CN104193379B - Liquid phase pyrolysis deposition prepares device and the technique of carbon fiber reinforced carbon based composites - Google Patents
Liquid phase pyrolysis deposition prepares device and the technique of carbon fiber reinforced carbon based composites Download PDFInfo
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- CN104193379B CN104193379B CN201410375092.1A CN201410375092A CN104193379B CN 104193379 B CN104193379 B CN 104193379B CN 201410375092 A CN201410375092 A CN 201410375092A CN 104193379 B CN104193379 B CN 104193379B
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Abstract
The invention discloses the device that a kind of liquid phase pyrolysis deposition prepares carbon fiber reinforced carbon based composites, comprise integrated control system, cvd furnace, DC heating system, heating system, liquid-cooling equipment, gas cooler, filtering system, raw materials storage system.Integrated control system realizes intelligent control and remote control, by direct current and heating system, the workpiece be immersed in liquid precursor is heated in turn, reduce presoma temperature by cooling recirculation system and cool workpiece, make workpiece form controlled thermograde, realize the fast pyrogenation deposition of workpiece; Realized the recovery of volatilization liquid by condensing reflux system, improve raw material availability; By to filter and raw materials storage system realizes supplementing of presoma in the removal of impurity and working cycle.The present invention prepares that the based composite material of carbon efficiency such as charcoal/charcoal are high, cost is low, raw material availability is high, energy-saving and emission-reduction, can run at normal pressure, has burn-proof and explosion prevention, security is good, reliability is high feature.
Description
Technical field
The present invention relates to material processing plant and technology field, be related specifically to device and technique that a kind of fast performance liquid pyrolytic deposition prepares carbon fiber reinforced carbon based composites.
Background technology
Carbon/carbon composite is the warm structured material of a kind of novel super-high of current field of new primary study and exploitation, there is the advantages such as low density, high strength, Gao Bimo, low ablation rate, high-heat resistance shock resistant, low linear expansion coefficient (being only 1/5 ~ 1/10 of metal), high, the resistance to ablation of thermal conductivity, wear resisting property and anti-fatigue performance are good, particularly anti-fatigue performance matrix material intensity temperature 1000 DEG C ~ 2300 DEG C time raises and raises, and is desirable aerospace and the high-temperature material of other industrial circle.U.S.'s the nineties in last century has just carried out the research work that low cost is prepared fast, US National Aeronautics and Space Administration (NASA) is successful low cost is prepared fast charcoal/Carbon Materials its be applied to aeroplane brake discs and larynx lining etc.
The occurring first of carbon/carbon composite accidentally obtained in 1958 in Chance Vought airline laboratory, carbon/carbon composite technology is very slow what develop during the decade at first, to latter stage in the sixties, just start to develop into a member new in engineering materials, from the seventies, be greatly developed at US and European, be proposed the multidirectional knitting skill of Carbon fibe, high-pressure liquid phase impregnation technology and chemical gas phase pickling process (CVI), effectively obtain highdensity carbon/carbon composite, open wide prospect for it manufactures, produces in batches and applies.Since the eighties, the research of carbon/carbon composite is very active, and the state such as USSR (Union of Soviet Socialist Republics), Japan also all enters this advanced field, in raising performance, Rapid Densification Process of Preparing research and broadened application etc., to obtain remarkable progress.
