultrasound while carrying out fluorination reaction in the hydrothermal reaction kettle.
8. The method for producing a fluorinated graphene photothermal conversion film for laser ignition according to claim 7, wherein the fluoride solution is one or more of a hydrofluoric acid solution, an ammonium fluoride solution, a lithium fluoride solution, a sodium fluoride solution, and a potassium fluoride solution; the concentration of the fluoride solution is 1-40 wt%; the stirring time is 30-45 min; the temperature of the fluorination reaction is 150-250 ℃, and the time is 12-96 h; the alternating frequency of the double-frequency ultrasound is 30-45 kHz and 125-145 kHz, the time of the alternating processing of the double-frequency ultrasound is 60-120 s, and the power of the double-frequency ultrasound is 600-800W.
9. The method for preparing the fluorinated graphene photo-thermal conversion film for laser ignition according to claim 1, wherein in the third step, the obtained fluorinated graphene photo-thermal conversion film is placed in a low-temperature plasma processor for processing for 15-30 min, and the low-temperature plasma processor stops for 1-2 min after discharging for 1-2 min; the atmosphere of the low-temperature plasma processor is CF4(ii) a The frequency of the low-temperature plasma treatment instrument is 35-55 KHz, the power is 65-125W, and the pressure of the atmosphere is 30-60 Pa.
10. Use of the fluorinated graphene photothermal conversion film for laser ignition according to any one of claims 1 to 9 in laser ignition.
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