CN-118324130-B - Graphene preparation device and preparation method adopting high-voltage pulse power supply

CN118324130BCN 118324130 BCN118324130 BCN 118324130BCN-118324130-B

Abstract

The invention discloses a graphene preparation device and a graphene preparation method adopting a high-voltage pulse power supply, wherein the preparation device comprises a sliding track, a fixed shell and a movable shell which are arranged on the sliding track, and a four-way pipe which is arranged between the fixed shell and the movable shell, wherein the four-way pipe is fixedly arranged on the sliding track, an upper port is connected to a nitrogen source, a left port is connected to one conductor, a right port is connected to the other conductor, the two conductors are respectively connected to a test current source, and the positive electrode of the high-voltage pulse power supply is arranged on the same side of the conductor as the positive electrode of the test current source. The method has the advantages of stable and rapid preparation, high graphene quality, simplicity and convenience in operation and the like, and can effectively solve the problems of long preparation time, unstable graphene quality and the like in the traditional method. Meanwhile, the method saves energy and raw materials, improves the preparation efficiency and performance index, and has higher practical value.

Inventors

WANG YULONG
YIN HUIPENG
LIU TONGJIANG
LI LILI
GUO NING
GAO JUNGUO

Assignees

哈尔滨理工大学

Dates

Publication Date: 20260505
Application Date: 20240329

Claims (6)

1. The graphene preparation device adopting the high-voltage pulse power supply is characterized by comprising a sliding track, a fixed shell and a movable shell which are arranged on the sliding track, and a four-way pipe which is arranged between the fixed shell and the movable shell, wherein the four-way pipe is fixedly arranged on the sliding track, an upper port is connected to a nitrogen source, a left port is connected to one conductor, and a right port is connected to the other conductor; the four-way pipe is a four-way glass pipe and is provided with an upper port, a lower port, a left port and a right port, and a sealing plug is arranged at the lower port of the four-way glass pipe; the graphite powder is placed in the middle of the four-way glass tube, and the movable shell is adjusted to drive the conductor to move towards the center, so that the graphite powder is tightly pressed together with the copper conductor at the other end, and the graphite powder is tightly pressed in the four-way glass tube as much as possible; The nitrogen is enabled to be filled in the four-way glass tube by adjusting the nitrogen flow controller; the high-voltage pulse power supply adopts a relay to control the on-off of high-voltage current; keeping the test current source on, and adding current to two sides of the graphite powder; The control circuit in the relay is set to be conducted for a certain time, and the high-voltage pulse power supply is conducted, so that high voltage is instantaneously applied to two sides of the graphite powder; The high-voltage pulse power supply is controlled to be turned off by setting the turn-off time of the relay, so that the high voltage is instantaneously disappeared, the circuit is turned off, the current is disappeared, and the temperature is instantaneously reduced.
2. The manufacturing apparatus according to claim 1, wherein the fixed housing and the movable housing are glass housings, respectively, a fixed member and a movable member provided on the slide rail.
3. The apparatus of claim 1, wherein the stationary housing and the movable housing are made of plexiglas.
4. The manufacturing apparatus according to claim 1, wherein one end of each of the conductors passes through the same side of the fixed housing or the movable housing and the connection terminal electrical connection member so as to be connected to a test current source or a high voltage pulse power source, and the other end is embedded in the four-way pipe.
5. The manufacturing apparatus according to claim 1, wherein the container is a glass bottle.
6. A method for preparing graphene by using a high-voltage pulse power supply, which is characterized in that the preparation method comprises the following steps based on the preparation device of any one of claims 1 to 5: Step1, placing graphite powder in the middle of a four-way pipe, and adjusting a movable shell to drive a conductor to move towards the center so as to jointly compress the graphite powder with the conductor at the other end, so that the graphite powder is compacted in the four-way pipe as much as possible; step 2, enabling nitrogen to be filled in the four-way glass tube by adjusting the nitrogen flow controller; step 3, the test current source is respectively connected to conductors at the left side and the right side through a left wiring terminal and a right wiring terminal, and meanwhile, the positive electrode of the high-voltage pulse power source is added at the same side of the copper conductor and the positive electrode of the test current source; step 4, wrapping the surface of the glass tube connected with the conductor at the other side of the four-way tube by copper foil, and connecting the other side of the high-voltage pulse power supply to the copper foil; Step 5, keeping the test current source on, and adding current to two sides of the graphite powder; step 6, switching on the high-voltage pulse power supply for a certain time by setting a control circuit in the relay so that high voltage is instantaneously applied to two sides of the graphite powder; step 7, when a high-voltage current passes through the graphite powder, the high temperature causes the volume expansion of the graphite powder; step 8, under the promotion of high-temperature and high-voltage current, graphite powder is gradually converted into graphene and is attached to the inner wall of the four-way glass tube; Step 9, the high-voltage pulse power supply is controlled to be turned off by setting the off time of the relay, so that the high voltage is instantaneously disappeared, the circuit is opened, the current is disappeared, and the temperature is instantaneously reduced; and 10, storing the graphene attached to the inner wall of the four-way pipe into a glass bottle connected with the lower side opening of the four-way pipe through vibration of an ultrasonic vibrator.

