CN109553432B - High-density flexible carbon/carbon composite friction material and preparation method thereof - Google Patents

High-density flexible carbon/carbon composite friction material and preparation method thereof Download PDF

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CN109553432B
CN109553432B CN201811579315.0A CN201811579315A CN109553432B CN 109553432 B CN109553432 B CN 109553432B CN 201811579315 A CN201811579315 A CN 201811579315A CN 109553432 B CN109553432 B CN 109553432B
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carbon
friction material
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woven
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CN109553432A (en
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单云刚
龚承涛
陆千夏
赵志清
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Kunshan Shengxia Composite Materials Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83Carbon fibres in a carbon matrix
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins

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  • Ceramic Engineering (AREA)
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Abstract

The invention discloses a high-density flexible carbon/carbon composite friction material and a preparation method thereof, wherein polyacrylonitrile fibers, viscose-based fibers, pitch-based fibers and the like are subjected to pre-oxidation treatment in sequence, and then pre-oxidized silk yarns are woven into fabrics; then carbonizing the woven fabric to obtain a carbon fiber fabric; finally, the carbon fiber fabric is put into a gaseous state CxHyIn N2Under the protection of the carbon nano-tube, the prepared high-density flexible carbon/carbon composite friction material is obtained after chemical vapor deposition treatment. Finally obtaining the carbon fiber fabric reinforced carbon-based composite material with warp and weft yarn bending degree larger than 30 degrees. The carbon/carbon friction material with good flexibility can be obtained by utilizing the low modulus of the pre-oxidized silk and easily weaving the product with high warp and weft yarn flexibility, and simultaneously having excellent flexibility.

