CN100546945C - The rapid chemical liquid-phase vaporization osmose process prepares the technology of charcoal/charcoal component - Google Patents
The rapid chemical liquid-phase vaporization osmose process prepares the technology of charcoal/charcoal component Download PDFInfo
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Abstract
The invention discloses the technology that a kind of rapid chemical liquid-phase vaporization osmose process prepares charcoal/charcoal component, it may further comprise the steps: (1) shove charge (charcoal/charcoal component precast body, graphite heater and thermopair etc. are installed); (2) charging: in body of heater, add liquid precursor by liquid precursor supply and return-flow system; (3) bleed, fill protection gas: air in the body of heater is evacuated to below the 5kPa, in body of heater, charges into protection gas to one normal atmosphere then; (4) open heating power supply, intensification; (5) insulation, gaseous state precursor cracking deposit carbon; (6) powered-down, cooling; (7) take out goods: obtain charcoal/charcoal component density and reach 1.60～1.70g/cm
3
Description
(1) technical field:
The present invention relates to a kind of quick preparation carbon/carbon composite technology, particularly induction heating chemical liquid phase gasification infiltration prepares the method for charcoal/charcoal component, belongs to the carbon/carbon composite technical field.
(2) background technology:
Carbon/carbon composite is widely used in Aeronautics and Astronautics and civil area because of its excellent high-temperature mechanics, calorifics and friction and wear behavior, especially as aviation brake materials such as aeroplane brake discses.At present, two kinds of main method of preparation carbon/carbon composite are chemical vapor infiltration (Chemical Vapor Infiltration, be called for short CVI) and resin, bituminizing charring.But its preparation cycle often reaches hundreds and thousands of hours, thereby causes its cost too high.Therefore, the fast densified metallization processes of developing this advanced material has become various countries competitively to strive the focus of pursuing.
Chemical liquid phase vapor deposition method is the novel method of preparation carbon/carbon composite, have very big potentiality aspect the preparation cost that shortens preparation cycle and reduction carbon/carbon composite, particularly effect is particularly evident aspect preparation and reparation carbon/carbon composite aeroplane brake discs.But, show that according to the open results reported of home and overseas this method prepares the charcoal dish and also only limits to laboratory scale, also have with a certain distance from industrialization, and technology is still unstable.At present this method also just rest on small sample with and laboratory study stage of aspects such as sedimentation mechanism, performance.The quick liquid-phase vaporization method fabricating technology of large-sized charcoal dish does not also have maturation, the domestic charcoal dish overall dimension of this method preparation of utilizing is external diameter 140mm, the patent No. is CN1766153, name is called the patent of " method that heat gradient chemical gaseous phase permeation prepares carbon/carbon compound material fast ", but once can only prepare a dish.
(3) summary of the invention:
The objective of the invention is to: propose the technology that the rapid chemical liquid-phase vaporization osmose process prepares charcoal/charcoal component,, once can deposit polydisc to overcome the prior art deficiency; Shortened the preparation cycle of charcoal/charcoal component greatly, significantly reduced its preparation cost, provide direction for this material is widely applied to civil area.
A kind of rapid chemical liquid-phase vaporization osmose process of the present invention prepares the technology of charcoal/charcoal component, and its depositing device reaches technical process fully respectively as Fig. 1, shown in Figure 3, and implementation process mainly comprises the following steps:
(1) shove charge: the charcoal/charcoal component precast body is pressed on the graphite heater, in the body of heater of packing into; Separate with pad between the charcoal/charcoal component precast body, their are supported and have good positioning with support.
(2) charging: in body of heater, add liquid precursor by liquid precursor supply and return-flow system, be lower than charcoal/charcoal component precast body lower surface 50～150mm height up to liquid level.
(3) bleed, fill protection gas: start oil-sealed rotary pump, air in the body of heater is evacuated to below the 5kPa, stop oil-sealed rotary pump, in body of heater, charge into protection gas to one normal atmosphere by gas valve then; Open valve and guarantee that protection gas continues to charge in the body of heater in the whole process; Open each cooling water inlet and outlet.