Chemical vapour deposition technique (Chemical vapor deposition, be called for short CVD) be prepare the main technique that carbon/carbon composite Applicative time is long, technology maturity is high both at home and abroad at present, this technique is deposit carbon matrix in the base substrate with through gap or fibrage body skeleton, its technique is that fibrage body skeleton or base substrate are placed in chemical vapor deposition stove, pass into deposition reaction source gas, pyrolysis or react under depositing temperature, carbon/carbon composite needed for generation, be deposited in the hole of base substrate, and progressively fill up.The advantage of CVD technique is: the physical abuse that matrix material fiber in preparation process is subject to and chemical damage little; The goods of the multidirectional arrangement of fiber, braiding and complicated shape can be prepared; Can be used for preparing the adjustable gradient function matrix material of composition, this mature technology degree is high, is widely used at present.Common are the methods such as atmospheric pressure cvd, low pressure chemical vapor deposition, plasma CVD, hot CVD, clearance C VD and laser CVD at present.But CVD technology is Shortcomings also: the hole in base substrate easily blocks or forms closed pore in CVD process, even if raising pressure, reaction source gas also cannot enter, thus the matrix material obtaining high compactness is difficult to, often need to carry out the operations such as Multiple depositions, surface working, thermal treatment, its effective depositing time reaches more than 1000 hours, 3 ~ 4 months production cycles, production efficiency and material use efficiency low, production cost is high, at present mainly for the production of aerospace heat resistant structure part, be difficult to meet the actual demand that product for civilian use cost is low, demand is large.
CVI technique has compared with CVD that efficiency is high, speed is fast, density is high, intensity is high, toughness is high, critical strain values is high, can prepare the plurality of advantages such as large-size components.Conventional CVI technique is isothermal CVI, it has the advantage that simultaneously can deposit multiple or difform prefabricated component in same Reaktionsofen, but simple thin-wall part can only be deposited, often hole is occurred for thick thicker part inside, there is compactness difference, the problem that deposition of material is uneven, its process cycle is long especially simultaneously, and material preparation cost is higher.Although in order to reduce costs, shorten process cycle and Optimization Technology, having occurred impulse method, thermal gradient method, pressure reduction temperature gradient method etc. successively.In addition also have laser c VI (LCVI) method, forced-flow thermal gradient CVI method (FCVI), microwave CVI method (MWCVI) etc., but these techniques there is no industrialization to produce due to reasons such as equipment are complicated, processing requirement is high, production cost is high.
Chemical liquids vapor phase process (CLVD) significantly can shorten preparation cycle, but be subject to the limitation of its equipment and type of heating, there is precast body to be heated inequality, cause surface or core compactness extent uneven, and amplify production difficulty, still rest on laboratory stage, cannot apply in practice.
The data of carbon/carbon composite preparation technology and preparation facilities shows, the thermal source adopted for the preparation of such matrix material is single source, equipment is many by reaction vessel and heating unit, condensation exhaust system, feed system, temp measuring system and securing system composition, protect with nitrogen in preparation process, adopt single DC heating or induction heating mode, heating efficiency is low, be difficult to form desirable controlled temperature field and thermograde, most technique is only tested in laboratory scope, do not realize commercial scale production and application, and technology maturity and application more CVD explained hereafter cycle long, raw material availability is low, be difficult to obtain high-density carbon/carbon composite material, throughput is limited and goods price is high, be difficult to the goods promoting excellent property at civil area, the demand to energy-saving and emission-reduction in national economy fast development and world wide can not be met.
Summary of the invention
The object of the invention is to overcome that original method prepares that the carbon/carbon composite production cycle is long, production cost is high, raw material availability is low, consume energy the deficiency such as large, there is provided a kind of fast performance liquid pyrolytic deposition to prepare device and the technique of carbon/carbon composite, meet the national economy especially demand of civil area development to high-performance and low-cost charcoal/charcoal composite wood.Basic conception of the present invention is, designs the device that a kind of fast performance liquid pyrolytic deposition prepares carbon/carbon composite, and provides corresponding preparation technology.
Fast performance liquid pyrolytic deposition designed by the present invention prepares the device of carbon fiber reinforced carbon based composites, comprise integrated control system, cvd furnace, DC heating system, heating system, liquid-cooling equipment, gas cooler, filtering system, raw materials storage system, supporting pipeline, pump, valve etc. are stainless steel, be arranged on the direct supply input electrode in cvd furnace, ruhmkorff coil is copper material.