Description

High-density flexible carbon/carbon composite friction material and preparation method thereof
Technical Field
The invention belongs to the technical field of friction materials, and particularly relates to a high-density flexible carbon/carbon composite friction material and a preparation method thereof.
Background
The synchronizer is an important component of the gearbox, and can effectively ensure smooth gear shifting, simplify operation and reduce the labor intensity of a driver. With the development of trucks in the direction of large tonnage and large torque, higher and higher requirements are put forward on synchronizers, and the traditional friction material for the synchronizer ring has the advantages of low strength, poor wear resistance, unstable friction coefficient and short service life, and cannot meet the use requirements. The carbon fiber reinforced carbon-based composite material has the characteristics of stable friction coefficient, high temperature resistance, corrosion resistance, impact resistance, wear resistance and the like, is widely applied to the fields of aircraft brake pads, high-performance sports car brake pads and the like, and is an ideal friction material at present. However, the carbon-carbon composite material is rigid and not easy to bend at present, and cannot be applied to the automobile synchronizer gear ring, and meanwhile, the carbon fiber has high modulus and relatively poor weaving performance, so that the carbon fiber is difficult to weave into a product with high warp and weft flexibility, and the fabric and the product thereof have poor flexibility. Therefore, the invention provides a method for preparing a high-density flexible carbon/carbon composite friction material and the material prepared by the method.
Disclosure of Invention
Aiming at the problems, the invention provides a high-density flexible carbon/carbon composite friction material and a preparation method thereof.
The technical purpose is achieved, the technical effect is achieved, and the invention is realized through the following technical scheme:
a method of making a high density flexible carbon/carbon composite friction material comprising the steps of:
the method comprises the following steps: performing pre-oxidation treatment on polyacrylonitrile fibers, viscose-based fibers, asphalt-based fibers and the like, and then weaving pre-oxidized silk yarns into fabrics;
step two: carbonizing the woven fabric to obtain a carbon fiber fabric;
step three: putting the carbon fiber fabric into a gaseous state CxHyIn N2Under the protection of the carbon nano-tube, the prepared high-density flexible carbon/carbon composite friction material is obtained after chemical vapor deposition treatment.
As a further improvement of the invention, the pre-oxidation treatment in the first step comprises the step of enabling the polyacrylonitrile fiber to pass through a guide roller of a pre-oxidation furnace and sequentially pass through four temperature zones arranged in the pre-oxidation furnace, wherein the pre-oxidation time is 30-120 min, and the pre-oxidation silk with the carbon content of more than 60% is obtained.
As a further improvement of the invention, the set temperatures of the four temperature zones in the pre-oxidation furnace are gradually increased from the wire inlet end to the wire outlet end, wherein the temperatures of the four temperature zones are 180-210 ℃ in the first zone, 210-250 ℃ in the second zone, 240-280 ℃ in the third zone and 270-300 ℃ in the fourth zone.
As a further improvement of the invention, the pre-oxidized yarn in the first step comprises continuous pre-oxidized fibers, and the obtained pre-oxidized continuous fibers are subjected to a spinning process to prepare the pre-oxidized yarn with 2-20 yarns and 0.5-30 twists/cm.
As a further improvement of the invention, the pre-oxidized silk yarn in the step one is woven in a single-warp single-weft or multi-warp multi-weft mode, and the warp and weft density of the woven fabric structure is 5-20 × 5-20 pieces/cm.
As a further improvement of the invention, the carbonization treatment in the second step comprises the step of putting the woven fabric structure into a carbonization furnace, and carbonizing for 30-60 min at the temperature of 500-1600 ℃ under the protection of nitrogen to obtain the carbon fiber fabric with the carbon content of more than 95%.
As a further improvement of the invention, the chemical vapor deposition in the third step is that the carbon fiber fabric is put into a vacuum deposition furnace, and the carbon fiber fabric is put into the vacuum deposition furnacexHyAn organic hydrocarbon selected from gases wherein x is less than 4, said CxHyPyrolysis is carried out at the temperature of 900-1000 ℃, and carbon generated by pyrolysis is deposited on the surface area of the fiber to form the carbon fiber reinforced carbon-based composite material.
As a further improvement of the invention, in the chemical vapor deposition process, the furnace pressure in the vacuum deposition furnace is 20-800 torr, and the gas flow CxHy: N2 is 1: 30-40, and the deposition time is 2-5 hours.
The invention also includes a high-density flexible carbon/carbon composite friction material prepared according to the preparation method.
The invention has the beneficial effects that: the carbon/carbon friction material with good flexibility can be obtained by utilizing the low modulus of the pre-oxidized silk and easily weaving the product with high warp and weft yarn flexibility, and simultaneously having excellent flexibility.
Drawings
FIG. 1 is a cross-sectional view of a high density flexible carbon/carbon composite friction material;
FIG. 2 is a flow chart of the preparation of a high density flexible carbon/carbon composite friction material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The following detailed description of the principles of the invention is provided in connection with the accompanying drawings.
The structure of the high-density flexible carbon/carbon composite friction material manufactured by the invention as shown in figure 1 comprises a double-warp double-weft planar fabric woven by intersecting warp yarns and weft yarns, fibers are combined together by a chemical vapor deposition carbon matrix, and the bending radius of the carbon/carbon composite friction material is less than 2 cm. The carbon fiber yarns of the warp yarns or the weft yarns are carbon fiber yarns which are obtained by pre-oxidizing and carbonizing protofilaments such as polyacrylonitrile fibers and viscose-based fibers and have carbon content of more than 95%, so that the high friction coefficient and the high bending degree can be maintained. The bending angle of the fiber filaments of the warp yarns or the weft yarns is more than 30 degrees. In one embodiment of the present invention, the density of the warp yarns or the weft yarns in the flat woven fabric is greater than or equal to 5 yarns/cm, and the thickness of the woven flat woven fabric is greater than 0.4 mm.
Since the flat fabric in fig. 1 is based on a carbon fiber reinforced carbon-based composite material, the carbon fiber has a high modulus and poor weaving performance when the carbon content is high. Therefore, in order to obtain the high-density flexible carbon/carbon fiber friction material shown in fig. 1, the present invention prepares a friction material through a preparation process as shown in fig. 2. The following two specific examples are given for illustration.
The first embodiment is as follows:
the preparation process of the high-density flexible carbon/carbon composite friction material shown in figure 1 comprises the following steps:
the first step is as follows: and preparing the pre-oxidized silk.
Selecting 1K polyacrylonitrile fiber, putting the polyacrylonitrile fiber into a pre-oxidation furnace, and sequentially passing through four temperature areas of the pre-oxidation furnace under the driving of the rotation of a guide roller in the pre-oxidation furnace. The set temperature is sequentially 180-210 ℃ in the first area, 220-250 ℃ in the second area, 270-280 ℃ in the third area, 290-300 ℃ in the fourth area and 60min in the fourth area, and finally the pre-oxidized fiber with the carbon content of more than 65% is obtained. The obtained pre-oxidized silk still has higher flexibility and is easy to weave.
The second step is that: and (3) preparing twisted pre-oxidized silk, namely twisting the pre-oxidized silk to 0.5-2 twists/cm through twisting equipment.
The third step: woven fabric structure
The pre-oxidized silk cloth is woven according to a double-warp and double-weft mode, the warp and weft density is 8.5 (+ -0.5) by 8.5 (+ -0.5) pieces/cm, and a flexible woven cloth structure is woven.
Because the carbon content of the prepared woven fabric is low, the strength is low, and the friction resistance is poor, the carbon content needs to be further improved by the following two steps of treatment.
The fourth step: preparation of carbon cloth
And under the protection of nitrogen, putting the woven fabric into a carbonization furnace at 500-1600 ℃ for carbonization for 30-60 min to obtain the carbon fiber cloth with the carbon content of more than 95%.
The fifth step: preparation of flexible carbon/carbon friction material
The carbon fiber cloth is put under the temperature of 950 ℃ and the furnace pressure of 220 and 260 torr, C3H8:N2Under the condition of the flow ratio of 1:35, carrying out chemical vapor deposition for 2-4 hours to obtain the high-density carbon/carbon friction-resistant material with the carbon content of more than 98%, wherein the prepared carbon/carbon friction-resistant material still has higher flexibility.
Example two:
the first step is as follows: and preparing the pre-oxidized silk.
Selecting 3K viscose-based fibers, putting the viscose-based fibers into a pre-oxidation furnace, and sequentially passing through four temperature areas of the pre-oxidation furnace under the driving of the rotation of a guide roller in the pre-oxidation furnace. The set temperature is sequentially 180-200 ℃ in the first area, 210-230 ℃ in the second area, 240-260 ℃ in the third area, 270-300 ℃ in the fourth area and 90min of pre-oxidation, and the pre-oxidized silk with the carbon content of more than 65% is obtained.
The second step is that: preparing twisted pre-oxidized silk, and twisting the pre-oxidized silk to 0.2-1 twist/cm through twisting equipment.
The third step: woven fabric structure
And (3) weaving the pre-oxidized silk cloth according to the warp and weft density of 7 (+ -0.5) by 7 (+ -0.5) roots/cm to weave a flexible woven cloth structure.
The fourth step: preparation of carbon cloth
And under the protection of nitrogen, putting the woven fabric into a carbonization furnace at 500-1600 ℃ for carbonization for 30-60 min to obtain the carbon fiber cloth with the carbon content of more than 95%.
The fifth step: preparation of flexible carbon/carbon friction material
Subjecting carbon fiber cloth to a furnace pressure of 280-300 torr at 900 ℃, wherein CH is4:N2And carrying out chemical vapor deposition for 3-5 hours under the condition that the flow ratio is 1:30 to obtain the high-density flexible carbon/carbon composite friction material with the carbon content of more than 98%.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (1)

