CN1156132A - Carbon/ceramic composite material and its preparing method - Google Patents
Carbon/ceramic composite material and its preparing method Download PDFInfo
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- CN1156132A CN1156132A CN 96101061 CN96101061A CN1156132A CN 1156132 A CN1156132 A CN 1156132A CN 96101061 CN96101061 CN 96101061 CN 96101061 A CN96101061 A CN 96101061A CN 1156132 A CN1156132 A CN 1156132A
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Abstract
A carbon/pottery composition with better self-lubricating performance, antioxidation and compactness and low cost is prepared by diffusion-hot press-sinter method of ceramic particles, where laminated BN is used as diffusant.
Description
The invention belongs to a kind of preparation method of matrix material, specifically belong to carbon/ceramic composite material and preparation method thereof.
Graphite material has the excellent lubrication feature, be widely used in the fluid machinery field of sealing technology, but the self-lubricating property of graphite is big to vapour, liquid medium dependency, when temperature raises or be in vacuum dry grinding state, it is big that frictional coefficient becomes, and wearing and tearing increase, and particularly use temperature is above 400 ℃, in oxidative environment, easily produce oxidational losses, its application is restricted.Therefore, human dipping MoS is arranged
2Contour gentle lubrication prescription improves the high-temperature self-lubrication of graphite material, but high-temperature oxidation resistance is still undesirable; Human impregnation of phosphoric acid salt or organic silicide are arranged, perhaps make the good carbon/ceramic composite material of high-temperature oxidation resistance, but high-temperature self-lubrication is poor, situation such as easily take place that cracking or surface film are peeled off in the use with CVD method lining SIC, BN etc.
The purpose of this invention is to provide a kind of have when in the high temperature oxidation stability environment, using good self lubricity, carbon/ceramic composite material of oxidation-resistance and compactness and preparation method thereof.
The object of the present invention is achieved like this, it adopts ceramic particle disperse hot pressing sintering method, make the good integrity of matrix material, can overcome surface film peels off and the rimose shortcoming, select for use with the similar aspect shape of crystal structure of graphite BN and make disperse means, aspect shape BN itself has the good high-temperature self lubricity, when high temperature oxidation, can generate liquid B at composite material surface
2O
3, the glassy B of generation
2O
3Both can make the high temperature lubricating film, be again protective oxide layer, and the laggard oxidation step that runs off can generate new protective membrane again, has self-healing.
Preparation method of the present invention is as follows:
A. prepare matrix
(1). form mixing and ball milling 6-16 hour by above-mentioned material, thickener is packed into through 60 mesh sieves in the graphite mo(u)ld,
(2). put into give on the thermocompressor molded after, when beginning to be warming up to sintering temperature 1800-2400 ℃, in 0.5-2.0 hour, slowly be forced into sintering pressure 15-40MPa, constant temperature, pressurize 5-20 minute,
(3). naturally cool to the demoulding after the room temperature.
B. flood, curing, carbonization
(1). is the matrix that makes 50-80 ℃ at dipping temperature, and impregnation pressure is under the 1.5-3.0MPa condition, is immersed in the novolac resin, and the pressurize dipping time is 2-4 hour.
(2). after the matrix behind the dipping is forced into solidifying pressure and is 0.5MPa, beginning heats up with 1-20 ℃/hour curing heat-up rate, when temperature reaches 100 ℃, in continuing temperature-rise period, the slow step-down of solidifying pressure, when solidification value was warmed up to 150 ℃, solidifying pressure was reduced to normal pressure, and constant temperature 2-4 hour
(3). the carbonization heat-up rate with 5-20 ℃/hour under normal pressure is warming up to 800 ℃, and carbonization 2-4 hour,
(4). obtain product behind the naturally cooling.
