CN115959908A - Method and device for uniformly growing graphene in carbon sliding block - Google Patents

Method and device for uniformly growing graphene in carbon sliding block Download PDF

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CN115959908A
CN115959908A CN202211561630.7A CN202211561630A CN115959908A CN 115959908 A CN115959908 A CN 115959908A CN 202211561630 A CN202211561630 A CN 202211561630A CN 115959908 A CN115959908 A CN 115959908A
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carbon
flash
graphene
slide block
sliding block
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CN115959908B (en
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魏文赋
周山刚
贾千喜
曾正洪
杨泽锋
高国强
吴广宁
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Southwest Jiaotong University
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Abstract

The invention discloses a method and a device for uniformly growing graphene in a carbon sliding block, which comprises the following steps: preparing a carbon slide block, carrying out discharge flash firing on the carbon slide block, and sintering the flash-fired slide block. Graphene can be uniformly grown in the carbon matrix through the flash firing step, and compared with the method of directly adding graphene into the carbon matrix in the preparation process, the problem that the graphene is not good in dispersity in the carbon matrix is solved. After sintering, the graphene grown in the carbon substrate can better connect carbon substrates together to form a complete carbon/graphite _ graphene _ carbon/graphite structure, so that the compression resistance, the breaking strength and the heat conduction performance of the carbon slide block are improved. The method is economical and convenient, and has low energy consumption.

Description

Method and device for uniformly growing graphene in carbon sliding block
Technical Field
The invention relates to the technical field of graphene carbon-based composite material preparation, in particular to a method and a device for uniformly growing graphene in a carbon sliding block.
Background
Graphene is a single-atom two-dimensional sheet material with a carbon atom hexagonal lattice, has excellent electrical conductivity, thermal conductivity, lubricity and mechanical properties, and becomes an excellent additive of a plurality of materials. The carbon sliding block is mainly applied to the pantograph slide plate in a high-speed rail pantograph system, the pantograph slide plate is a core component for acquiring energy of a train, the pantograph slide plate can normally work under the high-speed running condition of the train only by needing good electric conductivity, heat conductivity and mechanical property, and the preparation of the carbon slide plate material with good performance has important significance. After a very small amount of graphene is added in the process of preparing the carbon sliding plate substrate by related researchers, the electrical performance and the mechanical performance of the sliding plate are improved to a certain extent. However, graphene as a flaky nano material is easy to agglomerate in a matrix, the optimal effect of graphene modification cannot be achieved, and the preparation of the carbon sliding plate with uniformly dispersed graphene has important effects and values.
Disclosure of Invention
The invention aims to provide a method and a device for uniformly growing graphene in a carbon slide block, so as to solve the problem of nonuniform dispersion of the graphene in a carbon slide block matrix.
The technical scheme for solving the technical problems is as follows:
a method of uniformly growing graphene in a carbon slider, comprising the steps of:
step 1, preparing a carbon sliding block;
step 2, discharging and flashing the carbon slide block;
and 3, sintering the flash-burned slide block.
Further:
the method for preparing the carbon sliding block in the step 1 comprises the following steps: raw materials of asphalt coke, petroleum coke and carbon black are mixed according to the mass ratio of 3:3:2, crushing, screening, kneading, flaking, crushing and screening in sequence, and then pressing the screened powder into blocks by using a hydraulic press. The dimensions of the pressed slider were 100 x 35 x 20mm. Adding warm asphalt as a binder in the raw material kneading process, wherein the mass ratio of asphalt coke to warm asphalt is 3:1, the binder can well bond raw materials such as asphalt coke, petroleum coke and carbon black together, and the compactness of the material is improved.
The method for carrying out discharge flash on the carbon sliding block in the step 2 comprises the following steps: the prepared carbon sliding block is placed into a flash burning cavity, the voltage of the capacitor component is adjusted to flash the carbon sliding block in a discharging mode for 500-1000ms, the content of graphene in the carbon matrix is different due to different flash burning time, and uniformly dispersed graphene can be generated in the carbon matrix after flash sintering.
