CN1945048A - Process for preparing carbon/carbon braking material for high speed train - Google Patents
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- CN1945048A CN1945048A CN 200610117664 CN200610117664A CN1945048A CN 1945048 A CN1945048 A CN 1945048A CN 200610117664 CN200610117664 CN 200610117664 CN 200610117664 A CN200610117664 A CN 200610117664A CN 1945048 A CN1945048 A CN 1945048A
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Abstract
The present invention relates to high speed train braking material technology, and is especially process of preparing composite carbon/carbon material for braking in high speed train. The composite carbon/carbon material is prepared through needling large tow polyacrylonitrile carbon fiber or pre-oxidized no-weft fabric and thin short fiber felt to form blank, fast deposition to deposit pyrolytic carbon layer on the surface of carbon fiber to reach blank density of about 1.50 g/cu cm, medium pressure dipping and carbonizing to further increase the blank density to 1.70-1.80 g/cu cm and form the prefabricated part of composite carbon/carbon material, and final high temperature graphitization. The present invention has lowered cost of composite carbon/carbon material.
Description
Technical field
The present invention relates to a kind of technical field of high-speed train braking material preparation, especially a kind of high-speed train braking preparation method of carbon/carbon compound material.
Background technique
Long-term safety and lightweight are two key technical problems that development high-speed rail transportation technology must be considered.Braking system is to ensure hot-short safety and realize a light-weighted critical system.Along with improving constantly of train speed, the secondary fretting wear that will stand strong high temperature impact and mechanical brake of its brake, also more and more higher to the physical and chemical performance and the mechanical property requirement of braking device and brake material.Make a general survey of bullet train disc braking Development of Materials, its trend is by homogenous material, low heat capacity, low high temperature specific strength (intensity/proportion), lowly heat-resistingly split, the low-heat impact to composite material, high heat capacity, high specific strength, highly heat-resistingly split, high thermal shock resistance properties direction develops.The selection of bullet train friction braking material can reduce following requirement: stable frictional behaviour, friction factor does not change with the variation of pressure, temperature, speed and humidity, higher wear-resisting and anti-fatigue performance is guaranteed long working life, good braking ability, enough intensity, high thermal, lower density, be easy to make and lower cost, requiring it to have very high thermal capacity to be beneficial to Brake Energy stores, have good thermal conductivity simultaneously to reduce temperature gradient, reduce hot spot and form.High thermal shock, high energy when traditional high-speed train braking material such as spheroidal graphite cast iron, middle phosphorus cast iron, high-phosphorous iron, (semimetal) Steel Fibre reinforced plastic, ceramic powder metallurgical material are difficult to satisfy the 250-350km/H braking carries, the requirement of high heat radiation, high strength, high friction ractor, low abrasion loss.When retro-speed reached 250-350km/H, the brake lining temperature was up to 1000-1200 ℃, and the semimetal brake lining can decompose in carbonization, and the ceramic powder brake lining can lose by force, distortion, adhesion, even cracked.Therefore need the more satisfactory high-speed train braking material of development performance.
Carbon/carbon compound material has excellent high temperature abrasion resistance, heat-resistant cracking and hot strength, and it is in light weight, and specific strength is big, the specific modulus height, and thermal expansion coefficient is low, and specific heat is big.Superior structure and functional characteristic make it become desirable braking material.Be used for guided missile, astrovehicle, aircraft in a large number at present.But because process for manufacturing carbon/carbon composite material complexity, the manufacture cycle of this type of purposes are tediously long, raw material are expensive, make its cost high, hinder its application to civilian industry.With regard to advanced country in the world, the key that carbon/carbon braking material for high speed train is not widely applied as yet also is the restriction that is subjected to price.And train is different from aircraft, and its weight price is than much smaller, thereby more is necessary to prepare the low-cost and high-performance carbon/carbon braking material that is suitable for bullet train.
In order to satisfy the high request of train speed raising to brake material, and the cost problem of solution restriction carbon/carbon braking material application, the present invention adopts the whole felt of low-cost large-tow carbon fiber acupuncture by uniting, liquid vapor deposition compact technology, middle pressure carbonization technology prepare carbon/carbon braking material for high speed train fast, and its cost is reduced significantly.
