CN101215182B - Device and method for preparing carbon/carbon composite material with gradient distribution density - Google Patents
Device and method for preparing carbon/carbon composite material with gradient distribution density Download PDFInfo
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- CN101215182B CN101215182B CN2008100172680A CN200810017268A CN101215182B CN 101215182 B CN101215182 B CN 101215182B CN 2008100172680 A CN2008100172680 A CN 2008100172680A CN 200810017268 A CN200810017268 A CN 200810017268A CN 101215182 B CN101215182 B CN 101215182B
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Abstract
The invention relates to a device of carbon/carbon composite material of which the density distributes in gradient and a process for preparation. Basing on soaking method isothermal chemical vapor infiltration technology of preparing carbon/carbon composite material, the outer and inner surfaces of the precast member is filled with high concentration reacting gas and inert protective gas or low concentration reacting gas, using the concentration of the different reacting gas of the outer and inner surfaces to control gas to flow along the predetermined direction, remarkable reacting gas concentration gradient is radically formed along the member, using the different deposition rate of different reacting gas concentration under the condition of the same temperature to obtain the carbon/carbon composite material the density of which is outer high and inner low and is distributed in gradient. The invention can be used for researching solid rocket engine gradient function polybasic base composite material throat insert with different decomposition carbon content along radial direction and polybasic carbon base carbon/carbon composite material plane brake wheel and the like, which is suited for solid rocket engine throat insert, various plane carbon brake stator and the tail wheel structure.
Description
Technical field
The present invention relates to a kind of device and method for preparing carbon/carbon composite, particularly relate to a kind of device and method for preparing the carbon/carbon composite of its density distribution gradient.
Background technology
The application of density gradient carbon/carbon composite has mainly utilized the different qualities of different matrix in the matrix material or dissimilar charcoals to carry out the accurate design of composite structure.For example, obtain having the matrix material of ideal structure and performance for charcoal-refractory carbide multi-phase matrix matrix material, mixed matrix charcoal carbon/carbon composite provide base substrate.
At present, the preparation method who realizes the density gradient matrix material utilizes heat gradient chemical gaseous phase permeation (CVI) technology to be achieved, its principle is to have utilized the different sedimentation rates of carbon-source gas under differing temps, obtains the carbon/carbon composite that density gradient distributes.According to application demand, making high density area is the hot junction, and low density area is a cold junction.At present, the equipment that adopts Thermal Gradient CVI Process to produce carbon/carbon composite mainly contains two types both at home and abroad: first type is the interior hot external cooling Thermal Gradient CVI Process equipment that adopts resistance-type or Medium frequency induction formula, it is characterized in that the inboard of heating element at charcoal dish precast body, the outside is by the furnace wall water-cooled, in the radially foundation thermal gradient from the inside to the outside of precast body; What this equipment obtained is the low inside and high outside density gradient carbon/carbon composite of density, can be applicable to the development of solid propellant rocket larynx lining and aeroplane brake discs Moving plate, mainly utilize the different performance characteristics of dissimilar carbon matrixes in the carbon/carbon composite, must arrive the carbon/carbon composite that the working position has high pyrolytic carbon content.Second kind of equipment is with interior water cooling plant by the internal diameter at charcoal dish precast body, forms thermal gradient.But the density that obtains is relatively even, and the Gradient distribution characteristics are not remarkable.
Along with the development of the technology of matrix material, to more subtilizedization of design of material and the characteristics of functionalization.For this reason, functionally gradient multi-phase matrix matrix material occurred, required the carbon/carbon composite base substrate to have high outside and low outside density distribution, so that obtain the functional gradient composite materials of the outer low and inner high distribution of refractory carbide content in the later stage.
Summary of the invention
The objective of the invention is at above-mentioned the deficiencies in the prior art, provide a kind of and can be used in that radially density is high outside and low outside, have the device and method of carbon/carbon composite of its density distribution gradient of preparation of developments such as the solid propellant rocket gradient function multi-phase matrix matrix material larynx lining of different pyrolytic carbon content requirement, polynary carbon matrix carbon/carbon composite aeroplane brake discs.
For achieving the above object, the technical solution adopted in the present invention is: a kind of device for preparing the carbon/carbon composite of its density distribution gradient, comprise the chemical vapor infiltration furnace body, bell and furnace bottom lid, described upper of furnace body is provided with vacuum pumping opening, be provided with insulation quilt and insulation cover plate in the described body of heater, be provided with graphite heater in the described insulation quilt, it is characterized in that described graphite heater inside part is equipped with the graphite gas cylinder, be provided with sub-air chamber's cover plate with holes of placing precast body to be infiltrated in the described graphite gas cylinder, being positioned at sub-air chamber cover plate with holes top in the graphite gas cylinder is permeate chamber, being positioned at sub-air chamber cover plate with holes bottom in the graphite gas cylinder is sub-air chamber, and described precast body to be infiltrated top is provided with lamina tecti; Pass described furnace bottom lid and be provided with the outer and interlayer inlet pipe internal layer of interlayer inlet pipe, described interlayer inlet pipe is outer to be communicated with described sub-air chamber, and described interlayer inlet pipe internal layer is higher than described sub-air chamber cover plate with holes and the upper end extends precast body endoporus to be infiltrated; Described interlayer inlet pipe skin is the reactant gases inlet pipe, and described interlayer inlet pipe internal layer is shielding gas or lower concentration reactant gases inlet pipe.
