CN102320853B - Preparation method of carbon-based composite cathode material with highly-oriented emission characteristic - Google Patents
Preparation method of carbon-based composite cathode material with highly-oriented emission characteristic Download PDFInfo
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- CN102320853B CN102320853B CN 201110244028 CN201110244028A CN102320853B CN 102320853 B CN102320853 B CN 102320853B CN 201110244028 CN201110244028 CN 201110244028 CN 201110244028 A CN201110244028 A CN 201110244028A CN 102320853 B CN102320853 B CN 102320853B
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Abstract
The invention discloses a preparation method of a carbon-based composite cathode material with a highly-oriented emission characteristic, which comprises the following steps of: 1) weaving a highly-oriented carbon-fiber prefabricated body to enable carbon fibers in the carbon-fiber prefabricated body to be distributed along an axial direction, wherein an included angle is 0-15 degrees; 2) placing the carbon-fiber prefabricated body into a chemical vapor carburizing furnace, implementing chemical vapor carburization by using C3H6 as carbon-source gas and N2 as diluent gas to obtain matrix carbon in the carbon-fiber prefabricated body, controlling the volume ratio of C3H6 to N2 to be 1.5-4:1, the furnace temperature to be 1000-1100 DEG C and the furnace pressure to be 21-30kPa, discharging after accumulating the chemical vapor carburization for 400-500 hours, and carrying out 3-6 times of intermediate graphitization processing in the meantime; and 3) placing into a high-temperature furnace to implement final graphitization processing, controlling the atmosphere in a furnace to be 0.11-0.13Mpa of argon gas, the furnace temperature to be 2400-2700 DEG C and the heat-preserving time to be 1-2 hours, and cooling along with the furnace. In the preparation method, the flowing, cracking and depositing processes of the carbon-source gas in the prefabricated body are controlled by adopting the highly-oriented carbon-fiber prefabricated body to obtain a high-texture pyrolytic-carbon matrix.
Description
Technical field
The present invention relates to a kind of preparation method of C-base composte material, particularly relate to a kind of preparation method with carbon back composite cathode material of high orientation emission characteristic.
Background technology
Graphite is the common used material of electron beam diode cathode in the High-Power Microwave.Because graphite material is frangible, dust is bigger, and easily adsorbed gas, in use often pollute vacuum environment, have a strong impact on the High-Power Microwave working performance of devices.Therefore be badly in need of development novel cathode material.The carbon back composite cathode material is the matrix material by the carbon fiber reinforced carbon matrix body, it had both improved, and graphite material is frangible, dust reaches shortcomings such as easy adsorbed gas more greatly, simultaneously also keep advantages such as graphite is high temperature resistant, electron emission is even, become the developing direction of high orientation emission characteristic cathode material.
The key that acquisition has the carbon back composite cathode material of high orientation emission characteristic is only to keep the directivity of enhancing body carbon fiber spatial arrangement and highly-texturedization of matrix carbon structure.Chemical gas phase carburizing technology is the prefered method of preparation high-performance carbon back composite cathode material, and the matrix RESEARCH OF PYROCARBON of this method preparation has even structure, complete, advantage such as compactness is good.But being matrix RESEARCH OF PYROCARBON structure, shortcoming is difficult to control.The chemical gas phase carburizing is the technological process of a complexity, and in this course, carbon-source gas is under 1000 ℃ of hot conditionss, and cracking goes out carbon, and deposits to carbon fiber surface, forms the matrix RESEARCH OF PYROCARBON.The matrix RESEARCH OF PYROCARBON that generates mainly contains three kinds of typical structure types, is respectively the smooth layer structure RESEARCH OF PYROCARBON of the isotropy RESEARCH OF PYROCARBON of low texture, middle texture, and highly-textured rough laminar microstructure RESEARCH OF PYROCARBON.The structure of matrix RESEARCH OF PYROCARBON is controlled by carbon-source gas flowing in precast body, cracking and deposition process mainly.Therefore, must adopt special process, control carbon-source gas flowing in precast body, cracking and deposition process obtain highly-textured RESEARCH OF PYROCARBON matrix.
Goal of the invention
Technical problem to be solved by this invention provides a kind of preparation method who obtains the carbon back composite cathode material of the high orientation emission characteristic of having of highly-textured RESEARCH OF PYROCARBON matrix at high oriented carbon fiber precast body.