The extraordinary polyacrylonitrile carbon fiber of little tow is the first-selected reinforcing material that the carbon/carbon compound material of Aeronautics and Astronautics, national defense industry purposes is made for many years always, but it costs an arm and a leg, and product is difficult to owing to preparation technology is highly confidential circulate.After the mid-90, big tow polyacrylonitrile carbon fiber performance obtains to significantly improve, its greatest feature is under the suitable prerequisite of performance, and price is than the low 30%-50% of little tow polyacrylonitrile carbon fiber, and can adopt civilian polyacrylonitrile that market openly can buy as the preparation raw material; Best performance is vapor deposition carbon (CVD carbon) in the matrix carbon of carbon/carbon compound material, thereby 60-70% is a CVD carbon in the aeroplane brake discs material matrix, but the high cycle of the cost that obtains this carbon is long, the brake disc vapor deposition time of general Φ 320 * 25 up to 1500 hours about, this makes the cost of aeroplane brake discs up to 4000-6000 unit/kilogram, at the carbon/carbon compound material of the termination of rocket portion unexpectedly up to ten thousand yuan/kilogram of 1.5-2.The liquid vapour deposition process (CLVD) that development in recent years is got up can be fine and close in 1.8g/cm at 8 hours with the aeroplane brake discs of Φ 320
3When with the CLVD method with the goods densification to 1.4g/cm
3-1.6g/cm
3The time, increase density rate and slow down, need use the further density of dipping-carbonizatin method.In order to reduce cost the shortening cycle, press dipping, the further density of middle pressure carbonizatin method in the employing.Though press carbonizatin method to make the carboloy residue of the carboloy residue of pitch in this, but equipment manufacturing cost is the 1/5-1/10 of high pressure carbonization a little less than the high pressure carbonization.Safe in the high pressure carbonization, plant maintenance is simplified, and operation is simple.
The method and the technology of not appearing in the newspapers at present with the whole carbon felt of big tow polyacrylonitrile, CLVD-middle pressure dipping-middle pressure carbonization densification prepare carbon/carbon braking material for high speed train.
Summary of the invention
Technical problem to be solved by this invention is to unite to adopt low-cost body preparation technology, quick liquid vapor deposition compact technology, middle pressure carbonization technology to prepare carbon/carbon braking material for high speed train, and its cost is reduced significantly.
The technical solution used in the present invention: a kind of preparation method of carbon/carbon braking material for high speed train comprises the following steps:
(1) preparation of base substrate
Selection is paved into no latitude cloth more than or equal to big tow polyacrylonitrile-based carbon fibre of 48K or pre-oxygen silk, weak point cuts large-tow carbon fiber or pre-oxygen silk is made mat, one deck does not have latitude cloth and one deck mat lamination mutually, adjacent two layers does not have latitude cloth and is 0～90 ° of shop layer, gets discoid whole carbon felt base substrate with TN1200-YCX type pre-shaping needing machine and the acupuncture of TN700-CX type shaping needing machine interlayer;
(2) the chemical liquids vapour deposition process densification of base substrate
Adopt the chemical liquids vapour deposition process that the base substrate that step (1) makes is carried out densification, the chemical liquids vapor deposition is finished in homemade induction heating liquid gaseous phase deposition stove, the discoid base substrate that step (1) is made is fixed in the stove on the cylindric heater, add liquid hydrocarbon in the stove with the base substrate submergence, energising heats up, after system is heated to 900-1200 ℃ of temperature, with solid-liquid interface that base substrate contacts on, liquid hydrocarbon absorbs heat and is converted into gaseous state, vaporized liquid hydrocarbon infiltrates base substrate inside rapidly by the pore structure of base substrate, lytic response takes place deposit RESEARCH OF PYROCARBON, liquid hydrocarbon ebullition, gasification thermal loss descends the base substrate temperature outside and the inboard that contacts with heater still keeps high temperature, like this in the bigger temperature gradient of the inner generation of base substrate, along with the pore structure of inside gradually by packing, pass gradually laterally from the base substrate inboard in the densification forward position, obtains all even compacts of inside and outside at last, density is 1.50g/cm
3-1.60g/cm
3Carbon/carbon compound material, in experimentation, continue to feed protective gas N
2Or argon gas, flow 30-120L/h is till furnace temperature is reduced to room temperature;
(3) the middle pressure dipping-carbonization densification of the fine and close part of chemical liquids vapor deposition