And 3, sintering the flash-burned slide block in a high-temperature sintering furnace. Specifically, the prepared sliding block is placed into a flash burning cavity, the voltage of the capacitor assembly is adjusted to discharge and flash the carbon sliding block, and the voltage of the capacitor is adjusted to be 400-450 v. The on-time of the relay switch is controlled by adjusting the output waveform of the signal generator into a pulse wave line, so as to control the discharge time, and the discharge time is controlled to be 500-1000 ms. And the vacuum environment is kept during sintering, so that the raw materials and graphene are prevented from being oxidized to reduce the performance of the carbon matrix, and the sintering time is 5-7 days.
The invention has the beneficial effects that: petroleum coke and carbon black in a carbon slider matrix are all raw materials with rich carbon content, the carbon matrix is discharged in a very short time through a capacitor component, instantaneous large current flows in the carbon matrix, the carbon matrix generates very high temperature through the current, after the carbon matrix is subjected to instantaneous high-temperature thermal annealing, chemical bonds around carbon atoms inside the carbon matrix are disordered and then recombined to generate uniformly dispersed graphene.
Further, the step of sintering the flash-burned sliding block comprises the step of placing the flash-burned sliding block into a high-temperature sintering furnace for sintering. After sintering, a large amount of gas in the carbon matrix is discharged, the tightness of the carbon matrix is improved, due to the fact that the graphene generated by flash firing can enable asphalt coke, petroleum coke and carbon black to be better connected together, a complete carbon/graphite _ graphene _ carbon/graphite structure is generated, and the tightness of the carbon matrix is further improved. Due to the introduction of the graphene in the carbon matrix, the electric conductivity, the heat conductivity and the mechanical property of the carbon matrix can be improved.
Also provided is an apparatus for uniformly growing graphene in a carbon slider, for use in the method, the apparatus comprising: the flash memory comprises a cuboid flash memory cavity, a capacitor assembly, a capacitor charging assembly, a capacitor discharging assembly and a direct current power supply. The rectangular flash-burning cavity is a box body formed by five acrylic glass plates, the top surface of the rectangular flash-burning cavity is not closed, the first round copper electrode and the second round copper electrode are respectively arranged on the acrylic glass plates on the two side edges, and the first round copper electrode and the second round copper electrode are respectively connected with the two ends of the capacitor assembly; the size of the inner dimension of the cuboid flash-burning cavity is 100 x 35 x 20mm, and the thickness of each acrylic glass plate is 3mm;
the capacitor assembly comprises a plurality of electrolytic capacitors connected in parallel and a diode connected in anti-parallel;
the capacitor charging assembly comprises a direct-current power supply, a resistor and a push type switch which are sequentially connected with the capacitor assembly; the rated voltage of the DC power supply is 800v, and when the switch is pressed, the power supply charges the capacitor through the resistor, and when the switch is released, the charging is stopped.
The capacitor discharging assembly comprises a signal generator, a millisecond-level relay switch and a direct current contactor which are sequentially connected; the direct current contactor is connected to the first round copper electrode; the millisecond relay switch is provided with a switching power supply. The relay switch is powered by the switching power supply, the output of the signal generator is adjusted to be a pulse waveform, the width of the pulse waveform is adjusted to control the on-time of the relay, and meanwhile, the relay switch controls the communication of the direct current contactor, so that the discharging time of the flash process is controlled.
Drawings
Fig. 1 is a schematic view of an apparatus for uniformly growing graphene in a carbon slider according to the present invention.
Wherein, 1, a cuboid flash chamber; 2. a capacitor component; 11. a first circular copper electrode; 12. a second circular copper electrode; 21. an electrolytic capacitor; 22. a diode; 23. a direct current power supply; 24. a resistance; 25. a push switch; 26. a signal generator; 27. a millisecond relay switch; 28. a direct current contactor; 29. and switching the power supply.