In order to solve the problems of the technologies described above, the preparation method with carbon back composite cathode material of high orientation emission characteristic provided by the invention comprises the steps:
1) the high oriented carbon fiber precast body of braiding makes that the carbon fiber in the prefabricated carbon fiber body distributes vertically, and angle is 0～15 degree;
2) the prefabricated carbon fiber body is placed chemical gas phase carburizing stove, with C
3H
6Be carbon source gas, N
2Be carrier gas, implement the chemical gas phase carburizing and in the prefabricated carbon fiber body, obtain matrix carbon, control C
3H
6: N
2Volume ratio is 1.5～4: 1, furnace temperature is that 1000～1100 ℃, furnace pressure are 21～30kPa, comes out of the stove behind accumulative total chemical gas phase carburizing 400～500h, carry out 3～6 times therebetween in the middle of graphitization processing;
3) the prefabricated carbon fiber body that will obtain matrix carbon places High Temperature Furnaces Heating Apparatus to implement final graphitization processing, the control furnace atmosphere is that argon gas 0.11～0.13Mpa, furnace temperature are that 2400～2700 ℃, soaking time are 1～2h, and furnace cooling namely gets the carbon back composite cathode material with high orientation emission characteristic.
The apparent density of described prefabricated carbon fiber body is 0.81g/cm
3～1.2g/cm
3
Described matrix carbon is highly-textured RESEARCH OF PYROCARBON matrix, and its degree of graphitization is 90%～100%.
Graphitization processing is that the prefabricated carbon fiber body that will obtain matrix carbon places High Temperature Furnaces Heating Apparatus to implement graphitization processing in the middle of described, and furnace atmosphere is that argon gas 0.11～0.13Mpa, furnace temperature are that 2000～2200 ℃, soaking time are 1～2h.
The present invention is owing to adopt above-mentioned processing method, thereby, have following advantage and positively effect:
1, adopts C
3H
6: N
2Volume ratio is 1.5～4: 1 high volume ratio, guarantees the rapid carburization of C-base composte material.
2, adopt the high furnace pressure of 21～30kPa, guarantee the evening chemical Gas Carburizing of C-base composte material, avoid producing the even property of density unevenness.
3, by step 1 and step 2, guarantee highly-texturedization of matrix RESEARCH OF PYROCARBON in the C-base composte material.
4, adopting the present invention, is 0.86g/cm with the apparent density
3The prefabricated carbon fiber body, through the carburizing of 400～500h chemical gas phase, can prepare apparent density is 1.87g/cm
3C-base composte material, the material axial tensile strength is 126Mpa, thermal expansivity is 2.6 * 10
-6/ ℃, thermal conductivity is that 56W/mK, emission are greater than 1kA/cm
2
In sum, preparation method with carbon back composite cathode material of high orientation emission characteristic provided by the invention, by adopting high oriented carbon fiber precast body, control carbon-source gas flowing in precast body, cracking and deposition process, obtain highly-textured RESEARCH OF PYROCARBON matrix, provide a kind of practicable method for having the high preparation that is orientated the carbon back composite cathode material of emission characteristic.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment 1:
Referring to Fig. 1, weave high oriented carbon fiber precast body, the apparent density of prefabricated carbon fiber body is 0.81g/cm
3, making that the carbon fiber in the prefabricated carbon fiber body distributes vertically, angle is 0 degree; The prefabricated carbon fiber body is placed chemical gas phase carburizing stove, with C
3H
6Be carbon source gas, N
2Be carrier gas, the carburizing of enforcement chemical gas phase obtains matrix carbon in the prefabricated carbon fiber body be highly-textured RESEARCH OF PYROCARBON matrix, control C
3H
6: N
2Volume ratio is that 1.5: 1, furnace temperature are that 1000 ℃, furnace pressure are 30kPa, come out of the stove behind the accumulative total chemical gas phase carburizing 500h, graphitization processing in the middle of carrying out 5 times therebetween, middle graphitization processing is to place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, and furnace atmosphere is that argon gas 0.11Mpa, furnace temperature are that 2200 ℃, soaking time are 2h; Place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, the control furnace atmosphere is that argon gas 0.11Mpa, furnace temperature are 2400, soaking time is 2h, the degree of graphitization of highly-textured RESEARCH OF PYROCARBON matrix is 90%, and furnace cooling namely gets the carbon back composite cathode material with high orientation emission characteristic of the present invention.