Described cvd furnace comprises tank body, induction heating device and DC heating device is provided with in tank body, induction heating device and DC heating device are connected with the DC heating system outside tank body, heating system respectively, be provided with pyrolytic deposition district in described tank body, induction heating device and DC heating device heat pyrolytic deposition district; The bottom of described tank body is connected with raw materials storage system by liquid filtering pump, filtering system; raw materials storage system is connected with gas cooler by condensing reflux pipe; gas cooler is also connected with tank body respectively by gas outlet channels, cooling for reflux pipe; described liquid-cooling equipment is bi-directionally connected by refrigeration cycle pipe and tank body, and described tank body is also provided with gas atmosphere inlet.Described condensing reflux pipe is provided with condensing reflux pump; described refrigeration cycle pipe is provided with liquid cooling recycle pump and liquid cooling control valve; described cooling for reflux pipe is provided with cooling for reflux valve; gas atmosphere inlet is provided with shielding gas valve, and described integrated control system is for controlling DC heating system, heating system, liquid filtering pump, condensing reflux pump, liquid cooling recycle pump, liquid cooling control valve, cooling for reflux valve, shielding gas valve.
As a further improvement on the present invention, described tank base is also provided with work holder.
Tank base is also provided with waste discharge mouth.
The tank body of described cvd furnace is the vertical circular furnace tank body of stainless steel, and this cvd furnace is also provided with at the bottom of packaged type top cover and tank, adopts Flange joint and keep sealing with tank body.Cvd furnace height overall 2.0-3.0 rice, tank body internal diameter 1.0-2.5 rice, cvd furnace is built with heating units such as direct current input electrode, ruhmkorff coils; Tank body is provided with liquidometer, and the work holder of bottom dress can move with tank base; Top cover is provided with porthole, tensimeter, pressure relief device, explosion-proof equipment and gas exhaust duct etc.
The cooling recirculation system of coordinative composition of equipments is the Integrated predict model of matured product, the liquid precursor volatilized during cooling system energy condensation heating outside stove; Stove internal cooling system can cool the presoma around workpiece and workpiece in tank body, jointly in workpiece, forms required temperature field and thermograde with heating unit, realizes the quick sedimentation process of workpiece.
Condensation cycle system of the present invention is part outside cvd furnace, the liquid precursor volatilized during energy condensation heating; The refrigerating unit of cvd furnace can form stably stratified flow in tank body, cools the presoma around workpiece and workpiece, jointly in workpiece, forms controlled temperature field and thermograde with heating unit, realizes the quick depositing operation in turn of workpiece.
Present invention also offers the technique that a kind of liquid phase pyrolysis deposition prepares carbon fiber reinforced carbon based composites, comprise the steps:
1) first to pre-treatment such as the coating of Carbon fibe prefabricated component protective layer material, oven dry etc., prefabricated component finished product is prepared into.
2) the prefabricated component finished product will prepared, puts into pyrolytic deposition district, injects liquid precursor from liquid raw material storage tank, closes cooling for reflux valve, liquid cooling control valve, makes whole tank body be in closed state,
3), after passing into shielding gas certain hour, open DC heating system by integrated control system, DC heating device acts on workpiece; The electric current in a DC induction source can be adjusted according to processing requirement at interval of certain hour, after DC heating system reaches certain power, open induction heating device by integrated control system; Needed for described induction heating, electric current is provided by induction heating power, the induction frequencies of this induction heating power can variable frequency adjustment, its band limits is 0.01K-80KHZ, and maximum rated power can be provided to be 800KW, and can realize any adjustment of heating power within the scope of this; Needed for described DC heating, electric current is provided by DC heating power supply, and the range of current that provides is 1.0-30000.0A, and can regulate arbitrarily within the scope of this.
4) liquid cooling control valve and liquid cooling recycle pump is opened in turn by integrated control system; When pressure reach both constant-pressure time, open cooling reverse flow valve and condensing reflux pump in turn, the gas that heating volatilization and cracking produce enters gas condenser by gas outlet channels, and cooled liquid enters tank body by cooling for reflux pipe, realizes the recycling of volatilization gas; Because the gas of volatilization and cracking forms stable air-flow, the inflow of air can be stoped, now can close 7 shielding gas valves;
5) open liquid filtering pump by integrated control device, make filtering system work, liquid towards presoma carries out filtration treatment.
