CN114656271A - Carbon-carbon crucible and preparation method thereof - Google Patents
Carbon-carbon crucible and preparation method thereof Download PDFInfo
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- CN114656271A CN114656271A CN202210412676.6A CN202210412676A CN114656271A CN 114656271 A CN114656271 A CN 114656271A CN 202210412676 A CN202210412676 A CN 202210412676A CN 114656271 A CN114656271 A CN 114656271A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C—CHEMISTRY; METALLURGY
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
Abstract
The application relates to the technical field of carbon-carbon crucibles, in particular to a carbon-carbon crucible and a preparation method thereof, wherein the method comprises the following steps: processing the recycled carbon fiber preform to obtain a prefabricated carbon fiber net tire and a prefabricated net tire felt layer; winding the first silk winding layer at a first angle and winding the second silk winding layer on the first silk winding layer at a second angle to obtain a target prefabricated shell; sequentially needling the carbon fiber net tire layer and the prefabricated carbon fiber net tire to a target preset shell to obtain a prefabricated body with a preset second thickness; pre-curing, carbonizing and densifying the prefabricated body to obtain a densified crucible; carrying out surface treatment, dipping and carbonization treatment on the densified crucible until the density reaches a second preset density to obtain a carbon-carbon crucible; this application will be prefabricated net child felt-layer and prick to the both sides of composite bed respectively, and this can carry out the attenuate to prefabricated net child felt-layer when using densification back carbon-carbon crucible surface hole to be blockked up, avoids extravagant carbon fiber raw and other materials, and then reduction in production cost.
Description
Technical Field
The application relates to the technical field of carbon-carbon crucibles, in particular to a carbon-carbon crucible and a preparation method thereof.
Background
For a long time, energy has been a hot problem in economic development of all countries. Since this century, the energy problems of various countries have been unprecedented in tension due to the rising prices of petroleum and natural gas. By means of energy strategy and policy of all countries around the world, many common points can be seen. Wherein, the energy strategy height is mentioned in the policy of applying energy conservation to actively developing and utilizing new energy and renewable energy for the first time and improving the utilization efficiency of energy.
In recent years, China sets up corresponding energy strategies according to the situation of the country, actively guides the development and utilization of new energy and renewable energy, and encourages the development of related industries. Particularly, the solar photovoltaic industry has achieved remarkable results. The rapid development of the photovoltaic industry in China also brings historical development opportunities to related production enterprises. The usage amount of the high-purity isobaric graphite crucible which is a key part of a thermal field of a single crystal furnace is increased year by year, the defects of the graphite crucible are increasingly exposed due to the gradual increase of the size of the thermal field, and the carbon/carbon crucible with higher comprehensive cost performance is started to enter the market to gradually replace the graphite crucible.
With the application of carbon fiber composite materials becoming more and more extensive, in the production process of the carbon fiber composite materials, particularly, the production of carbon fiber preform cutting scraps is more and more, the storage land occupation is larger, the treatment cost needs to be paid as solid waste, and the recycling of carbon fiber waste materials is one of the problems in the carbon/carbon composite material industry at present. The currently known carbon fiber composite material recovery processes are as follows: landfill, incineration and pulverization. Among them, the incineration method can recover part of the energy, but the incineration process needs to burn a large amount of energy and is not environment-friendly.
Accordingly, there is a need to provide an improved carbon-carbon crucible and a preparation scheme thereof to overcome the existing problems described above.
Disclosure of Invention
In order to solve the technical problem, the application provides a carbon-carbon crucible and a preparation method thereof, the application remanufactures a recycled carbon fiber preform into a prefabricated net felt layer with a preset first thickness, and two prefabricated net felt layers are respectively needled to two sides of a composite layer formed by composite carbon fiber cloth, a first filament winding layer, a second filament winding layer and a carbon fiber net tire, when pores on the surface of the densified carbon-carbon crucible are blocked, the prefabricated net felt layer with a certain thickness is removed, waste of raw carbon fiber materials is avoided, the production cost is further reduced, a complex manufacturing process is not needed, industrial production is facilitated, and the carbon-carbon crucible has a good market application prospect.
The application discloses a preparation method of a carbon-carbon crucible, which comprises the following steps:
s1: sequentially carrying out shredding treatment and net tire treatment on the recycled carbon fiber prefabricated body to obtain a prefabricated carbon fiber net tire;
s2: carrying out needling molding on the prefabricated carbon fiber net tire to obtain a first prefabricated net tire felt layer with a preset first thickness;
s3: placing the composite carbon cloth layer on the first prefabricated net felt layer, and performing needling molding to obtain a prefabricated shell with an arc-shaped transition part between the side wall and the bottom;
s4: winding an annular carbon wire layer on the side wall of the prefabricated shell, and winding a first winding wire layer on the annular carbon wire layer, the bottom of the composite carbon cloth layer and the arc transition part at a first angle; winding a second filament winding layer on the first filament winding layer at a second angle to obtain a target prefabricated shell;
s5: sequentially needling the carbon fiber net tire layer and the prefabricated carbon fiber net tire to the target preset shell to obtain a prefabricated body with a preset second thickness;
s6: sequentially carrying out pre-curing treatment, carbonization treatment and densification treatment on the prefabricated body to obtain a densified crucible with a first preset density;
s7: performing surface treatment, dipping and carbonization treatment on the densified crucible until the density of the densified crucible reaches a second preset density to obtain a carbon-carbon crucible; wherein, the surface treatment is to thin the inner and outer surfaces of the densified crucible.