Embodiment 2:
Referring to Fig. 1, weave high oriented carbon fiber precast body, the apparent density of prefabricated carbon fiber body is 0.9g/cm
3, making that the carbon fiber in the prefabricated carbon fiber body distributes vertically, angle is 4 degree; The prefabricated carbon fiber body is placed chemical gas phase carburizing stove, with C
3H
6Be carbon source gas, N
2Be carrier gas, the carburizing of enforcement chemical gas phase obtains matrix carbon in the prefabricated carbon fiber body be highly-textured RESEARCH OF PYROCARBON matrix, control C
3H
6: N
2Volume ratio is that 2: 1, furnace temperature are that 1100 ℃, furnace pressure are 28kPa, come out of the stove behind the accumulative total chemical gas phase carburizing 500h, graphitization processing in the middle of carrying out 5 times therebetween, middle graphitization processing is to place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, and furnace atmosphere is that argon gas 0.13Mpa, furnace temperature are that 2000 ℃, soaking time are 1.5h; Place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, the control furnace atmosphere is that argon gas 0.11Mpa, furnace temperature are that 2400 ℃, soaking time are 2h, the degree of graphitization of highly-textured RESEARCH OF PYROCARBON matrix is 92%, and furnace cooling namely gets the carbon back composite cathode material with high orientation emission characteristic of the present invention.
Embodiment 3:
Referring to Fig. 1, weave high oriented carbon fiber precast body, the apparent density of prefabricated carbon fiber body is 1.0g/cm
3, making that the carbon fiber in the prefabricated carbon fiber body distributes vertically, angle is 8 degree; The prefabricated carbon fiber body is placed chemical gas phase carburizing stove, with C
3H
6Be carbon source gas, N
2Be carrier gas, the carburizing of enforcement chemical gas phase obtains matrix carbon in the prefabricated carbon fiber body be highly-textured RESEARCH OF PYROCARBON matrix, control C
3H
6: N
2Volume ratio is that 2.5: 1, furnace temperature are that 1100 ℃, furnace pressure are 26kPa, come out of the stove behind the accumulative total chemical gas phase carburizing 400h, graphitization processing in the middle of carrying out 5 times therebetween, middle graphitization processing is to place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, and furnace atmosphere is that argon gas 0.12Mpa, furnace temperature are that 2100 ℃, soaking time are 1h; Place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, the control furnace atmosphere is that argon gas 0.12Mpa, furnace temperature are that 2500 ℃, soaking time are 2h, the degree of graphitization of highly-textured RESEARCH OF PYROCARBON matrix is 94%, and furnace cooling namely gets the carbon back composite cathode material with high orientation emission characteristic of the present invention.
Embodiment 4:
Referring to Fig. 1, weave high oriented carbon fiber precast body, the apparent density of prefabricated carbon fiber body is 1.1g/cm
3, making that the carbon fiber in the prefabricated carbon fiber body distributes vertically, angle is 10 degree; The prefabricated carbon fiber body is placed chemical gas phase carburizing stove, with C
3H
6Be carbon source gas, N
2Be carrier gas, the carburizing of enforcement chemical gas phase obtains matrix carbon in the prefabricated carbon fiber body be highly-textured RESEARCH OF PYROCARBON matrix, control C
3H
6: N
2Volume ratio is that 3: 1, furnace temperature are that 1100 ℃, furnace pressure are 24kPa, come out of the stove behind the accumulative total chemical gas phase carburizing 450h, graphitization processing in the middle of carrying out 4 times therebetween, middle graphitization processing is to place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, and furnace atmosphere is that argon gas 0.11Mpa, furnace temperature are that 2200 ℃, soaking time are 1.2h; Place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, the control furnace atmosphere is that argon gas 0.12Mpa, furnace temperature are that 2500 ℃, soaking time are 1.5h, the degree of graphitization of highly-textured RESEARCH OF PYROCARBON matrix is 94%, and furnace cooling namely gets the carbon back composite cathode material with high orientation emission characteristic of the present invention.