Adjust galvanic current, induction frequencies and voltage etc. according to given process route respectively by 1 integrating control operator's console, can prepare density through 10 hours is 1.7g/cm3 carbon fiber reinforced carbon based composites.
Period can observe liquid precursor quantity in tank body by liquidometer; Workpiece heat situation is observed by porthole.Realized the recovery of volatilization liquid by gas condenser, improve raw material availability; In the remover working cycle being realized presoma impurity by filtering system and raw materials storage system, presoma supplements; Form controlled thermograde by DC heating system, heating system and cooling recirculation system in pyrolytic deposition district, realize the technological process that workpiece deposits gradually in turn from heart portion to periphery; Pressure relief opening is protector, can avoid producing excessive pressure in tank body.
Further, the technique that liquid phase pyrolysis deposition prepares carbon fiber reinforced carbon based composites also comprises:
6) liquid precursor is withdrawn into liquid raw material storage tank by liquid filtering pump after terminating by the workpiece deposition of batch; Not available waste material is finally discharged by waste discharge mouth, empties pot liquid, closes all valves, open main tank body upper cover and lower cover successively, takes out workpiece, then enters the operations such as later stage graphitization processing, machining after drying process.
The invention has the beneficial effects as follows, this device prepares that carbon/carbon composite efficiency is high, and cost is low, and raw material availability is high, energy-saving and emission-reduction, and can run at normal pressure, burn-proof and explosion prevention, and security is good, and reliability is high.This device and technique can make the preparation cycle of such matrix material within more than 1000 hours, shorten to 10 hours by effective depositing time of the CVD preparation technology extensively adopted at present, considerably reduce preparation cycle and the production cost of carbon/carbon composite, improve the production efficiency of goods and raw-material utilization ratio, there is wide market popularization value.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is preparation technology's schema of the present invention.
Wherein, 1 integrating control operator's console; 2 heating systems; 3 DC heating systems; 4 electric current input-output units; 5 liquidometers; 6 main tank bodies; 7 shielding gas valves; 8 tensimeters; 9 pressure relief openings; 10 gas outlet channels; 11 portholes; 12 cooling for reflux pipes; 13 cooling for reflux valves; 14 gas condensers; 15 liquid cooling control valves; 16 liquid cooling recycle pumps; 17 liquid-cooling equipment; 18 condensing reflux pumps; 19 condensing reflux pipes; 20 refrigeration cycle pipes; 21 liquid raw material storage tanks; 22 filtering systems; 23 tank supports; 24 liquid filtering pumps; 25 pyrolytic deposition districts; 26 waste discharge mouths; 27 induction and DC heating devices; 28 Workpiece clamping devices.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the invention will be further described.
As Figure 1-Figure 2, the present embodiment first to pre-treatment such as the coating of Carbon fibe prefabricated component protective layer material, oven dry etc., is prepared into prefabricated component finished product.By the prefabricated component finished product prepared, accurately locate bottom main tank body 6, and support fixing with workpiece clamping apparatus 28, at the bottom of tank and tank deck enters station and sealing is fixing, main tank body 6 is placed on tank support 23.Liquid precursor is injected to correct position by condensing reflux pipe 19 from liquid raw material storage tank 21, liquid precursor add-on is controlled by liquidometer 5, close cooling for reflux valve 13, liquid cooling control valve 15, whole tank body is made to be in closed state, then open shielding gas valve 7 and pass into shielding gas, after keeping certain hour, open DC heating system 3 by integrating control operator's console 1, electric current enters tank body by electric current input-output unit 4 and acts on workpiece; Adjust the electric current in a DC induction source at interval of certain hour according to processing requirement, after DC heating system 3 reaches certain power, induction heating device 2 is opened by integrating control operator's console 1, then by integrating control operator's console 1, open the liquid cooling control valve 15 on cooling circulation tube 20 and liquid cooling recycle pump 16 in turn, liquid-cooling equipment 17 works; Observe tensimeter 8, when pressure reach both constant-pressure time, open cooling reverse flow valve 13 and condensing reflux pump 18 in turn, the gas that heating volatilization and cracking produce enters gas condenser 14 by gas outlet channels 10, cooled liquid enters main tank body 6 by cooling for reflux pipe 12, realizes the recycling of volatilization gas; Because the gas of volatilization and cracking forms stable air-flow, the inflow of air can be stoped, now can close shielding gas valve 7; Then open liquid filtering pump 24 and filtering system 22 by integrating control operator's console 1, liquid towards presoma carries out filtration treatment.Adjust galvanic current, induction frequencies and voltage etc. according to given process route respectively by integrating control operator's console 1, can prepare density through 10 hours is 1.7g/cm
3carbon fiber reinforced carbon based composites.