1. A preparation method of a high-density flexible carbon/carbon composite friction material is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
the first step is as follows: preparation of Pre-oxidized yarn
Selecting 3K viscose-based fibers, putting the viscose-based fibers into a pre-oxidation furnace, and sequentially passing through four temperature areas of the pre-oxidation furnace under the driving of the rotation of a guide roller in the pre-oxidation furnace; the set temperature is as follows in sequence: pre-oxidizing for 90min at the first zone temperature of 180-200 ℃, the second zone temperature of 210-230 ℃, the third zone temperature of 240-260 ℃ and the fourth zone temperature of 270-300 ℃ to obtain pre-oxidized fibers with carbon content of more than 65%;
the second step is that: preparing twisted pre-oxidized silk, and twisting the pre-oxidized silk to 0.2-1 twist/cm through twisting equipment;
the third step: woven fabric structure
Weaving the pre-oxidized silk cloth according to the warp and weft density (7 +/-0.5) × (7 +/-0.5) roots/cm to be woven into a flexible woven cloth structure; the fourth step: preparation of carbon cloth
Under the protection of nitrogen, putting the woven fabric into a carbonization furnace at 500-1600 ℃ for carbonization for 30-60 min to obtain carbon fiber cloth with the carbon content of more than 95%;
the fifth step: preparation of flexible carbon/carbon friction material
Subjecting carbon fiber cloth to a furnace pressure of 280-300 torr at 900 ℃, wherein CH is4: N2And carrying out chemical vapor deposition for 3-5 hours under the condition that the flow ratio is 1:30 to obtain the high-density flexible carbon/carbon composite friction material with the carbon content of more than 98%.
CN201811579315.0A 2018-12-24 2018-12-24 High-density flexible carbon/carbon composite friction material and preparation method thereof Active CN109553432B (en)