Embodiment 5:
Referring to Fig. 1, weave high oriented carbon fiber precast body, the apparent density of prefabricated carbon fiber body is 0.88g/cm
3, making that the carbon fiber in the prefabricated carbon fiber body distributes vertically, angle is 15 degree; The prefabricated carbon fiber body is placed chemical gas phase carburizing stove, with C
3H
6Be carbon source gas, N
2Be carrier gas, the carburizing of enforcement chemical gas phase obtains matrix carbon in the prefabricated carbon fiber body be highly-textured RESEARCH OF PYROCARBON matrix, control C
3H
6: N
2Volume ratio is that 3.5: 1, furnace temperature are that 1000 ℃, furnace pressure are 22kPa, come out of the stove behind the accumulative total chemical gas phase carburizing 450h, graphitization processing in the middle of carrying out 4 times therebetween, middle graphitization processing is to place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, and furnace atmosphere is that argon gas 0.13Mpa, furnace temperature are that 2000 ℃, soaking time are 1.6h; Place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, the control furnace atmosphere is that argon gas 0.12Mpa, furnace temperature are that 2600 ℃, soaking time are 1.5h, the degree of graphitization of highly-textured RESEARCH OF PYROCARBON matrix is 95%, and furnace cooling namely gets the carbon back composite cathode material with high orientation emission characteristic of the present invention.
Embodiment 6:
Referring to Fig. 1, weave high oriented carbon fiber precast body, the apparent density of prefabricated carbon fiber body is 0.95g/cm
3, making that the carbon fiber in the prefabricated carbon fiber body distributes vertically, angle is 7 degree; The prefabricated carbon fiber body is placed chemical gas phase carburizing stove, with C
3H
6Be carbon source gas, N
2Be carrier gas, the carburizing of enforcement chemical gas phase obtains matrix carbon in the prefabricated carbon fiber body be highly-textured RESEARCH OF PYROCARBON matrix, control C
3H
6: N
2Volume ratio is that 4: 1, furnace temperature are that 1050 ℃, furnace pressure are 21kPa, come out of the stove behind the accumulative total chemical gas phase carburizing 400h, graphitization processing in the middle of carrying out 3 times therebetween, middle graphitization processing is to place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, and furnace atmosphere is that argon gas 0.13Mpa, furnace temperature are that 2100 ℃, soaking time are 2h; Place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, the control furnace atmosphere is that argon gas 0.13Mpa, furnace temperature are that 2600 ℃, soaking time are 1h, the degree of graphitization of highly-textured RESEARCH OF PYROCARBON matrix is 98%, and furnace cooling namely gets the carbon back composite cathode material with high orientation emission characteristic of the present invention.
Embodiment 7:
Referring to Fig. 1, weave high oriented carbon fiber precast body, the apparent density of prefabricated carbon fiber body is 1.1g/cm
3, making that the carbon fiber in the prefabricated carbon fiber body distributes vertically, angle is 5 degree; The prefabricated carbon fiber body is placed chemical gas phase carburizing stove, with C
3H
6Be carbon source gas, N
2Be carrier gas, the carburizing of enforcement chemical gas phase obtains matrix carbon in the prefabricated carbon fiber body be highly-textured RESEARCH OF PYROCARBON matrix, control C
3H
6: N
2Volume ratio is that 3: 1, furnace temperature are that 1000 ℃, furnace pressure are 21kPa, come out of the stove behind the accumulative total chemical gas phase carburizing 400h, graphitization processing in the middle of carrying out 3 times therebetween, middle graphitization processing is to place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, and furnace atmosphere is that argon gas 0.12Mpa, furnace temperature are that 2000 ℃, soaking time are 1h; Place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, the control furnace atmosphere is that argon gas 0.13Mpa, furnace temperature are that 2700 ℃, soaking time are 1h, the degree of graphitization of highly-textured RESEARCH OF PYROCARBON matrix is 100%, and furnace cooling namely gets the carbon back composite cathode material with high orientation emission characteristic of the present invention.