(4) open heating power supply, intensification: start induction heating power system and cooling for reflux system, make the graphite heater surface temperature rise to 900～1200 ℃ fast.
(5) insulation, deposition: liquid precursor evaporation back enters the charcoal/charcoal component precast body by the mode of infiltration and diffusion, and densification process is progressively passed laterally by inboard high temperature face; Reaction product small molecules hydrocarbon polymer and hydrogen are discharged by valve, and unreacted or partial reaction product are back in the body of heater after condensation; Furnace pressure is a normal atmosphere or pressure-fired; Depositing time is 20～30 hours.
(6) powered-down, cooling.
(7) take out goods: obtain charcoal/charcoal component density and reach 1.60～1.70g/cm
3
Wherein, the graphite heater in the described step (1) is of a size of: external diameter 300～540mm, internal diameter 150～300mm, thick 80～120mm;
Wherein, the thickness of the pad in the described step (1) is 5～20mm.
Wherein, protection gas is nitrogen or argon gas in the described step (3).
Wherein, when the graphite heater surface temperature in the described step (4) rises to 900～1200 ℃, in charcoal/charcoal component precast body thickness direction formation 500～700 ℃ thermograde from inside to outside, the side high-temperature zone forms 20～40 ℃ thermograde along radial direction within it.
Wherein, the pressure-fired in the described step (5) is: 1～1.1 normal atmosphere.
The rapid chemical liquid-phase vaporization depositing device mainly comprises body of heater 6, Controlling System 9, induction heating power system 12, ruhmkorff coil 13, bell 20, refrigeration system 27, online gas detecting system 29, tank level control system 9, liquid precursor supply and return-flow system 40 etc.
The present invention's beneficial effect compared with prior art is:
(1) the present invention has improved existing chemical liquid phase vapor deposition tooling, prepares large size (external diameter 300～540mm) charcoal/charcoal components.
(2) the present invention has shortened the preparation cycle of charcoal/charcoal component greatly, can disposable in 30 hours charcoal/charcoal component density be brought up to 1.6g/cm
3More than, thereby significantly reduced its preparation cost.
(3) the specially designed cooling for reflux of employing system refluxes more presoma or unreacted hydrocarbon polymer, thereby has improved raw material availability, has reduced the Composite Preparation cost.
(4) adopt the Frequency Induction Heating graphite heater, guaranteed the thermograde of enough temperature rise rates, thickness direction and the homogeneity of radial temperature.
(5) the present invention has overcome the shortcoming that prior art one stove can only deposit a charcoal/charcoal component, once can deposit four charcoal/charcoal components simultaneously.And the number of components can be according to the lengthening of ruhmkorff coil and corresponding increase.
(4) description of drawings:
Fig. 1 is charcoal/charcoal component rapid chemical liquid-phase vaporization osmose process deposition apparatus figure among the present invention
Fig. 2 is charcoal/charcoal component precast body and thermopair scheme of installation
Fig. 3 prepares the charcoal/charcoal component process flow sheet for the rapid chemical liquid-phase vaporization osmose process
Fig. 4 is a different positions temperature variation curve in the charcoal/charcoal component preparation process
Fig. 5 a is the densification curve under 1100 ℃ of the charcoal felt precast body charcoal/charcoal components
Fig. 5 b is the densification curve under 1100 ℃ of the Nomex precast body charcoal/charcoal components
Fig. 6 a is charcoal felt precast body charcoal/charcoal component sample polarized light microscopy (PLM) photo
Fig. 6 b is Nomex precast body charcoal/charcoal component sample polarized light microscopy (PLM) photo
Concrete label is as follows among the figure:
1 cooling water inlet, 2 cooling water outlets, 3 furnace bottoms
4 ceramic insulation supports, 5 cooling water inlets, 6 bodies of heater
7 supports, 8 charcoal/charcoal component precast bodies, 9 Controlling System
10 graphite heaters, 11 lagging materials, 12 induction heating power systems
13 ruhmkorff coils, 14 thermopairs, 15 optical observation windows