The pore of described sub-air chamber cover plate with holes is along described precast body outer rim uniform distribution to be infiltrated.
Described lamina tecti is conical, truncated cone-shaped or discoideus, and the spacing of itself and described graphite gas cylinder inwall is 5mm～10mm.
Pass described body of heater, insulation quilt and graphite heater and be provided with temperature thermocouple.
Another object of the present invention provides a kind of method for preparing the carbon/carbon composite of its density distribution gradient, it is characterized in that this method may further comprise the steps:
(1) according to the dimensioned chemical vapor infiltration graphite gas cylinder of precast body to be infiltrated;
(2) successively described graphite gas cylinder, hollow cylinder precast body to be infiltrated and lamina tecti are packed in the chemical vapor infiltration furnace body;
(3) according to predetermined temperature increasing schedule furnace body temperature is risen to 800 ℃～1050 ℃;
(4) under negative pressure, feed reactant gases and shielding gas or lower concentration reactant gases, precast body outer wall to be infiltrated is a reactant gases, its inwall is shielding gas or lower concentration reactant gases, control reactant gases and shielding gas or the two relative discharge of lower concentration reactant gases, the concentration gradient that makes precast body to be infiltrated radially set up reactant gases distributes;
(5) densification rate of precast body to be infiltrated is reduced towards inboard low-concentration area gradually by its outside high density, and through 72-300 hour gas-phase carbon deposition, promptly making its external diameter density was 1.0～1.4g/cm
3, internal diameter density is 0.3～0.6g/cm
3The carbon/carbon composite of its density distribution gradient.
Reactant gases is propylene C described in the step (4)
3H
6Or methane CH
4, described shielding gas is a rare gas element.
Temperature increasing schedule described in the step (3) is furnace body temperature to be risen to 800 ℃～1050 ℃ in 6-16 hour.
Shielding gas or lower concentration reactant gases described in the step (4) feed hollow cylinder precast body endoporus to be infiltrated, and the back diffuses to precast body outer wall to be infiltrated along the hole in the precast body to be infiltrated; Reactant gases feeds sub-air chamber, after the pore on sub-air chamber's cover plate with holes flows into the outer wall of hollow cylinder precast body to be infiltrated, two kinds of gases flow out through the air outlet of precast body lamina tecti to be infiltrated top along predetermined passage directed flow.
Reactant gases and shielding gas or lower concentration flow rate of reactive gas are 1.0 ± 0.8m described in the step (4)
3/ h.
The present invention compared with prior art has the following advantages:
(1) concentration gradient by graphite frock and air inlet control design realization response gas distributes, and is little to the dependence of equipment;
(2) can realize the preparation of high outside and low outside density gradient C/C matrix material, be particularly suitable for radially having the development of the solid propellant rocket gradient function multi-phase matrix matrix material larynx lining of different pyrolytic carbon content requirement, polynary carbon matrix C/C composite airplane brake flange etc.
(3) method and apparatus of the present invention also can be used for the preparation of other type matrix density gradient composites.
Description of drawings
Fig. 1 is the apparatus structure synoptic diagram of the present invention's carbon/carbon composite of preparing its density distribution gradient.