Density after step (2) densification is not reached the base substrate of requirement, press dipping in continuing to use, the method of middle pressure carbonization is densification repeatedly, promptly in the dipping still with step (2) densification after the density base substrate that do not reach requirement be dipped in the liquid hydrocarbon, the 2-5Mpa medium pressure, in liquid hydrocarbon, flood 1-4h under the 150-300 ℃ of temperature conditions, make liquid hydrocarbon infiltrate base substrate gradually and fill space residual in the base substrate, base substrate after will flooding again is placed on heat treatment in the vacuum carburization stove, make the liquid hydrocarbon carbonization of infiltration, pressure in the stove: 6～10Mpa, temperature: 800-1000 ℃, time: 2-5h makes base substrate fine and close in 1.70g/cm
3～1.80g/cm
3, form the carbon/carbon compound material prefabricated component;
(4) high temperature graphitization of densification base substrate prefabricated component is handled
Density after step (2), step (3) densification is met the requirements of the carbon/carbon compound material prefabricated component in the high temperature graphitization stove, carry out the high temperature graphitization processing; Turbostratic carbon in the prefabricated component is changed to the graphite crystal of three-dimensional order; earlier system of bf body is vacuumized during graphitization processing; degree of vacuum reaches-charge into the shielding gas high-purity argon gas behind the 0.1MPa, and gas flow is 20-30Lh
-1, graphitization temperature: 1800 ℃-2800 ℃, holding time: 1-3h, heating rate: 1 ℃ of min
-1-10 ℃ of min
-1, the high temperature graphitization treatment process of densification base substrate finishes the back and freely lowers the temperature, and treats stove cooling back sampling.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.A kind of low-cost carbon/carbon braking material preparation method comprises the following steps:
(1) preparation of base substrate
Select above big tow polyacrylonitrile carbon fiber (PANCF) of 48K or pre-oxygen silk body preparation raw material as carbon/carbon braking material.With big tow polyacrylonitrile carbon fiber through a minute silk, the shop put no latitude cloth, the 40-100mm chopped strand is through carding, one-tenth net, get the short fibre mat with the acupuncture of TN1200-YCX type pre-shaping needing machine, one deck PANCF does not have latitude cloth and one deck short fibre mat lamination mutually, the no latitude cloth of each layer long filament is one dimension and distributes angled between adjacent layer (0～90 °).Adopt TN700-CX type shaping acupuncture eedle sting accurate three-dimension integrally carbon felt base substrate, short fibre provides the tow source for acupuncture, short fibre plays fixedly long filament by the Vertical direction of the hook introducing cloth cover of dental nerve hook, and no latitude cloth and short fibre mat are become one.
(2) the chemical liquids vapour deposition process densification of base substrate
Adopt the chemical liquids vapour deposition process that the base substrate that step (1) makes is carried out densification.Precipitation equipment is an induction heater, adds liquid hydrocarbon in the furnace chamber, and precast body is immersed in the liquid hydrocarbon, and closely contact with cylindric heater, the side temperature that base substrate contacts with heater is higher, and base substrate outer surface one side temperature is lower, like this in the bigger heat gradient of the inner generation of precast body.After whole system was heated to uniform temperature, the liquid hydrocarbon boiling was more and more violent, and the inboard high-temperature zone of base substrate lytic response takes place deposits RESEARCH OF PYROCARBON, by product such as hydrogen and various hydrocarbons etc. are discharged from condenser overhead, with the carrying out of deposition process, progressively extrapolate in the high-temperature zone, finishes densification.In experimentation, continue to feed protective gas, till furnace temperature is reduced to room temperature.Process parameter is:
Liquid hydrocarbon: cyclopentane, cyclohexane, kerosene, gasoline (90
#), diesel oil (0
#)
Depositing temperature: 900-1200 ℃
Deposition pressure: 1-5ATM
Shielding gas: N
2Or argon gas, flow 30-120L/h
(3) the middle pressure dipping-carbonization densification of the fine and close part of chemical liquids vapor deposition
Density after step (2) densification is not reached the base substrate of requirement, continue with in press dipping, middle pressure carbonization method densification repeatedly.Impregnating equipment is the dipping still, and carbonizing apparatus is the vacuum carburization stove.Process parameter is:
The middle dipping of pressing:
Impregnating agent: coal tar pitch, phenolic resin, furan
Pressure: 2-5Mpa, temperature: 150-300 ℃, the time: 1-4h
The carbonization of middle pressure:
Pressure: 6～10Mpa, temperature: 800-1000 ℃, the time: 2-5h
(4) high temperature graphitization of densification base substrate is handled
Density after step (2), step (3) densification is met the requirements of base substrate carry out the high temperature graphitization processing.