The aforesaid ball milling time is preferably 10-13 hour,
Aforesaid calcined coke content is preferably 60-65%,
The softening temperature of aforesaid hard pitch is 150-200 ℃, is preferably 170-180 ℃, and content is preferably 20-25%,
Aforesaid aspect shape BN content is preferably 10-15%,
Aforesaid sintering temperature is preferably 2000-2200 ℃,
Aforesaid sintering pressure is preferably 20-30MPa,
Aforesaid dipping temperature is preferably 60-70 ℃,
Aforesaid impregnation pressure is preferably 2.0-2.5MPa,
Aforesaid curing heat-up rate is preferably 2-5 ℃/hour,
Aforesaid calcined coke is to forge oil to burn, calcining pitch coke or metallurgical coke,
Aforesaid graphite is synthetic graphite or lepidiod natural graphite,
As above the hard pitch that is stopped is that coal tar is gone through green grass or young crops or petroleum pitch.
It is as follows that the product of the present invention and preparation thereof has advantage:
1. low 3. 4. self-lubricitys easy to make of simple 2. costs of technology are good
5. good in oxidation resistance 6. compactness 7. intensity height
Embodiments of the invention are as follows:
Embodiment 1
Calcined petroleum coke with 60% (weight percent), the softening temperature of 20% (weight percent) is 175 ℃ a coal-tar pitch, the aspect shape BN mixing and ball milling of the graphous graphite powder of 5% (weight percent) and 15% (weight percent) 6 hours, thickener is crossed in the graphite mo(u)ld of packing into behind 60 mesh sieves, give on the thermocompressor molded after, beginning is warming up to 2200 ℃ of sintering temperatures with 300 ℃/speed at one hour rating, in 1.5 hours, be forced into 25MPa under the homothermic condition afterwards, constant temperature, pressurize 15 minutes naturally cool to the room temperature demoulding then.Is the matrix that makes 70 ℃ at dipping temperature, impregnation pressure is under the 2.0MPa condition, be immersed in two urea formaldehydes of thermoplasticity, the pressurize dipping time is 2 hours, taking out the back is 0.5MPa at solidifying pressure, is 5 ℃ of/hour intensifications to solidify heat-up rate, when temperature rises to 100 ℃, solidifying pressure slowly reduces pressure in temperature-rise period, when solidification value rose to 150 ℃, solidifying pressure was kept to normal pressure, and constant temperature 2 hours, sample after the curing is under normal pressure, with the charing heat-up rate is 10 ℃/hour, is warming up to 800 ℃, and carbonization is naturally cooling after 4 hours, obtain product, the performance of product sees Table.
Embodiment 2
Graphous graphite powder is become natural flake graphite, and it is 183 ℃ petroleum pitch that coal-tar pitch becomes softening temperature, and other is with embodiment 1, and the performance of products obtained therefrom sees Table.
Embodiment 3
Sintering temperature is become 2000 ℃, and other is with embodiment 1, and the performance of products obtained therefrom sees Table.
Embodiment 4
The content of calcined petroleum coke is become 65% (weight percent), and the content of aspect shape BN becomes 10% (weight percent), and other is with embodiment 1, and the performance of products obtained therefrom sees Table.
Embodiment 5
To become 65% (weight percent) containing of calcined petroleum coke most, petroleum pitch content becomes 25% (weight percent), and other is with embodiment 2, and the performance of products obtained therefrom sees Table.
Embodiment 6
With impregnation pressure is 30MPa, and other condition is with embodiment 4, and the products obtained therefrom performance sees Table.