16 protection gas, 17 gas valves, 18 gas meters
19 cooling water outlets, 20 bells, 21 cooling water inlets
22 cooling for reflux systems, 23 tensimeters, 24 pressure safety valves
25 furnace top covers, 26 cooling water outlets
27 refrigeration systems, 28 valves, 29 online gas detecting systems
30 cooling water inlets, 31 knockout towers, 32 valves
33 check valves, 34 exhaust treatment systems, 35 valves
36 cooling water outlets, 37 oil-sealed rotary pumps, 38 valves
39 tank level control systems, 40 liquid precursor are supplied with and return-flow system
41 valves, 42 pads
Nomenclature:
T
1: the inboard temperature of precast body inner surface radial direction
T
2: precast body inner surface radial direction temperature outside
T
3: the precast body outside surface is the middle part temperature radially
The unit explanation:
℃ degree centigrade
Min minute
G/cm
3Gram per centimeter
3
H hour
KPa kPa
(5) embodiment:
A kind of rapid chemical liquid-phase vaporization osmose process of the present invention prepares the technology of charcoal/charcoal component, and as Fig. 1, shown in Figure 3, implementation process mainly comprises the following steps: respectively for its depositing device and technical process
(1) shove charge: charcoal/charcoal component precast body 8 is pressed on the graphite heater 10, in the body of heater 6 of packing into; Separate with pad 42 between the charcoal/charcoal component precast body 8, their are supported and have good positioning with support 7.
(2) charging: in body of heater 6, add liquid precursor by liquid precursor supply and return-flow system 40, be lower than charcoal/charcoal component precast body 8 lower surfaces 50～150mm height up to liquid level.
(3) bleed, fill protection gas: start oil-sealed rotary pump, air in the body of heater 6 is evacuated to below the 5kPa, stop oil-sealed rotary pump, in body of heater 6, charge into protection gas to one normal atmosphere by gas valve then; Open valve and guarantee that protection gas continues to charge in the body of heater in the whole process; Open each cooling water inlet and outlet.
(4) open heating power supply, intensification: start induction heating power system 12 and cooling for reflux system 22, make graphite heater 10 surface temperatures rise to 900～1200 ℃ fast.
(5) insulation, deposition: liquid precursor evaporation back enters charcoal/charcoal component precast body 8 by the mode of infiltration and diffusion, and densification process is progressively passed laterally by inboard high temperature face; Reaction product small molecules hydrocarbon polymer and hydrogen are discharged by valve, and unreacted or partial reaction product are back to after condensation in the body of heater 6; Furnace pressure is a normal atmosphere or pressure-fired; Depositing time is 20～30 hours.
(6) powered-down, cooling.
(7) take out goods: obtain charcoal/charcoal component density and reach 1.60～1.70g/cm
3
The rapid chemical liquid-phase vaporization deposition apparatus of the present invention design as shown in Figure 1, is characterised in that: fixing body of heater 6 on the furnace bottom 3, and assembling bell 20 to be opened/closed has been installed cooling for reflux system 22 on the body of heater 6 on the bell 20, and said structure is formed the main body of deposition apparatus.Ruhmkorff coil 13 is installed in the body of heater 6, and connection induction heating power system 12, induction heating power system 12 connection control system 9, graphite heater 10 closely is connected with charcoal/charcoal component precast body 8, be placed on ruhmkorff coil 13 central authorities and be fixed on the support 7 on the furnace bottom 3, in cooling for reflux system 22 conduit is installed, (not shown) is introduced online gas detecting system 29 with reacted gas, and is back in the body of heater 6 through liquid precursor supply and return-flow system 40.Cooling water inlet 1 and cooling water outlet 2 are installed on the above-mentioned furnace bottom 3.The furnace wall of body of heater 6 is a water wall, and cooling water inlet 5 and cooling water outlet 36 are installed on the outer wall, and optical observation window 15 is installed on the body of heater 6, is used to observe the various phenomenons in the body of heater 6.Connect protection gas 16 on