Period observes liquid precursor quantity in tank body by liquidometer 5; Workpiece heat situation is observed by porthole 11.Realized the recovery of volatilization liquid by gas condenser 14, improve raw material availability; Supplementing of presoma in the removal of presoma impurity and working cycle is realized by storing and transporting systems such as filtering system 22 and liquid raw material tanks 21; Form controlled thermograde by induction and DC heating device 27 and cooling recirculation system in pyrolytic deposition district 25, realize the technological process that workpiece deposits gradually in turn from heart portion to periphery; Pressure relief opening 9 is protector, can avoid producing excessive pressure in tank body.Liquid precursor is withdrawn into liquid raw material storage tank 21 by liquid filtering pump 24 after depositing and terminating by the workpiece of batch; Not available waste material is finally discharged by waste discharge mouth 26, empties pot liquid, closes all valves, open main tank body 6 upper cover and lower cover successively, takes out workpiece, then enters the operations such as later stage graphitization processing, machining after drying process.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (10)
1. liquid phase pyrolysis deposition prepares the device of carbon fiber reinforced carbon based composites, it is characterized in that, comprise integrated control system, cvd furnace, DC heating system, heating system, liquid-cooling equipment, gas cooler, filtering system, raw materials storage system; Described cvd furnace comprises tank body, induction heating device and DC heating device is provided with in tank body, induction heating device and DC heating device are connected with the DC heating system outside tank body, heating system respectively, be provided with pyrolytic deposition district in described tank body, induction heating device and DC heating device heat pyrolytic deposition district; The bottom of described tank body is connected with raw materials storage system by liquid filtering pump, filtering system, raw materials storage system is connected with gas cooler by condensing reflux pipe, gas cooler is also connected with tank body respectively by gas outlet channels, cooling for reflux pipe, described liquid-cooling equipment is bi-directionally connected by refrigeration cycle pipe and tank body, and described tank body is also provided with gas atmosphere inlet; Described condensing reflux pipe is provided with condensing reflux pump; described refrigeration cycle pipe is provided with liquid cooling recycle pump and liquid cooling control valve; described cooling for reflux pipe is provided with cooling for reflux valve; gas atmosphere inlet is provided with shielding gas valve, and described integrated control system is for controlling DC heating system, heating system, liquid filtering pump, condensing reflux pump, liquid cooling recycle pump, liquid cooling control valve, cooling for reflux valve, shielding gas valve.
2. liquid phase pyrolysis deposition as claimed in claim 1 prepares the device of carbon fiber reinforced carbon based composites, and it is characterized in that, described tank base is also provided with work holder.
3. liquid phase pyrolysis deposition as claimed in claim 1 prepares the device of carbon fiber reinforced carbon based composites, and it is characterized in that, described tank base is also provided with waste discharge mouth.
4. liquid phase pyrolysis deposition as claimed in claim 1 prepares the device of carbon fiber reinforced carbon based composites, it is characterized in that, the tank body of described cvd furnace is the vertical circular furnace tank body of stainless steel, and this cvd furnace is also provided with at the bottom of packaged type top cover and tank, adopts Flange joint and keep sealing with tank body.
