CN1803721A - Jointing method for carbon/carbon composite material - Google Patents

Jointing method for carbon/carbon composite material Download PDF

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Publication number
CN1803721A
CN1803721A CN 200610041656 CN200610041656A CN1803721A CN 1803721 A CN1803721 A CN 1803721A CN 200610041656 CN200610041656 CN 200610041656 CN 200610041656 A CN200610041656 A CN 200610041656A CN 1803721 A CN1803721 A CN 1803721A
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China
Prior art keywords
carbon
mass percent
compound material
room temperature
heating
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CN 200610041656
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Chinese (zh)
Inventor
李贺军
席琛
李克智
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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Priority to CN 200610041656 priority Critical patent/CN1803721A/en
Publication of CN1803721A publication Critical patent/CN1803721A/en
Pending legal-status Critical Current

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Abstract

The disclosed connection method for a C/C composite material comprises: 1) weighing tungsten phenolic resin, adding anhydrous alcohol, and preparing 59% anhydrous alcohol solution; adding hexamethylene tetramine as curative for full dissolution, then, adding tungsten powder to mix evenly; 2) cleaning and drying the C/C material; 3) coating evenly the resin from step 1) on composite material surface, drying, putting two surfaces to be connected face-to-face on steel mould, pressing, heating, and solidifying; 4) putting the connection piece from 3) into graphite mould then together with the mould into a high-temperature hot-compression furnace with graphite as heating member, leading argon gas, pressing, heating the furnace temperature from room temperature to 1500Deg, and holding; then, cooling to room temperature. The product has well physical properties.