body of heater 6 outer walls, protection gas 16 is connected with body of heater 6 with gas valve 17 by gas meter 18.Protection gas 16 is by gas valve 17 controls, and gas meter 18 is measured protection airshed size, and protection gas can be nitrogen or argon gas.Graphite heater 10 adopts lagging material 11 to coat, charcoal/charcoal component precast body 8 is placed on the upper and lower surface of graphite heater 10, the outside surface of charcoal/charcoal component precast body 8 coats charcoal felt or the glass mat of one deck 2～3mm, guarantee that this precast body surface energy effectively deposits, obtain the high quality charcoal/charcoal component, its thickness is decided according to the thickness of charcoal/charcoal component precast body 8 and density and liquid precursor.Thermopair 14 is placed on graphite heater 10 and charcoal/charcoal component precast body 8 different positionss, as shown in Figure 2, measures the temperature value of different positions, and reading shows on Controlling System 9 display screens.Tank level control system 39 is installed on the body of heater 6, is controlled liquid precursor effectively, and control replenishes the time of liquid precursor in body of heater 6 internal volumes.Cooling water inlet 30 and cooling water outlet 19 are installed on the bell 20.Cooling for reflux system 22 outer walls have cooling water inlet 21 and cooling water outlet 26, and refrigeration system 27 is installed in the cooling for reflux system 22, and liquid precursor is evaporated in cooling effectively, and it is back in the body of heater 6.Tensimeter 23 is installed in the cooling for reflux system 22, the pressure in the measuring system.Pressure safety valve 24 is installed in the top of cooling for reflux system 22, and when pressure surpasses certain value, moving valve will eject automatically, effectively prevent the excessive generation blast of body of heater 6 internal pressures etc.Online gas detecting system 29 is connected the top of cooling for reflux system 22, the composition of online detection cooling gas and composition by conduit.Knockout tower 31 is connected the top of cooling for reflux system 22 by conduit, refrigerative liquid be back to by conduit that liquid precursor is supplied with and return-flow system 40 in, the refrigerative gaseous molecular flows via a conduit in the exhaust treatment system 34.Liquid precursor supplies with by liquid precursor and return-flow system 40 flows in the body of heater 6 with certain speed, and liquid precursor can be selected kerosene, gasoline, hexanaphthene, benzene, naphthalene and toluene etc. for use.
Embodiment one: rapid chemical liquid-phase vaporization osmose process of the present invention prepares the technology of charcoal/charcoal component:
(1) adopt the charcoal felt as charcoal/charcoal component precast body 8, external diameter is 450mm, and internal diameter is 230mm, and thickness is 20mm, the about 0.17g/cm of initial density
3, be placed in graphite heater 10 upper and lower surfaces, put it into then in the quick liquid-phase vaporization cvd furnace body of heater 6, with support 7 it is supported, separate with pad 42 between middle two precast bodies.Thermopair 14 is installed in as shown in Figure 2 three positions respectively.Wrap lagging material 11, build bell 20.
(2) start oil-sealed rotary pump 37, body of heater 6 is vacuumized, when furnace pressure is lower than 5KPa, charge into shielding gas 16 (nitrogen N
2) make interior 6 air pressure of stove return to a normal atmosphere; Open valve 41, allow liquid precursor kerosene enter body of heater 6, be lower than the height of charcoal/charcoal component precast body 8 lower surface 100mm up to liquid level.Open each cooling water inlet and outlet, refrigeration system 27.
(3) open induction heating power system 12, adopt 150KW power to make graphite heater 10 temperature rise to 1080～1120 ℃ of the technological temperatures of setting very soon, and charcoal/charcoal component precast body 8 outsides are because the existence of a large amount of hydrocarbon polymers makes temperature maintenance at 300～600 ℃, thereby have formed 500～700 ℃ thermograde in charcoal/charcoal component precast body 8 inside.Charcoal/charcoal component precast body 8 different sites temperature variation as shown in Figure 4.