Embodiment
A kind of device for preparing the carbon/carbon composite of its density distribution gradient as shown in Figure 1, comprise chemical vapor infiltration furnace body 2, bell 1 and furnace bottom lid 15, described body of heater 2 tops are provided with vacuum pumping opening 3, be provided with insulation quilt 14 and insulation cover plate 4 in the described body of heater 2, be provided with graphite heater 5 in the described insulation quilt 14, described graphite heater 5 inside parts are equipped with graphite gas cylinder 16, be provided with sub-air chamber's cover plate 10 with holes of placing precast body 8 to be infiltrated in the described graphite gas cylinder 16, being positioned at sub-air chamber cover plate with holes 10 tops in the graphite gas cylinder 16 is permeate chamber 6, being positioned at sub-air chamber cover plate with holes 10 bottoms in the graphite gas cylinder 16 is sub-air chamber 11, and described precast body to be infiltrated 8 tops are provided with lamina tecti 7; Pass described furnace bottom lid 15 and be provided with interlayer inlet pipe outer 13 and interlayer inlet pipe internal layer 12, described interlayer inlet pipe outer 13 is communicated with described sub-air chamber 11, and described interlayer inlet pipe internal layer 12 is higher than described sub-air chamber cover plate 10 with holes and the upper end extends precast body 8 endoporus to be infiltrated; Described interlayer inlet pipe outer 13 is the reactant gases inlet pipe; described interlayer inlet pipe internal layer 12 is shielding gas or lower concentration reactant gases inlet pipe, and described lower concentration reactant gases is lower than the reactant gases of outer 13 reacting gas concentrations of interlayer inlet pipe for its concentration.The pore of described sub-air chamber cover plate 10 with holes is along described precast body 8 outer rim uniform distribution to be infiltrated; Described lamina tecti 7 is conical, truncated cone-shaped or discoideus, and the spacing of itself and described graphite gas cylinder 16 inwalls is 5mm～10mm; Pass described body of heater 2, insulation quilt 14 and graphite heater 5 and be provided with temperature thermocouple 9.
For the realization response gas concentration radially is high outside and low outside Gradient distribution along precast body 8 to be infiltrated, inlet system is designed to the sandwich-type intake method, promptly is made up of interlayer inlet mouth internal layer 12 and interlayer inlet mouth outer 13.The reactant gases of inert protective gas or lower concentration is directly fed the center of precast body 8 to be infiltrated by interlayer inlet mouth internal layer 12; the reactant gases of high density then enters the sub-air chamber 11 that is positioned at below the precast body to be infiltrated 8 by interlayer inlet mouth skin 13; after sub-air chamber's 11 diffusions evenly, be diffused into the periphery of precast body 8 to be infiltrated by sub-air chamber's uniform pore of cover plate 10 peripheries with holes; by the relative discharge of conditioned reaction gas and shielding gas or lower concentration reactant gases, can make reactant gases radially have different concentration distribution along precast body 8 to be infiltrated.Above precast body 8 to be infiltrated, add a lamina tecti 7 and can effectively control gas flow in the permeate chamber 6.The temperature of entire reaction system is monitored by temperature thermocouple 9.
A kind of method for preparing the carbon/carbon composite of its density distribution gradient, this method may further comprise the steps:
(1) the dimensioned special graphite frock according to product to be infiltrated is a graphite gas cylinder 16.
(2) size Φ 190mm/ Φ 30mm * 200mm hollow cylinder precast body 8 to be infiltrated is put into the graphite gas cylinder 16 about internal diameter 210mm, added lamina tecti 7.Notice that the diameter of lamina tecti 7 should be no more than the external diameter of precast body 8 to be infiltrated.
(3) start the vacuum unit, vacuumize by 3 pairs of bodies of heater 2 of vacuum pumping opening, vacuum meter show negative pressure be-0.086MPa～-0.1MPa.
(4) start heating system, furnace body temperature risen to 800 ℃～1050 ℃ of preset temperatures in 6-16 hour, and make precast body 8 thermally equivalents to be infiltrated through radiative transfer.
(5) feed reactant gases propylene C by interlayer inlet pipe outer 13 and interlayer inlet pipe internal layer 12 respectively
3H
6Or methane CH
4With inert protective gas or lower concentration reactant gases.The flow of reactant gases and shielding gas (or lower concentration reactant gases) is 1.0 ± 0.8m
3/ h can be according to the suitable relative discharge of adjusting two kinds of gases of the final requirement of product density.Described shielding gas or lower concentration reactant gases feed hollow cylinder precast body 8 endoporus to be infiltrated, and the back diffuses to precast body 8 outer walls to be infiltrated along the hole in the precast body 8 to be infiltrated; Reactant gases feeds sub-air chamber 11, after the pore on sub-air chamber's cover plate 10 with holes flows into the outer wall of hollow cylinder precast body 8 to be infiltrated, two kinds of gases are discharged out of the furnace by vacuum pumping hole 3 through the air outlet of precast body lamina tecti to be infiltrated 7 tops along predetermined passage directed flow.
When (6) reactant gases of high density is flowed through the outside surface of precast body 8 to be infiltrated, be diffused in the hole rapidly, and carry out the deposit carbon process in the outside of precast body 8 to be infiltrated.And the shielding gas of precast body to be infiltrated 8 inboards or light concentration gas be because diffusion, and externally the high density gas of surveying plays diluting effect, and the concentration gradient that makes precast body 8 to be infiltrated reactant gases radially occur distributes.
(7) densification rate of precast body 8 to be infiltrated is reduced towards inboard low-concentration area gradually by outside high density, and through 72-300 hour gas-phase carbon deposition, promptly can be made into external diameter density was 1.0～1.4g/cm
3, internal diameter density is 0.3～0.6g/cm
3The carbon/carbon composite of its density distribution gradient.