Description

The method of attachment of carbon/carbon compound material
Technical field
The present invention relates to a kind of method of attachment of carbon/carbon compound material.
Background technology
Carbon/carbon compound material has many advantages than other matrix material, and its intensity is not along with the rising of temperature not only reduces, even can be higher, and this is that other structured material is incomparable; Its proportion is less than 2.0g/cm 3, only be 1/4 of nickel base superalloy, 1/2 of stupalith; Anti-ablation property is good, ablates evenly, can bear to be higher than 3000 ℃ high temperature, applies to often be used to make rocket nozzle, larynx lining etc. at space industry in the environment of short period of time ablation; Rub resistance polishing machine excellence, little, the stable performance of its frictional coefficient, be various wear-resisting and the friction parts the optimal candidate material.Because carbon/carbon compound material can not weld, one of method that connects them at present is to fix with the bolt that refractory metal or carbon/carbon compound material are made.But it is satisfactory that the intensity of the joint that makes in this way is difficult to, and this mainly is because the shearing resistance and the ultimate compression strength of this joint are relatively poor, the place of load concentration around bolt or tack hole particularly, and this situation is even more serious.
Document " stone National Day etc.; airplane carbon brake disc bonding recovery technique research; novel charcoal material; 2000; 15 (4), 62~64 " has reported that the usefulness organic binder bond is bonding, is connected the method for airplane carbon brake disc through overcuring, carbonization and carburizing treatment, the joint 10.9Mpa that this method makes, and only limit to the reparation of airplane carbon brake disc bonding; Document " Dadras.P et al; Joining ofCarbon-Carbon Composites by Graphite Formation; J.Am..Ceram.Soc.; 1994; 77 (6) 1419~1424 " has been introduced with the method that forms the graphitized mesophase layer and has been connected carbon/carbon compound material, this method be with magnesium, manganese and aluminium as the middle layer, these metals earlier and the carbon/carbon compound material reaction form metallic carbide, then at high temperature through the decomposition and the evaporation of metals formation graphitized mesophase layer of percarbide.The highest connection temperature of this experiment is 2200 ℃.But the experiment of doing the middle layer with magnesium and aluminium is not succeeded.Two breach slip resistances of joint of doing the middle layer with manganese are very low, when probe temperature is 1200 ℃ and 1400 ℃, have only 0.15 and 1.61MPa.
Clearly, art methods connects carbon/carbon compound material and exists strength of joint not high, the higher deficiency of required connection temperature requirement, and only limit to the reparation of airplane carbon brake disc bonding.
Summary of the invention
Low in order to overcome the prior art strength of joint, the higher deficiency of required connection temperature requirement the invention provides a kind of method of attachment of carbon/carbon compound material, can obviously improve the strength of joint of joint.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method of attachment of carbon/carbon compound material is characterized in that adopting following step:
1) takes by weighing the Q-913 tungsten resol of mass percent 10~15%, the dehydrated alcohol that adds mass percent 10~15%, make 50% ethanol solution, the hexamethylenetetramine that adds mass percent 1~2% is made solidifying agent, fully dissolving back adding mass percent 68~79% purity are 95%, granularity is 200 purpose tungsten powders, mixes;
2) carbon/carbon compound material that will connect uses ethanol, acetone ultrasonic cleaning clean respectively, dries;
3) the joint face of the carbon/carbon compound material that will connect evenly brushing with two joint faces relatively and place steel die, on press, apply the pressure of 5~10MPa through the resin of step 1) preparation after drying, be heating and curing 2 hours in 200 ℃;
4) web member after step 3) is solidified places graphite jig; put into graphite and make the high temperature hot pressing furnace of heating member; logical argon gas; apply the pressure of 5~10MPa; subsequently furnace temperature is risen to 1500 ℃ from room temperature, temperature rise rate is controlled at 10~15 ℃/min, is incubated 1~2 hour after furnace temperature reaches 1500 ℃; reduce to room temperature subsequently, whole process is led to argon shield.
The present invention's advantage compared to existing technology is: because good wettability and the adhesion property of resol, again through the joint microstructure densification of 200 ℃ of cure under pressures, so intensity is higher, and shearing resistance reaches as high as 35.8MPa.After 1500 ℃ of processing, because resol charing and volumetric shrinkage, crackle and defective appear in joint.But owing to can at 1400 ℃ chemical reaction take place with tungsten after the resol charing, exactly because generated resistant to elevated temperatures wolfram varbide in the joint original position, just make joint still can keep higher strength of joint after pyroprocessing, shearing resistance is the highest still can to reach 16.1MPa.
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment
Embodiment 1: the Q-913 tungsten resol that takes by weighing mass percent 15%, the dehydrated alcohol that adds mass percent 15%, make 50% ethanol solution, add mass percent 2% hexamethylenetetramine and make solidifying agent, fully dissolving back adding mass percent 68% purity is 95%, granularity is 200 purpose tungsten powders, mixes;
The carbon/carbon compound material that will connect uses ethanol, acetone ultrasonic cleaning clean respectively, dries.
Aforesaid resin is evenly brushed on the carbon/carbon compound material surface of handling, dried the back and connect, form similar " sandwich " structure of matrix material/resin/matrix material; Be placed in the steel die, on press, apply the pressure of 5MPa, be heating and curing 2 hours in 200 ℃.
Sample after solidifying is placed graphite jig; then mould is put into the high temperature hot pressing furnace that graphite is made heating member; logical argon gas; apply the pressure of 5MPa; subsequently furnace temperature is risen to 1500 ℃ from room temperature, temperature rise rate is controlled at 10 ℃/min, reaches after the predetermined top temperature insulation 1 hour; reduce to room temperature subsequently, whole process is led to argon shield.
Open mould after the blow-on, take out the carbon/carbon compound material that connects, can see that one deck articulamentum is arranged in the middle of two block of material.Scanning electron microscope, X-Ray diffraction analysis show: the densification of 200 ℃ of solidified joint microstructures, so intensity is higher, shearing resistance reaches as high as 35.8MPa.After 1500 ℃ of processing, because resol charing and volumetric shrinkage, crackle and defective appear in joint.But owing to can at 1400 ℃ chemical reaction take place with tungsten after the resol charing, exactly because generated resistant to elevated temperatures wolfram varbide in the joint original position, just make joint still can keep higher strength of joint after pyroprocessing, shearing resistance is the highest still can to reach 16.1MPa.
Subordinate list is the amount of adding tungsten powder and the mol ratio and the shearing resistance of joint after heat treatments at different of resin remaining carbon
The shearing resistance of joint after heat treatments at different
Carbon/tungsten (mol ratio) The shearing resistance of joint (MPa)
200℃ 1500℃
1∶0 1∶0.25 1∶0.5 1∶1 29.4 24.0 35.8 5.5 Ftracture 16.1 7.3 5.5
Embodiment 2: the Q-913 tungsten resol that takes by weighing mass percent 10%, the dehydrated alcohol that adds mass percent 10%, make 50% ethanol solution, add mass percent 1% hexamethylenetetramine and make solidifying agent, fully dissolving back adding mass percent 79% purity is 95%, granularity is 200 purpose tungsten powders, mixes;
The carbon/carbon compound material that will connect uses ethanol, acetone ultrasonic cleaning clean respectively, dries.
Aforesaid resin is evenly brushed on the carbon/carbon compound material surface of handling, dried the back and connect, form similar " sandwich " structure of matrix material/resin/matrix material; Be placed in the steel die, on press, apply the pressure of 10MPa, be heating and curing 2 hours in 200 ℃.
Sample after solidifying is placed graphite jig; then mould is put into the high temperature hot pressing furnace that graphite is made heating member; logical argon gas; apply the pressure of 10MPa; subsequently furnace temperature is risen to 1500 ℃ from room temperature, temperature rise rate is controlled at 15 ℃/min, reaches after the predetermined top temperature insulation 2 hours; reduce to room temperature subsequently, whole process is led to argon shield.