Further, the step of S7 includes:
s71: thinning the inner surface and the outer surface of the densified crucible by a preset third thickness to realize surface treatment;
s72: dipping the densified crucible after surface treatment in an inert atmosphere environment to obtain a dipped densified crucible; wherein the pressure of the impregnation treatment is 1.2-1.8MPa, the impregnation time is 1.5-3h, and the impregnation resin is furfuryl ketone resin/phenolic resin;
s73: carbonizing the impregnated densified crucible to obtain a carbonized densified crucible;
s74: and detecting the density of the carbonized densified crucible, and if the density is less than the second preset density, repeating the steps S71-S73 until the density is more than or equal to the second preset density to obtain the carbon-carbon crucible.
Further, the carrier gas for the densification in the step 6 is an inert gas, the flow rate of the carrier gas is 13-23l/min, the deposition temperature is 800-1050 ℃, and the deposition time is 180-230 h.
Further, the first preset density is 1.1-1.2g/cm3The second preset density is 1.35g/cm3-1.5g/cm3。
Further, the first angle is 30-45 °; the second angle is-30 ° -45 °.
Further, the step of sequentially performing pre-curing treatment, carbonization treatment and densification treatment on the preform to obtain a densified crucible with a first preset density comprises:
sleeving the prefabricated body on a profiling tool, coating resin, standing for a period of time, demolding, and carbonizing to obtain a low-density crucible;
and carrying out densification treatment on the low-density crucible, and obtaining the densified crucible with the first preset density when the density reaches the first preset density.
Further, the resin comprises 9-10 parts by weight of phenolic resin, 1-1.5 parts by weight of alcohol and 1-2 parts by weight of curing agent.
Further, the resin comprises 3-4 parts by weight of epoxy colloid and 1 part by weight of curing agent;
sleeving the prefabricated body on a profiling tool, coating resin, standing for a period of time, demolding and carbonizing to obtain the low-density crucible, wherein the method comprises the following steps:
s61: after demolding treatment, detecting the deformation of the preform, and judging whether the deformation meets a preset deformation or not;
s62: if the deformation does not meet the preset deformation, placing the prefabricated body in a high-temperature environment with the temperature of more than 200 ℃ and removing the resin;
s63: performing orthopedic treatment on the prefabricated body after the resin is removed;
s64: sleeving the preform subjected to the shape correction treatment on the profiling tool, coating resin, standing for a period of time, demolding, and performing carbonization treatment to obtain the low-density crucible.
Further, the gram weight of the prefabricated net tire felt layer is 60-100g/m2The preset first thickness is 2-3mm, and the preset third thickness is 1-2 mm.
The invention also provides a carbon-carbon crucible which is prepared by the preparation method of the carbon-carbon crucible.
Based on the technical scheme, the method has the following beneficial effects:
this application makes the prefabricated net child felt layer of presetting first thickness with the carbon fiber preform who retrieves again, and with two prefabricated net child felt layers acupuncture to composite carbon fiber cloth respectively, first twine the silk layer, the both sides of the composite bed of the formation of second twine silk layer and carbon fiber net child, this can be when using densification back carbon crucible surface hole to be blockked up, get rid of the prefabricated net child felt layer of certain thickness, this has avoided extravagant carbon fiber raw and other materials, and then reduced manufacturing cost, and also need not complicated preparation technology, be favorable to the industrial production, make the carbon crucible of this application have good market perspective.
Drawings
In order to more clearly illustrate the technical solution of the present application, the drawings used in the description of the embodiment or the prior art will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the application, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1: the flow schematic diagram of the preparation method of the carbon-carbon crucible provided by the embodiment of the application;
FIG. 2: the structure diagram of carbon crucible that this application embodiment provided.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
For the following defined terms, these definitions shall be applied, unless a different definition is given in the claims or elsewhere in this specification. All numerical values are defined herein as modified by the term "about", whether or not explicitly indicated. The term "about" generally refers to a range of values that one of ordinary skill in the art would consider equivalent to the recited value to produce substantially the same property, function, result, etc. A numerical range indicated by a low value and a high value is defined to include all numbers subsumed within the numerical range and all subranges subsumed within the numerical range.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the application described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprising" and "having," as well as any variations thereof, are intended to cover non-exclusive inclusions.