(4) kerosene constantly enters in the body of heater 6 by liquid precursor supply and return-flow system 40, and the gaseous hydrocarbon that evaporation is got up forms pyrolytic carbon in charcoal/charcoal component precast body 8 and graphite heater 10 contact site generation scission reactions.Outwards pass gradually in the densification forward position afterwards, finally finishes whole densification process.The power of in time adjusting induction heating power system 12 in the deposition process makes depositing temperature keep stable.
(5) reaction product small molecules hydrocarbon polymer and hydrogen are discharged by valve 32, and unreacted or partial reaction product are back to after condensation in the body of heater 6.
(6) through after 14～18 hours the chemical liquid phase vapor deposition, charcoal/charcoal component density reaches 1.65～1.70g/cm
3, its densification curve is shown in Fig. 5 a, and the charcoal/charcoal component density uniformity is good.The polarized light microscopy tissue is based on rough layer pyrolytic carbon structure, shown in Fig. 6 a.
Embodiment two: rapid chemical liquid-phase vaporization osmose process of the present invention prepares the technology of charcoal/charcoal component:
(1) adopt Nomex as charcoal/charcoal component precast body 8, external diameter is 450mm, and internal diameter is 230mm, and thickness is 20mm, the about 0.55g/cm of initial density
3, be placed in graphite heater 10 upper and lower surfaces, put it into then in the quick liquid-phase vaporization cvd furnace body of heater 6, with support 7 it is supported, separate with pad 42 between middle two precast bodies.Thermopair 14 is installed in as shown in Figure 2 three positions respectively.Wrap lagging material 11, build bell 20.
(2) start oil-sealed rotary pump 37, body of heater 6 is vacuumized, when furnace pressure is lower than 5KPa, charge into N
2Shielding gas 16 makes interior 6 air pressure of stove return to a normal atmosphere; Open valve 41, allow liquid precursor kerosene enter body of heater 6, be lower than the height of charcoal/charcoal component precast body 8 lower surface 100mm up to liquid level.Open each cooling water inlet and outlet, refrigeration system 27.
(3) open induction heating power system 12, adopt 150KW power to make graphite heater 10 temperature rise to 1080～1120 ℃ of the technological temperatures of setting very soon, and charcoal/charcoal component precast body 8 outsides are because the existence of a large amount of hydrocarbon polymers makes temperature maintenance at 300～700 ℃, thereby have formed 500～700 ℃ thermograde in charcoal/charcoal component precast body 8 inside.
(4) kerosene constantly enters in the body of heater 6 by liquid precursor supply and return-flow system 40, and the gaseous hydrocarbon that evaporation is got up forms pyrolytic carbon in charcoal/charcoal component precast body 8 and graphite heater 10 contact site generation scission reactions.Outwards pass gradually in the densification forward position afterwards, finally finishes whole densification process.The power of in time adjusting induction heating power system 12 in the deposition process makes depositing temperature keep stable.
(5) reaction product small molecules hydrocarbon polymer and hydrogen are discharged by valve 32, and unreacted or partial reaction product are back to after condensation in the body of heater 6.
(6) through 25～30 hours chemical liquid phase gasification ooze long-pending after, charcoal/charcoal component density reaches 1.60～1.65g/cm
3, its densification curve is shown in Fig. 5 b, and the charcoal/charcoal component density uniformity is good.The polarized light microscopy tissue is based on rough layer pyrolytic carbon structure, shown in Fig. 6 b.