Fig. 2 is a schematic view of the microstructure of the prepared carbon slider.
Detailed Description
The specific technical scheme of the invention is described by combining the embodiment.
As shown in fig. 1, an apparatus for uniformly growing graphene in a carbon slider includes: the flash memory comprises a cuboid flash memory cavity 1, a capacitor component 2, a capacitor charging component, a capacitor discharging component and a direct-current power supply. The cuboid flash-firing cavity 1 is a box body formed by five acrylic glass plates, the top surface of the cuboid flash-firing cavity is not sealed, a first circular copper electrode 11 and a second circular copper electrode 12 are respectively arranged on the acrylic glass plates on the two side edges, and the first circular copper electrode 11 and the second circular copper electrode 12 are respectively connected with the two ends of the capacitor assembly 2; the internal dimension of the cuboid flash-firing cavity 1 is 100 × 35 × 20mm, and the thickness of each acrylic glass plate is 3mm;
the capacitor assembly 2 comprises a plurality of electrolytic capacitors 21 connected in parallel and a diode 22 connected in anti-parallel;
the capacitor charging assembly comprises a direct current power supply 23, a resistor 24 and a push type switch 25 which are sequentially connected with the capacitor assembly 2;
the capacitor discharging assembly comprises a signal generator 26, a millisecond relay switch 27 and a direct current contactor 28 which are connected in sequence; the direct current contactor 28 is connected to the first circular copper electrode 11; the millisecond relay switch 27 is provided with a switching power supply 29.
The following preparation process is carried out by adopting the device:
example 1
(1) Raw materials of asphalt coke, petroleum coke and carbon black are mixed according to the mass ratio of 3:3:2, sequentially crushing, screening, kneading, flaking, crushing and screening, adding warm asphalt as a binder in the raw material kneading process, wherein the mass ratio of asphalt coke to warm asphalt is 3:1, pressing the sieved powder into blocks by a hydraulic press.
(2) Put into the slider that the suppression obtained and dodge and burn in the cavity, then charge to 400v to the capacitor subassembly through pressing the switch, readjust signal generator output and be pulse waveform, pulse width is 500ms, opens switching power supply and begins to dodge to burn the carbon slider after that, dodges and burns the time and be 500ms.
(3) And (4) putting the flash-burned slide block into a high-temperature sintering furnace, vacuumizing the sintering furnace, and sintering at 1000 ℃ for 5 days.
Example 2
(1) Raw materials of asphalt coke, petroleum coke and carbon black are mixed according to the mass ratio of 3:3:2, sequentially crushing, screening, kneading, flaking, crushing and screening, adding warm asphalt as a binder in the raw material kneading process, wherein the mass ratio of asphalt coke to warm asphalt is 3:1, pressing the sieved powder into blocks by a hydraulic press.
(2) The slider that will suppress and obtain is put into and dodges and burns the cavity, then charges to 400v to the condenser subassembly through pressing the switch, and the output of readjustment signal generator is pulse waveform, and pulse width is 750ms, opens switching power supply and begins to dodge and burn the carbon slider after that, dodges and burns the time and is 750ms.
(3) And (3) putting the flash-burned slide block into a high-temperature sintering furnace, vacuumizing the sintering furnace, and sintering at 1000 ℃ for 5 days.
Example 3
(1) Raw materials of asphalt coke, petroleum coke and carbon black are mixed according to the mass ratio of 3:3:2, sequentially crushing, screening, kneading, flaking, crushing and screening, adding warm asphalt as a binder in the raw material kneading process, wherein the mass ratio of asphalt coke to warm asphalt is 3:1, pressing the sieved powder into blocks by a hydraulic press.