Embodiment 8:
Referring to Fig. 1, weave high oriented carbon fiber precast body, the apparent density of prefabricated carbon fiber body is 1.2g/cm
3, making that the carbon fiber in the prefabricated carbon fiber body distributes vertically, angle is 2 degree; The prefabricated carbon fiber body is placed chemical gas phase carburizing stove, with C
3H
6Be carbon source gas, N
2Be carrier gas, the carburizing of enforcement chemical gas phase obtains matrix carbon in the prefabricated carbon fiber body be highly-textured RESEARCH OF PYROCARBON matrix, control C
3H
6: N
2Volume ratio is that 3: 1, furnace temperature are that 1100 ℃, furnace pressure are 21kPa, come out of the stove behind the accumulative total chemical gas phase carburizing 500h, graphitization processing in the middle of carrying out 6 times therebetween, middle graphitization processing is to place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, and furnace atmosphere is that argon gas 0.11Mpa, furnace temperature are that 2200 ℃, soaking time are 1.5h; Place High Temperature Furnaces Heating Apparatus to implement graphitization processing prefabricated carbon fiber body and highly-textured RESEARCH OF PYROCARBON matrix, the control furnace atmosphere is that argon gas 0.12Mpa, furnace temperature are that 2700 ℃, soaking time are 2h, the degree of graphitization of highly-textured RESEARCH OF PYROCARBON matrix is 100%, and furnace cooling namely gets the carbon back composite cathode material with high orientation emission characteristic of the present invention.
Claims (3)
1. the preparation method with carbon back composite cathode material of high orientation emission characteristic is characterized in that: comprise the steps:
(1), the braiding high oriented carbon fiber precast body, make that the carbon fiber in the prefabricated carbon fiber body distributes vertically, angle be 0～15 the degree;
(2), the prefabricated carbon fiber body is placed chemical gas phase carburizing stove, with C
3H
6Be carbon source gas, N
2Be carrier gas, implement the chemical gas phase carburizing and in the prefabricated carbon fiber body, obtain matrix carbon, control C
3H
6: N
2Volume ratio is that 1.5～4:1, furnace temperature are that 1000～1100 ℃, furnace pressure are 21～30kPa, comes out of the stove behind accumulative total chemical gas phase carburizing 400～500h, carry out 3～6 times therebetween in the middle of graphitization processing;
(3), the prefabricated carbon fiber body that will obtain matrix carbon places High Temperature Furnaces Heating Apparatus to implement final graphitization processing, furnace atmosphere is that argon gas 0.11～0.13Mpa, furnace temperature are that 2400～2700 ℃, soaking time are 1～2h, and furnace cooling namely gets the carbon back composite cathode material with high orientation emission characteristic.
2. the preparation method with carbon back composite cathode material of high orientation emission characteristic according to claim 1, it is characterized in that: the apparent density of described prefabricated carbon fiber body is 0.81g/cm
3～1.2g/cm
3
3. the preparation method with carbon back composite cathode material of high orientation emission characteristic according to claim 1, it is characterized in that: described matrix carbon is highly-textured RESEARCH OF PYROCARBON matrix, and its degree of graphitization is 90%～100%.
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| CN102515810A (en) * | 2011-11-22 | 2012-06-27 | 中南大学 | Preparation method of carbon-based composite cathode material with high-orientation emission characteristic |
| CN104498893B (en) * | 2014-12-19 | 2017-01-11 | 中南大学 | Rapid preparation method of highly textured pyrolytic carbon film |
| CN106518091B (en) * | 2016-10-27 | 2019-04-19 | 西北工业大学 | A method of improving two-dimentional carbon/carbon compound material mechanical property |
| CN108878233B (en) * | 2018-06-19 | 2019-06-07 | 大连理工大学 | A kind of preparation method of the carbon-fiber cathode for electron beam transmitting |
| CN108899260B (en) * | 2018-06-19 | 2020-01-17 | 大连理工大学 | Preparation method of mixed disordered carbon fiber cathode for emitting electron beams |
| CN111302821A (en) * | 2020-02-27 | 2020-06-19 | 深圳市晖耀电线电缆有限公司 | Preparation method of C/C composite material |
| CN111646814A (en) * | 2020-06-23 | 2020-09-11 | 湖州师范学院 | Manufacturing method of C/C grid of ion thruster |
| CN112174686A (en) * | 2020-09-28 | 2021-01-05 | 西北工业大学 | Preparation method of one-millimeter-thick sheet-shaped carbon/carbon composite material |
| CN112608163B (en) * | 2020-12-17 | 2022-02-18 | 中南大学 | Barium titanate doped modified carbon-based composite material and preparation method thereof |
| CN115652282B (en) * | 2022-11-16 | 2024-04-05 | 湖南碳材科技有限公司 | Composite CVD graphite material and preparation method and application thereof |
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