High temperature graphitization is handled and is carried out in the high temperature graphitization stove.Earlier system of bf body being vacuumized during graphitization processing, degree of vacuum reaches-charge into protection gas (high-purity argon gas) behind the 0.1MPa, gas flow is 20-30Lh
-1Technology finishes the back and freely lowers the temperature, and treats stove cooling back sampling.Process parameter is:
Graphitization temperature: 1800 ℃-2800 ℃
Holding time: 1-3h
Heating rate: 1 ℃ of min
-1-10 ℃ of min
-1
Embodiment 1
Select the big tow polyacrylonitrile carbon fiber of 48K (PANCF) of cellulose ester company of Japanese eastern nation to arrange into no latitude cloth, the pre-oxygen silk of the big tow polyacrylonitrile of 48K (PANOF) acupuncture prepares the chopped strand mat.Adopt one deck PANCF not have latitude cloth and one deck PANOF short fibre mat lamination mutually, adjacent two layers does not have latitude cloth and is 90 ° of shop layers, respectively in X, Y direction continuous needle and must whole carbon felt successively.
Adopt the chemical liquids vapour deposition process to acupuncture and whole carbon felt base substrate carry out densification.Add liquid hydrocarbon in the induction heater furnace chamber, precast body is contained on the heater, and immerse in the liquid hydrocarbon, energising makes the whole system heating.In experimentation, continue to feed protective gas, till furnace temperature is reduced to room temperature.Process parameter is:
Precursor: kerosene
Depositing temperature: 950 ℃
Deposition pressure: 1-5ATM
Shielding gas atmosphere: N
2, flow 90L/h
In the high temperature graphitization stove, density after densification is met the requirements of base substrate and carry out the high temperature graphitization processing.Earlier system of bf body being vacuumized, degree of vacuum reaches-charge into protection gas (high-purity argon gas) behind the 0.1MPa, gas flow is 30Lh
-1Technology finishes the back and freely lowers the temperature, and treats stove cooling back sampling.
Process parameter is:
Graphitization temperature: 2600 ℃
Holding time: 1h
Heating rate: 10 ℃ of min
-1
Every performance of the carbon/carbon braking material that makes of technology is as follows thus:
| Project | Measured result |
| Density | 1.78g/cm 3 |
| Resistance to flexure | 103.77Mpa |
| Interlaminar shearing strength | 12.04Mpa |
| Compressive strength | 80.21Mpa |
| Thermal conductivity (under 800 ℃) | 78.5W/mK |
| Specific heat (under 800 ℃) | 0.439cal·g -1·K -1 |
| Expansion coefficient (under 800 ℃) | -0.328 |
Embodiment 2
Adopt the 48K pre-oxygen silk of big tow polyacrylonitrile (PANOF) of cellulose ester company of Japanese eastern nation to arrange into no latitude cloth, the pre-oxygen silk of TX-3 type polyacrylonitrile (PANOF) acupuncture of Jilin carbon element 12K that group company produces prepares the chopped strand mat.Adopt one deck PANOF not have latitude cloth and one deck PANOF short fibre mat lamination mutually, adjacent two layers does not have latitude cloth and is 90 ° of shop layers, respectively in X, Y direction continuous needle and must whole carbon felt successively.
Adopt the chemical liquids vapour deposition process to acupuncture and whole carbon felt base substrate carry out densification.Add liquid hydrocarbon in the induction heater furnace chamber, precast body is contained on the heater, and immerse in the liquid hydrocarbon, energising makes the whole system heating.In experimentation, continue to feed protective gas, till furnace temperature is reduced to room temperature.Process parameter is:
Precursor: kerosene
Depositing temperature: 900 ℃
Deposition pressure: 1-5ATM
Shielding gas atmosphere: N
2, flow 90L/h
In the high temperature graphitization stove, density after densification is met the requirements of base substrate and carry out the high temperature graphitization processing.Earlier system of bf body being vacuumized, degree of vacuum reaches-charge into protection gas (high-purity argon gas) behind the 0.1MPa, gas flow is 30Lh
-1
Technology finishes the back and freely lowers the temperature, and treats stove cooling back sampling.