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CN110128160B (en) * 2019-04-22 2021-05-11 湖南东映碳材料科技有限公司 Method for preparing high-thermal-conductivity carbon-carbon composite material from two-dimensional network of pitch fiber precursors
CN110616493B (en) * 2019-09-23 2021-09-10 潘魏豪 Manufacturing method of flexible conductive carbon cloth
CN110655908A (en) * 2019-10-11 2020-01-07 山东万邦新材料科技有限公司 Preparation method of carbon fiber friction material
CN114857192A (en) * 2022-06-06 2022-08-05 杜建华 Carbon fiber reinforced carbon-based friction plate structure and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1320531A (en) * 2000-04-27 2001-11-07 李荣立 Method for making braking disk with composite carbon/carbon material
CN101787504A (en) * 2010-01-21 2010-07-28 上海大学 Preparation method for carbon/carbon-copper composite material
CN101805200A (en) * 2010-03-17 2010-08-18 上海大学 Method for producing carbon/carbone composite material for bearings
CN104177111A (en) * 2014-08-18 2014-12-03 中国科学院上海应用物理研究所 Method for preparing carbon/carbon composite material profile by slurry casting
EP3109221A2 (en) * 2015-06-26 2016-12-28 Goodrich Corporation Systems and methods for producing a carbon composite material
CN108314458A (en) * 2018-02-09 2018-07-24 西安天运新材料科技有限公司 A kind of preparation method of high heat conduction carbon/carbon compound material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1320531A (en) * 2000-04-27 2001-11-07 李荣立 Method for making braking disk with composite carbon/carbon material
CN101787504A (en) * 2010-01-21 2010-07-28 上海大学 Preparation method for carbon/carbon-copper composite material
CN101805200A (en) * 2010-03-17 2010-08-18 上海大学 Method for producing carbon/carbone composite material for bearings
CN104177111A (en) * 2014-08-18 2014-12-03 中国科学院上海应用物理研究所 Method for preparing carbon/carbon composite material profile by slurry casting
EP3109221A2 (en) * 2015-06-26 2016-12-28 Goodrich Corporation Systems and methods for producing a carbon composite material
CN108314458A (en) * 2018-02-09 2018-07-24 西安天运新材料科技有限公司 A kind of preparation method of high heat conduction carbon/carbon compound material

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