Claims (7)
1, a kind of rapid chemical liquid-phase vaporization osmose process prepares the technology of charcoal/charcoal component, it is characterized in that: this technology comprises following key step:
(1) shove charge: the charcoal/charcoal component precast body is placed in the graphite heater upper and lower surface, in the body of heater of packing into; Separate with pad between the charcoal/charcoal component precast body, their are supported and have good positioning with support;
(2) charging: in body of heater, add liquid precursor by liquid precursor supply and return-flow system, be lower than charcoal/charcoal component precast body lower surface 50～150mm height up to liquid level;
This liquid precursor is selected one or more mixtures in kerosene, gasoline, hexanaphthene, benzene, naphthalene and the toluene for use;
(3) bleed, fill protection gas: start oil-sealed rotary pump, air in the body of heater is evacuated to below the 5kPa, stop oil-sealed rotary pump, in body of heater, charge into protection gas to one normal atmosphere by gas valve then; Open valve and guarantee that protection gas continues to charge in the body of heater in the whole process; Open each cooling water inlet and outlet;
(4) open heating power supply, intensification: start induction heating power system and cooling for reflux system, make the graphite heater surface temperature rise to 900～1200 ℃ fast;
(5) insulation, deposition: liquid precursor evaporation back enters the charcoal/charcoal component precast body by the mode of infiltration and diffusion, and densification process is progressively passed laterally by inboard high temperature face; Reaction product small molecules hydrocarbon polymer and hydrogen are discharged by valve, and unreacted or partial reaction product are back in the body of heater after condensation; Furnace pressure is a normal atmosphere or pressure-fired; Depositing time is 20～30 hours;
Described pressure-fired is: 1～1.1 normal atmosphere;
(6) powered-down, cooling;
(7) take out goods and obtain charcoal/charcoal component.
2, rapid chemical liquid-phase vaporization osmose process according to claim 1 prepares the technology of charcoal/charcoal component, it is characterized in that: the charcoal/charcoal component precast body is of a size of in the described step (1): external diameter 300～540mm, internal diameter 150～300mm, thick 15～30mm.
3, rapid chemical liquid-phase vaporization osmose process according to claim 1 prepares the technology of charcoal/charcoal component, it is characterized in that: the graphite heater in the described step (1) is of a size of: external diameter 300～540mm, and internal diameter 150～300mm, thick 80～120mm:
4, rapid chemical liquid-phase vaporization osmose process according to claim 1 prepares the technology of charcoal/charcoal component, it is characterized in that: the thickness of the pad in the described step (1) is 5～20mm.
5, rapid chemical liquid-phase vaporization osmose process according to claim 1 prepares the technology of charcoal/charcoal component, it is characterized in that: protection gas is nitrogen or argon gas in the described step (3).
6, rapid chemical liquid-phase vaporization osmose process according to claim 1 prepares the technology of charcoal/charcoal component, it is characterized in that: when the graphite heater surface temperature rises to 900～1200 ℃ in the described step (4), in charcoal/charcoal component precast body thickness direction formation 500～700 ℃ thermograde from inside to outside.
7, rapid chemical liquid-phase vaporization osmose process according to claim 1 prepares the technology of charcoal/charcoal component, it is characterized in that: when the graphite heater surface temperature rose to 900～1200 ℃ in the described step (4), the side high-temperature zone formed 20～40 ℃ thermograde along radial direction within it.
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| CN103044056B (en) * | 2013-01-10 | 2014-08-13 | 湖南南方搏云新材料有限责任公司 | Technology and equipment for preparing C/C composite |
| CN103193498B (en) * | 2013-04-07 | 2014-06-18 | 山东国晶新材料有限公司 | Narrow flow induction coupling chemical vapor deposition (CVD) densification method for rapidly preparing carbon/carbon composite material crucible |
| CN104193379B (en) * | 2014-07-31 | 2015-09-02 | 山东大学 | Liquid phase pyrolysis deposition prepares device and the technique of carbon fiber reinforced carbon based composites |
| CN105016760B (en) * | 2015-07-09 | 2017-04-05 | 西北工业大学 | A kind of preparation method of the modified C/C composites of superhigh temperature ceramics |
| CN110030828A (en) * | 2019-04-23 | 2019-07-19 | 西安航空制动科技有限公司 | A kind of vaccum sensitive stove |
| CN116283330A (en) * | 2022-10-19 | 2023-06-23 | 西北工业大学 | Preparation method of directional deposition heterogeneous CC composite material |
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