Claims (1)

1, a kind of method of attachment of carbon/carbon compound material is characterized in that adopting following step:
1) takes by weighing the Q-913 tungsten resol of mass percent 10~15%, the dehydrated alcohol that adds mass percent 10~15%, make 50% ethanol solution, the hexamethylenetetramine that adds mass percent 1~2% is made solidifying agent, fully dissolving back adding mass percent 68~79% purity are 95%, granularity is 200 purpose tungsten powders, mixes;
2) carbon/carbon compound material that will connect uses ethanol, acetone ultrasonic cleaning clean respectively, dries;
3) the joint face of the carbon/carbon compound material that will connect evenly brushing with two joint faces relatively and place steel die, on press, impose on the pressure of 5~10MPa through the resin of step 1) preparation after drying, be heating and curing 2 hours in 200 ℃;
4) place graphite jig through step 3) solidified web member; put into graphite and make the high temperature hot pressing furnace of heating member; logical argon gas; impose on the pressure of 5~10MPa; subsequently furnace temperature is risen to 1500 ℃ from room temperature, heat-up rate is controlled at 10~15 ℃/min, is incubated 1~2 hour after furnace temperature reaches 1500 ℃; reduce to room temperature subsequently, whole process is led to argon shield.
CN 200610041656 2006-01-12 2006-01-12 Jointing method for carbon/carbon composite material Pending CN1803721A (en)

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Application Number Priority Date Filing Date Title
CN 200610041656 CN1803721A (en) 2006-01-12 2006-01-12 Jointing method for carbon/carbon composite material

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CN 200610041656 CN1803721A (en) 2006-01-12 2006-01-12 Jointing method for carbon/carbon composite material

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CN1803721A true CN1803721A (en) 2006-07-19

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102908669A (en) * 2012-09-17 2013-02-06 西北工业大学 Preparation method of carbon foam/hydroxyapatite composite coating
CN106967372A (en) * 2016-01-14 2017-07-21 北京航空航天大学 For the modification connecting material of composite and connection method
CN110483086A (en) * 2019-08-28 2019-11-22 山东道普安制动材料有限公司 A kind of preparation method of carbon pottery brake disc
CN113912408A (en) * 2021-11-30 2022-01-11 甘肃新西北碳素科技有限公司 Rapid preparation method of airplane brake disc

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102908669A (en) * 2012-09-17 2013-02-06 西北工业大学 Preparation method of carbon foam/hydroxyapatite composite coating
CN102908669B (en) * 2012-09-17 2014-04-02 西北工业大学 Preparation method of carbon foam/hydroxyapatite composite coating
CN106967372A (en) * 2016-01-14 2017-07-21 北京航空航天大学 For the modification connecting material of composite and connection method
CN110483086A (en) * 2019-08-28 2019-11-22 山东道普安制动材料有限公司 A kind of preparation method of carbon pottery brake disc
CN113912408A (en) * 2021-11-30 2022-01-11 甘肃新西北碳素科技有限公司 Rapid preparation method of airplane brake disc

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