Process parameter is:
Graphitization temperature: 2600 ℃
Holding time: 1h
Heating rate: 10 ℃ of min
-1
Every performance of the carbon/carbon braking material that makes of technology is as follows thus:
| Project | Measured result |
| Density | 1.77g/cm 3 |
| Resistance to flexure | 102.13 |
| Interlaminar shearing strength | 11.91 |
| Compressive strength | 128.4 |
| Thermal conductivity (under 800 ℃) | 0.456cal·g-1·K-1 |
| Specific heat (under 800 ℃) | -0.149 |
| Expansion coefficient (under 800 ℃) | 102.13 |
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technological scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (4)
1. the preparation method of a carbon/carbon braking material for high speed train comprises the following steps:
(1) preparation of base substrate
Selection is paved into no latitude cloth more than or equal to big tow polyacrylonitrile-based carbon fibre of 48K or pre-oxygen silk, weak point cuts large-tow carbon fiber or pre-oxygen silk is made mat, one deck does not have latitude cloth and one deck mat lamination mutually, adjacent two layers does not have latitude cloth and is 0～90 ° of shop layer, gets discoid whole carbon felt base substrate with TN1200-YCX type pre-shaping needing machine and the acupuncture of TN700-CX type shaping needing machine interlayer;
(2) the chemical liquids vapour deposition process densification of base substrate
Adopt the chemical liquids vapour deposition process that the base substrate that step (1) makes is carried out densification, the chemical liquids vapor deposition is finished in homemade induction heating liquid gaseous phase deposition stove, the discoid base substrate that step (1) is made is fixed in the stove on the cylindric heater, add liquid hydrocarbon in the stove with the base substrate submergence, energising heats up, after system is heated to 900-1200 ℃ of temperature, on a solid liquid interface that contacts with base substrate, liquid hydrocarbon absorbs heat and is converted into gaseous state, vaporized liquid hydrocarbon infiltrates base substrate inside rapidly by the pore structure of base substrate, lytic response takes place deposit RESEARCH OF PYROCARBON, liquid hydrocarbon ebullition, gasification thermal loss descends the base substrate temperature outside and the inboard that contacts with heater still keeps high temperature, like this in the bigger temperature gradient of the inner generation of base substrate, along with the pore structure of inside gradually by packing, pass gradually laterally from the base substrate inboard in the densification forward position, obtains all even compacts of inside and outside at last, density is 1.40g/cm
3-1.60g/cm
3Carbon/carbon compound material, in experimentation, continue to feed protective gas N
2Or argon gas, flow 30-120L/h is till furnace temperature is reduced to room temperature;
(3) the middle pressure dipping-carbonization densification of the fine and close part of chemical liquids vapor deposition
Density after step (2) densification is not reached the base substrate of requirement, press dipping in continuing to use, the method of middle pressure carbonization is densification repeatedly, promptly in the dipping still with step (2) densification after the density base substrate that do not reach requirement be dipped in the liquid hydrocarbon, the 2-5Mpa medium pressure, in liquid hydrocarbon, flood 1-4h under the 150-300 ℃ of temperature conditions, make liquid hydrocarbon infiltrate base substrate gradually and fill space residual in the base substrate, base substrate after will flooding again is placed on heat treatment in the vacuum carburization stove, make the liquid hydrocarbon carbonization of infiltration, pressure in the stove: 6～10Mpa, temperature: 800-1000 ℃, time: 2-5h makes base substrate fine and close in 1.70g/cm
3～1.80g/cm
3, form the carbon/carbon compound material prefabricated component;
(4) high temperature graphitization of densification base substrate prefabricated component is handled
Density after step (2), step (3) densification is met the requirements of the carbon/carbon compound material prefabricated component in the high temperature graphitization stove, carry out the high temperature graphitization processing; Turbostratic carbon in the prefabricated component is changed to the graphite crystal of three-dimensional order; earlier system of bf body is vacuumized during graphitization processing; degree of vacuum reaches-charge into the shielding gas high-purity argon gas behind the 0.1MPa, and gas flow is 20-30Lh
-1, graphitization temperature: 1800 ℃-2800 ℃, holding time: 1-3h, heating rate: 1 ℃ of min
-1-10 ℃ of min
-1, the high temperature graphitization treatment process of densification base substrate finishes the back and freely lowers the temperature, and treats stove cooling back sampling.
2. the preparation method of a kind of carbon/carbon braking material for high speed train according to claim 1 is characterized in that, used body preparation raw material is big tow polyacrylonitrile-based carbon fibre or the pre-oxygen silk more than or equal to 48K in the described method step (1).
3. the preparation method of a kind of carbon/carbon braking material for high speed train according to claim 1, it is characterized in that the densification of base substrate is to adopt the chemical liquids vapour deposition process in the described method step (2), its used liquid hydrocarbon is cyclopentane, cyclohexane, kerosene, gasoline (90
#), diesel oil (0
#).
4. the preparation method of a kind of carbon/carbon braking material for high speed train according to claim 1 is characterized in that, impregnating agent used in the described method step (3) is: medium temperature coal pitch, phenolic resin, furan.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101176641A CN100501185C (en) | 2006-10-27 | 2006-10-27 | Process for preparing carbon/carbon braking material for high speed train |
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|---|---|---|---|
| CNB2006101176641A CN100501185C (en) | 2006-10-27 | 2006-10-27 | Process for preparing carbon/carbon braking material for high speed train |
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| Publication Number | Publication Date |
|---|---|
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| CN100501185C CN100501185C (en) | 2009-06-17 |
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|---|---|---|---|
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