Description

Graphene preparation device and preparation method adopting high-voltage pulse power supply Technical Field The invention belongs to the technical field of graphene preparation, and particularly relates to a graphene preparation device and method adopting a high-voltage pulse power supply. Background Graphene, which is an innovative material, has excellent electrical conductivity, thermal conductivity, mechanical strength and chemical stability, and has great application potential in various fields such as biomedicine, electronic equipment, sensors, energy storage and the like. However, many technical difficulties remain in the mass production process, such as long preparation period, high cost, low efficiency, etc. Currently, methods for preparing graphene mainly include Chemical Vapor Deposition (CVD), chemical reduction, mechanical exfoliation, and the like. However, the conventional method for preparing graphene has limitations in that, firstly, the conventional chemical vapor deposition method requires high temperature and complicated equipment, resulting in long preparation period and high cost, which limits the large-scale application of graphene, secondly, the chemical reduction method-based preparation method requires the use of toxic reducing agents such as hydrazine hydrate, sodium borohydride, etc., which is poor in safety and causes adverse effects on the environment, and finally, the mechanical stripping method can obtain single-layer graphene, but has low production efficiency and high cost. In summary, there is a need for an efficient, low cost method for preparing graphene to achieve stable, rapid, and efficient graphene production. Disclosure of Invention In order to overcome the problems in the prior art, the invention provides a graphene preparation device and a graphene preparation method adopting a high-voltage pulse power supply. The invention provides a graphene preparation device adopting a high-voltage pulse power supply, which comprises a sliding track, a fixed shell, a movable shell, a four-way pipe, a nitrogen source, a conductor, a test current source and a test current source, wherein the fixed shell and the movable shell are arranged on the sliding track, the four-way pipe is arranged between the fixed shell and the movable shell and is fixedly arranged on the sliding track, an upper port is connected to the nitrogen source, a left port is connected to the conductor, a right port is connected to the other conductor, the two conductors are respectively connected to the test current source, and the positive electrode of the high-voltage pulse power supply is arranged on the same side of the conductor as the positive electrode of the test current source. In the embodiment of the invention, the fixed shell and the movable shell are both glass shells and are respectively a fixed piece and a movable piece which are arranged on the sliding track. Furthermore, the fixed shell and the movable shell are made of organic glass. In the embodiment of the invention, the four-way pipe is a four-way glass pipe and is provided with four ports, namely an upper port, a lower port, a left port and a right port, and a sealing plug is arranged at the lower port of the four-way glass pipe. In the embodiment of the invention, the conductors at the two ends of the four-way pipe are copper conductors. Further, one end of each conductor passes through the fixed shell or the movable shell at the same side and is electrically connected with the wiring terminal, so that the conductor is connected to a test current source or a high-voltage pulse power source, and the other end of each conductor is embedded into the four-way pipe. In the embodiment of the invention, the graphene packaging box further comprises a container connected to the lower port of the four-way pipe and used for storing graphene products, and the container is a glass bottle. Further, the device also comprises an ultrasonic vibrator connected to the lower port of the four-way pipe, and the ultrasonic vibrator vibrates so that the graphene attached to the inner wall of the four-way glass pipe is stored in a glass bottle connected to the lower port of the four-way glass pipe. In the embodiment of the invention, the glass shell is made of organic glass, has better transparency, chemical stability, mechanical property and weather resistance, is convenient for directly observing test phenomena, improves the understanding of test data and increases the safety of the test. Furthermore, the high-voltage pulse power supply adopts a relay to control the on-off of high-voltage current. As a second aspect of the present invention, there is provided a graphene preparation method using a high-voltage pulse power supply, based on the graphene preparation apparatus using a high-voltage pulse power supply, the preparation method comprising the steps of: Step1, placing graphite powder in the middle of a four-way pipe, and adjusting a movable shell to drive