(2) Put into the slider that the suppression obtained and dodge and burn in the cavity, then charge to 400v to the capacitor subassembly through pressing the switch, readjust signal generator output and be pulse waveform, pulse width is 1000ms, opens switching power supply and begins to dodge to burn the carbon slider after that, dodges and burns the time and be 1000ms.
(3) And (4) putting the flash-burned slide block into a high-temperature sintering furnace, vacuumizing the sintering furnace, and sintering at 1000 ℃ for 5 days.
A schematic view of the microstructure of the carbon slider prepared is shown in fig. 2.
Comparative example 1
(1) Raw materials of asphalt coke, petroleum coke and carbon black are mixed according to the mass ratio of 3:3:2, crushing, screening, kneading, flaking, crushing and screening in sequence, and then pressing the screened powder into blocks by using a hydraulic press.
(2) And (3) putting the pressed sliding block into a high-temperature sintering furnace, vacuumizing the sintering furnace, and sintering at 1000 ℃ for 5 days.
Comparative example 2
(1) Raw materials of asphalt coke, petroleum coke and carbon black are mixed according to the mass ratio of 3:3:2, sequentially crushing, screening and kneading, adding 0.5wt% of graphene (which is purchased from the market and is uniformly dispersed by ultrasonic waves) in the kneading process, then flaking, crushing and screening, and pressing the screened powder into blocks by using a hydraulic press.
(2) And (3) putting the pressed sliding block into a high-temperature sintering furnace, vacuumizing the sintering furnace, and sintering at 1000 ℃ for 5 days.
The sliders prepared in the above examples and comparative examples were subjected to performance tests, and the results are shown in Table 1
TABLE 1 slider Performance test
Figure BDA0003984898320000041
Figure BDA0003984898320000051
As can be seen from table 1, in comparative example 1, the carbon matrix is directly pressed into a block and then sintered without introducing graphene, so that each property thereof is the lowest compared to the other two; in the comparative example 2, the graphene purchased in the market is added in the kneading process, and each performance of the graphene is improved to a certain extent compared with that of the comparative example 1, but is far lower than that of the graphene in examples 1, 2 and 3, because the performance of the graphene is not obviously improved due to the agglomeration phenomenon generated in the carbon matrix; examples 1, 2, and 3, which employ the apparatus and method of uniformly growing graphene in a carbon slider according to the present invention, have the best mechanical and electrical properties because the graphene generated to be uniformly dispersed in the carbon matrix forms a complete carbon/graphene _ carbon/graphite structure. In the three examples, the content of graphene in the carbon slider is different due to the difference of the control of the pulse time and the control of the flash time, and the content of graphene is increased with the increase of the flash time, in the three groups of examples, the performances of example 2 are obviously better than those of examples 1 and 3, because the content of graphene in example 1 is less, and the performances of example 3 are reduced due to graphitization of the carbon source in the carbon slider due to the overlong flash time and the overlong energy change rate.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (9)

1. A method for uniformly growing graphene in a carbon slider is characterized by comprising the following steps:
step 1, preparing a carbon sliding block;
step 2, discharging and flashing the carbon slide block;
and 3, sintering the flash-burned slide block.
2. The method for uniformly growing graphene in a carbon sliding block according to claim 1, wherein the step 1 of preparing the carbon sliding block comprises: raw materials of asphalt coke, petroleum coke and carbon black are mixed according to the mass ratio of 3:3:2, crushing, screening, kneading, flaking, crushing and screening in sequence, and then pressing the screened powder into blocks by using a hydraulic press.
3. The method for uniformly growing graphene in the carbon sliding block according to claim 2, wherein warm asphalt is added as a binder in the raw material kneading process, and the mass ratio of asphalt coke to warm asphalt is 3:1.
4. the method of claim 2, wherein the pressed slider has a dimension of 100 x 35 x 20mm.