Claims (8)
1. device for preparing the carbon/carbon composite of its density distribution gradient, comprise the chemical vapor infiltration furnace body, bell and furnace bottom lid, described upper of furnace body is provided with vacuum pumping opening, be provided with insulation quilt and insulation cover plate in the described body of heater, be provided with graphite heater in the described insulation quilt, it is characterized in that, pass described body of heater, insulation quilt and graphite heater are provided with temperature thermocouple, described graphite heater inside part is equipped with the graphite gas cylinder, be provided with sub-air chamber's cover plate with holes of placing precast body to be infiltrated in the described graphite gas cylinder, being positioned at sub-air chamber cover plate with holes top in the graphite gas cylinder is permeate chamber, being positioned at sub-air chamber cover plate with holes bottom in the graphite gas cylinder is sub-air chamber, and described precast body to be infiltrated top is provided with lamina tecti; Pass described furnace bottom lid and be provided with the outer and interlayer inlet pipe internal layer of interlayer inlet pipe, described interlayer inlet pipe is outer to be communicated with described sub-air chamber, and described interlayer inlet pipe internal layer is higher than described sub-air chamber cover plate with holes and the upper end extends precast body endoporus to be infiltrated; Described interlayer inlet pipe skin is the reactant gases inlet pipe, and described interlayer inlet pipe internal layer is shielding gas or lower concentration reactant gases inlet pipe.
2. the device of the carbon/carbon composite of its density distribution gradient of preparation according to claim 1, the pore that it is characterized in that described sub-air chamber cover plate with holes is along described precast body outer rim uniform distribution to be infiltrated.
3. the device of the carbon/carbon composite of its density distribution gradient of preparation according to claim 1 is characterized in that described lamina tecti is conical, truncated cone-shaped or discoideus, and the spacing of itself and described graphite gas cylinder inwall is 5mm～10mm.
4. utilize the method for the carbon/carbon composite of its density distribution gradient of device preparation according to claim 1, it is characterized in that this method may further comprise the steps:
(1) according to the dimensioned chemical vapor infiltration graphite gas cylinder of precast body to be infiltrated;
(2) successively described graphite gas cylinder, hollow cylinder precast body to be infiltrated and lamina tecti are packed in the chemical vapor infiltration furnace body;
(3) according to predetermined temperature increasing schedule furnace body temperature is risen to 800 ℃～1050 ℃;
(4) under negative pressure, feed reactant gases and shielding gas or lower concentration reactant gases, precast body outer wall to be infiltrated is a reactant gases, its inwall is shielding gas or lower concentration reactant gases, control reactant gases and shielding gas or the two relative discharge of lower concentration reactant gases, the concentration gradient that makes precast body to be infiltrated radially set up reactant gases distributes;
(5) densification rate of precast body to be infiltrated is reduced towards inboard low-concentration area gradually by its outside high density, and through 72-300 hour gas-phase carbon deposition, promptly making its external diameter density was 1.0～1.4g/cm
3, internal diameter density is 0.3～0.6g/cm
3The carbon/carbon composite of its density distribution gradient.
5. the method for the carbon/carbon composite of its density distribution gradient of preparation according to claim 4 is characterized in that reactant gases is propylene C described in the step (4)
3H
6Or methane CH
4, described shielding gas is a rare gas element.
6. the method for the carbon/carbon composite of its density distribution gradient of preparation according to claim 4 is characterized in that: temperature increasing schedule described in the step (3) is furnace body temperature to be risen to 800 ℃～1050 ℃ in 6-16 hour.
7. the method for the carbon/carbon composite of its density distribution gradient of preparation according to claim 4, it is characterized in that: shielding gas or lower concentration reactant gases described in the step (4) feed hollow cylinder precast body endoporus to be infiltrated, and the back diffuses to precast body outer wall to be infiltrated along the hole in the precast body to be infiltrated; Reactant gases feeds sub-air chamber, after the pore on sub-air chamber's cover plate with holes flows into the outer wall of hollow cylinder precast body to be infiltrated, two kinds of gases flow out through the air outlet of precast body lamina tecti to be infiltrated top along predetermined passage directed flow.
8. the method for the carbon/carbon composite of its density distribution gradient of preparation according to claim 4 is characterized in that: reactant gases and shielding gas or lower concentration flow rate of reactive gas are 1.0 ± 0.8m described in the step (4)
3/ h.
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Application publication date: 20080709 Assignee: Institute of space power technology Assignor: Xi'an Aerospace Composite Materials Institute Contract record no.: 2013610000048 Denomination of invention: Device and method for preparing carbon/carbon composite material with gradient distribution density Granted publication date: 20101117 License type: Exclusive License Record date: 20130515 |
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