5. the liquid phase pyrolysis deposition as described in claim 1 or 3 prepares the device of carbon fiber reinforced carbon based composites, and it is characterized in that, described tank body is provided with liquidometer.
6. liquid phase pyrolysis deposition as claimed in claim 4 prepares the device of carbon fiber reinforced carbon based composites, and it is characterized in that, described top cover is provided with porthole.
7. liquid phase pyrolysis deposition as claimed in claim 4 prepares the device of carbon fiber reinforced carbon based composites, and it is characterized in that, described top cover is provided with tensimeter.
8. liquid phase pyrolysis deposition as claimed in claim 4 prepares the device of carbon fiber reinforced carbon based composites, and it is characterized in that, described top cover is provided with pressure relief device.
9. device as claimed in claim 1 prepares a technique for carbon fiber reinforced carbon based composites, it is characterized in that, comprises the steps:
1) first to Carbon fibe prefabricated component coating protective layer material, oven dry, prefabricated component finished product is prepared into;
2) the prefabricated component finished product will prepared, puts into pyrolytic deposition district, injects liquid precursor from raw materials storage system, closes cooling for reflux valve, liquid cooling control valve, makes whole tank body be in closed state,
3), after passing into shielding gas certain hour, open DC heating system by integrated control system, DC heating device acts on workpiece; After DC heating system reaches certain power, open induction heating device by integrated control system; The induction frequencies of described induction heating, its band limits is 0.01K-80KHZ, maximum rated power 800KW; Range of current needed for described DC heating is 1.0-30000A;
4) liquid cooling control valve and liquid cooling recycle pump is opened in turn by integrated control system; When pressure reach both constant-pressure time, open cooling reverse flow valve and condensing reflux pump in turn, the gas that heating volatilization and cracking produce enters gas condenser by gas outlet channels, and cooled liquid enters tank body by cooling for reflux pipe, realizes the recycling of volatilization gas;
5) open liquid filtering pump by integrated control device, make filtering system work, liquid towards presoma carries out filtration treatment.
10. prepare the technique of carbon fiber reinforced carbon based composites as claimed in claim 9, it is characterized in that, the technique that described liquid phase pyrolysis deposition prepares carbon fiber reinforced carbon based composites also comprises: 6) by liquid filtering pump, liquid precursor is withdrawn into raw materials storage system, the step that not available waste material is discharged by waste discharge mouth.
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| CN109234710A (en) * | 2018-11-09 | 2019-01-18 | 西安宸瑞电工科技发展有限公司 | A kind of new chemical liquid deposition furnace |
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| CN1736947A (en) * | 2005-07-18 | 2006-02-22 | 西安交通大学 | Method for preparing carbon/carbon composite material |
| CN101157565A (en) * | 2007-09-13 | 2008-04-09 | 北京航空航天大学 | Novel process for preparing charcoal/charcoal component by rapid chemical liquid-phase vaporization osmosis method |
| CN201154987Y (en) * | 2007-09-13 | 2008-11-26 | 北京航空航天大学 | Novel liquid phase vaporization densification device for preparing C/C component |
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| JP5662078B2 (en) * | 2010-08-04 | 2015-01-28 | イビデン株式会社 | C / C composite material molded body and method for producing the same |
| CN203999390U (en) * | 2014-07-31 | 2014-12-10 | 山东大学 | Liquid phase pyrolytic deposition is prepared the device of carbon fiber reinforced carbon based composites |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1736947A (en) * | 2005-07-18 | 2006-02-22 | 西安交通大学 | Method for preparing carbon/carbon composite material |
| CN101157565A (en) * | 2007-09-13 | 2008-04-09 | 北京航空航天大学 | Novel process for preparing charcoal/charcoal component by rapid chemical liquid-phase vaporization osmosis method |
| CN201154987Y (en) * | 2007-09-13 | 2008-11-26 | 北京航空航天大学 | Novel liquid phase vaporization densification device for preparing C/C component |
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