5. The method for uniformly growing graphene in a carbon slider according to claim 1, wherein the step 2 of performing discharge flash on the carbon slider comprises: the prepared carbon sliding block is placed into a flash burning cavity, the voltage of the capacitor assembly is adjusted to flash the carbon sliding block in a discharging mode, the flash burning time is 500-1000ms, different graphene contents in the carbon matrix can be caused by different flash burning times, and uniformly dispersed graphene is generated in the carbon matrix after flash sintering.
6. The method for uniformly growing graphene in a carbon slide block according to claim 1, wherein the step 3 of sintering the flash-fired slide block comprises sintering the flash-fired slide block in a high-temperature sintering furnace.
7. The method of claim 6, wherein the sintering is performed in a vacuum environment for 5-7 days.
8. An apparatus for uniformly growing graphene in a carbon slider, for use in the method of any one of claims 1 to 7, the apparatus comprising: the device comprises a cuboid flash burning cavity (1), a capacitor assembly (2), a capacitor charging assembly, a capacitor discharging assembly and a direct current power supply. The cuboid flash-burning cavity (1) is a box body formed by five acrylic glass plates, the top surface of the cuboid flash-burning cavity is not sealed, a first round copper electrode (11) and a second round copper electrode (12) are respectively arranged on the acrylic glass plates on the two side edges, and the first round copper electrode (11) and the second round copper electrode (12) are respectively connected with the two ends of the capacitor assembly (2);
the capacitor assembly (2) comprises a plurality of electrolytic capacitors (21) connected in parallel and a diode (22) connected in anti-parallel;
the capacitor charging assembly comprises a direct-current power supply (23), a resistor (24) and a push type switch (25), which are sequentially connected with the capacitor assembly (2);
the capacitor discharging assembly comprises a signal generator (26), a millisecond relay switch (27) and a direct current contactor (28) which are connected in sequence; the direct current contactor (28) is connected to the first round copper electrode (11); the millisecond relay switch (27) is provided with a switch power supply (29).
9. The device for uniformly growing graphene in the carbon slide block according to claim 8, wherein the internal dimension of the rectangular flash chamber (1) is 100 x 35 x 20mm, and the thickness of each acrylic glass plate is 3mm.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104649700A (en) * 2013-11-18 2015-05-27 苏州东南电碳科技有限公司 Carbon contact strip of pantograph and manufacturing method thereof
CN105272254A (en) * 2015-10-10 2016-01-27 大同新成新材料股份有限公司 Preparation method of pantograph carbon contact strip material
CN106699181A (en) * 2015-11-13 2017-05-24 大同新成新材料股份有限公司 Method for preparing pantograph carbon slide strip material from graphene oxide
CN107805070A (en) * 2017-10-30 2018-03-16 大同新成新材料股份有限公司 A kind of graphene carbon slide plate
US20190126758A1 (en) * 2017-10-27 2019-05-02 Army Academy of Armored Forces Repairable sliding plate of pantograph of electric locomotive and method for making the same
JP2019136727A (en) * 2018-02-08 2019-08-22 品川リフラクトリーズ株式会社 Zirconia-containing alumina-carbonaceous slide plate refractory

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104649700A (en) * 2013-11-18 2015-05-27 苏州东南电碳科技有限公司 Carbon contact strip of pantograph and manufacturing method thereof
CN105272254A (en) * 2015-10-10 2016-01-27 大同新成新材料股份有限公司 Preparation method of pantograph carbon contact strip material
CN106699181A (en) * 2015-11-13 2017-05-24 大同新成新材料股份有限公司 Method for preparing pantograph carbon slide strip material from graphene oxide
US20190126758A1 (en) * 2017-10-27 2019-05-02 Army Academy of Armored Forces Repairable sliding plate of pantograph of electric locomotive and method for making the same
CN107805070A (en) * 2017-10-30 2018-03-16 大同新成新材料股份有限公司 A kind of graphene carbon slide plate
JP2019136727A (en) * 2018-02-08 2019-08-22 品川リフラクトリーズ株式会社 Zirconia-containing alumina-carbonaceous slide plate refractory

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