Product traditional performance detected result table
Annotate: a: normal temperature, stainless steel is to flour milling
| Embodiment | ??1 | ??2 | ??3 | ??4 | ??5 | ??6 |
| Bulk density (g/cm 3) | ??1.96 | ??1.95 | ??1.92 | ??1.91 | ??1.94 | ??1.95 |
| Percentage of open area (V%) | ??1.0 | ??1.2 | ??1.4 | ??1.8 | ??1.3 | ??1.0 |
| Hardness (Hs) | ??51 | ??49 | ??68 | ??56 | ??58 | ??60 |
| Static friction coefficient (a) | ??0.15 | ??0.14 | ??0.18 | ??0.16 | ??0.15 | ??0.15 |
| Kinetic friction coefficient (b) | ??0.03 | ??0.01 | ||||
| Oxidizing temperature (℃) (c) | ??670 | ??670 | ??650 | ??650 | ??670 | ??670 |
| Weightless (mg/cm 2.Se)(d) | ??0.325 | ??0.32 | ??0.33 | ??0.42 | ??0.327 | ??0.32 |
| Flexural strength (MPa) | ??92.5 | ??90.4 | ??86.5 | ??82.7 | ??89.6 | ??96.8 |
| Hydraulic pressure is saturating (MPa) not | ??22 | ??22 | ??20 | ??19 | ??21 | ??24 |
| N 2Press not saturating (MPa) | ??0.60 | ??0.60 | ??0.58 | ??0.54 | ??0.59 | ??0.62 |
B: rotating ring is a stainless steel, measures 20-599 ℃ of temperature
C: the beginning weightless temperature,
D:800 ℃, airflow 2L/min oxidation 2 hourly average weight losses.
Claims (16)
1. carbon/ceramic composite material, it is characterized in that: material consists of (weight percentage)
Calcined coke 50-70%
Hard pitch 15-30%
Graphite 2-5%
Aspect shape BN 5-20%
2. a kind of carbon/ceramic composite material according to claim 1 is characterized in that described calcined coke content is preferably 60-65% (weight percent).
3. a kind of carbon/ceramic composite material according to claim 1 is characterized in that the content of described hard pitch is preferably 20-25% (weight percent).
4. a kind of carbon/ceramic composite material according to claim 1 is characterized in that described aspect shape BN content is preferably 10-15% (weight percent).
5. a kind of carbon/ceramic composite material according to claim 1 is characterized in that described calcined coke is calcined petroleum coke, calcining pitch coke or metallurgical coke.
6. a kind of carbon/ceramic composite material according to claim 1 is characterized in that described graphite is synthetic graphite or natural graphite.
7. a kind of carbon/ceramic composite material according to claim 1 is characterized in that described hard pitch is coal-tar pitch or petroleum pitch.
8. breaking raw material coal and making its is characterized in that:
A. prepare matrix
(1). form mixing and ball milling 6-16 hour by above-mentioned material, in the graphite mo(u)ld of packing into behind 60 mesh sieves excessively,
Calcined coke 50-70%
Hard pitch 15-30%
Graphite 2-5%
Aspect shape BN 5-20%
(2). put into give on the thermocompressor molded after, when beginning to be warming up to sintering temperature 1800-2400 ℃, in 0.5-2.0 hour, slowly be forced into sintering pressure 15-40MPa, constant temperature, pressurize 5-20 minute:
(3). naturally cool to the demoulding after the room temperature,
B. flood, curing, carbonization
(1). is the matrix that makes 50-80 ℃ at dipping temperature, and impregnation pressure is under the 1.5-3.0MPa condition, is immersed in the novolac resin, and the pressurize dipping time is 2-4 hour.
(2). after the matrix behind the dipping is forced into solidifying pressure and is 0.5MPa, beginning heats up with 1-20 ℃/hour curing heat-up rate, when temperature reaches 100 ℃, in continuing temperature-rise period, the slow step-down of solidifying pressure, when solidification value was warmed up to 150 ℃, solidifying pressure was reduced to normal pressure, and constant temperature 2-4 hour
(3). the carbonization heat-up rate with 5-20 ℃/hour under normal pressure is warming up to 800 ℃, and carbonization 2-4 hour,
(4). obtain product behind the naturally cooling.
9. a kind of breaking raw material coal and making its according to claim 8 is characterized in that the described ball milling time is preferably 10-13 hour.
10. the multiple platform preparation methods of a kind of carbon according to claim 8/pottery, the softening temperature that it is characterized in that described hard pitch is 150-200 ℃.
11. a kind of breaking raw material coal and making its according to claim 10 is characterized in that the softening temperature of described hard pitch is preferably 170-180 ℃.
12. a kind of breaking raw material coal and making its according to claim 8 is characterized in that described sintering temperature is preferably 2000-2200 ℃.
13. a kind of breaking raw material coal and making its according to claim 8 is characterized in that described sintering pressure is preferably 20-30MPa.
14. a kind of breaking raw material coal and making its according to claim 8 is characterized in that described dipping temperature is preferably 60-70 ℃.
15. a kind of breaking raw material coal and making its according to claim 8 is characterized in that described impregnation pressure is preferably 2.0-2.5MPa.
16. a kind of breaking raw material coal and making its according to claim 8 is characterized in that described curing heat-up rate is preferably 2-5 ℃/hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96101061A CN1062541C (en) | 1996-01-30 | 1996-01-30 | Carbon/ceramic composite material and its preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96101061A CN1062541C (en) | 1996-01-30 | 1996-01-30 | Carbon/ceramic composite material and its preparing method |
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| CN1156132A true CN1156132A (en) | 1997-08-06 |
| CN1062541C CN1062541C (en) | 2001-02-28 |
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|---|---|---|---|
| CN96101061A Expired - Fee Related CN1062541C (en) | 1996-01-30 | 1996-01-30 | Carbon/ceramic composite material and its preparing method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041290C (en) * | 1996-04-12 | 1998-12-23 | 清华大学 | Welding electrode of carbon ceramic composite materials |
| CN101550008B (en) * | 2009-04-24 | 2011-08-17 | 无锡中强电碳有限公司 | Production method of carbon-pottery composite material |
| CN107721426A (en) * | 2017-11-07 | 2018-02-23 | 中国科学院山西煤炭化学研究所 | A kind of processing method for the graphite material for preparing mould |
| CN107887045A (en) * | 2017-11-07 | 2018-04-06 | 中国科学院山西煤炭化学研究所 | A kind of fusedsalt reactor is pyrolyzed the preparation method of carbon coating with graphite surface |
| CN108109707A (en) * | 2017-11-07 | 2018-06-01 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of fusedsalt reactor graphite surface pyrolytic graphite coating |
| CN112142469A (en) * | 2020-09-30 | 2020-12-29 | 山东博奥新材料技术有限公司 | Graphite-based oxidation-resistant section bar, preparation method and application |
| CN113185291A (en) * | 2021-04-20 | 2021-07-30 | 富耐克超硬材料股份有限公司 | Preparation method of heat dissipation substrate material for electronic packaging |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0676666B2 (en) * | 1987-02-10 | 1994-09-28 | 株式会社半導体エネルギ−研究所 | Carbon film production method |
| US5336454A (en) * | 1993-03-26 | 1994-08-09 | Advanced Ceramics Corporation | Ceramic composite and method |
-
1996
- 1996-01-30 CN CN96101061A patent/CN1062541C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041290C (en) * | 1996-04-12 | 1998-12-23 | 清华大学 | Welding electrode of carbon ceramic composite materials |
| CN101550008B (en) * | 2009-04-24 | 2011-08-17 | 无锡中强电碳有限公司 | Production method of carbon-pottery composite material |
| CN107721426A (en) * | 2017-11-07 | 2018-02-23 | 中国科学院山西煤炭化学研究所 | A kind of processing method for the graphite material for preparing mould |
| CN107887045A (en) * | 2017-11-07 | 2018-04-06 | 中国科学院山西煤炭化学研究所 | A kind of fusedsalt reactor is pyrolyzed the preparation method of carbon coating with graphite surface |
| CN108109707A (en) * | 2017-11-07 | 2018-06-01 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of fusedsalt reactor graphite surface pyrolytic graphite coating |
| CN112142469A (en) * | 2020-09-30 | 2020-12-29 | 山东博奥新材料技术有限公司 | Graphite-based oxidation-resistant section bar, preparation method and application |
| CN112142469B (en) * | 2020-09-30 | 2021-03-26 | 山东博奥新材料技术有限公司 | Graphite-based oxidation-resistant section bar, preparation method and application |
| CN113185291A (en) * | 2021-04-20 | 2021-07-30 | 富耐克超硬材料股份有限公司 | Preparation method of heat dissipation substrate material for electronic packaging |
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| Publication number | Publication date |
|---|---|
| CN1062541C (en) | 2001-02-28 |
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