The prior art has the following defects: with the application of carbon fiber composite materials becoming more and more extensive, in the production process of the carbon fiber composite materials, particularly, the production of carbon fiber preform cutting scraps is more and more, the storage land occupation is larger, the treatment cost needs to be paid as solid waste, and the recycling of carbon fiber waste materials is one of the problems in the carbon/carbon composite material industry at present. The currently known carbon fiber composite material recovery processes are as follows: landfill, incineration and pulverization. Among them, the incineration method can recover part of the energy, but the incineration process needs to burn a large amount of energy and is not environment-friendly.
To prior art's defect, the prefabricated net child felt layer of presetting first thickness is made again to the carbon fiber preform that this application will be retrieved, and with two prefabricated net child felt layers acupuncture respectively to compound carbon fiber cloth, first twine the layer, the both sides of the composite bed of the formation of second twine the layer and carbon fiber net child, this can be when using densification back carbon-carbon crucible surface hole to be blockked up, get rid of the prefabricated net child felt layer of certain thickness, this has avoided extravagant carbon fiber raw and other materials, and then reduced manufacturing cost, and also need not complicated preparation technology, be favorable to the industrial production, make the carbon-carbon crucible of this application have good market perspective.
The following describes a method for manufacturing a carbon-carbon crucible provided in an embodiment of the present application, please refer to fig. 1, where fig. 1 is a schematic flow chart of the manufacturing method. The specification provides the method steps as in the examples or flowcharts, but may include more or fewer steps based on conventional or non-inventive labor. The order of steps recited in the embodiments is merely one manner of performing the steps in a multitude of orders and does not represent the only order of execution. In the actual implementation of the preparation method, the method according to the embodiment or the drawings may be executed in sequence or in parallel. The method comprises the following steps:
s1: sequentially carrying out shredding treatment and net tire treatment on the recycled carbon fiber preform to obtain a prefabricated carbon fiber net tire;
s2: performing needling molding on the prefabricated carbon fiber net tire to obtain a first prefabricated net tire felt layer with a preset first thickness;
s3: placing the composite carbon cloth layer on the first prefabricated net felt layer, and performing needling molding to obtain a prefabricated shell with an arc-shaped transition part between the side wall and the bottom;
s4: winding the annular carbon wire layer on the side wall of the prefabricated shell, and winding the first wire winding layer on the annular carbon wire layer, the bottom of the composite carbon cloth layer and the arc transition part at a first angle; winding the second silk winding layer on the first silk winding layer at a second angle to obtain a target prefabricated shell;
s5: sequentially needling the carbon fiber net tire layer and the prefabricated carbon fiber net tire to a target preset shell to obtain a prefabricated body with a preset second thickness;
s6: sequentially carrying out pre-curing treatment, carbonization treatment and densification treatment on the prefabricated body to obtain a densified crucible with a first preset density;
s7: performing surface treatment, dipping and carbonization treatment on the densified crucible until the density of the densified crucible reaches a second preset density to obtain a carbon-carbon crucible; wherein, the surface treatment is to thin the inner and outer surfaces of the densified crucible.
It should be noted that: the prefabricated net child felt layer of presetting first thickness is made again to the carbon fiber preform who retrieves in this embodiment, and with two prefabricated net child felt layers acupuncture respectively to composite carbon fiber cloth, first twine the silk layer, the both sides of the composite bed of the formation of second twine silk layer and carbon fiber net child, this can be when using densification back carbon crucible surface hole to be blockked up, get rid of the prefabricated net child felt layer of certain thickness, this has avoided extravagant carbon fiber raw and other materials, and then reduced manufacturing cost, and also need not complicated preparation technology, be favorable to the industrial production, make the carbon crucible of this application have good market perspective.
It should also be noted that: the carbon fiber preform of retrieving is that carbon fiber fabric (carbon cloth) and net child are through spreading the layer design, through needle loom successive layer acupuncture shaping, this acupuncture process, because the product edge does not retrain, the repeated downstream of felting needle can make the carbon fiber at preform edge extend to the outside and slide to the border position can be because fibrous sliding, and some collapse appears the edge and is thin partially. Therefore, when the preform body is designed, a certain cutting allowance (the collapse position is cut off) is set, and the equal thickness of the edge and other places of the preform after cutting is ensured.
Specifically, the composite carbon cloth layer, the annular carbon filament layer, the first filament winding layer, the second filament winding layer and the carbon fiber net layer are needled by using a needle with a larger diameter of a needle handle, the needle is usually C333 type 14X 16X 36X 3, and interlayer combination can be better increased by using the needleThe strength and the needling density are controlled to be 30-35 needles/cm2The porosity is controlled between 60 and 70 percent.
Specifically, in step S5, the prefabricated carbon fiber mesh tire forms a second prefabricated mesh felt layer, and the thickness of the second prefabricated mesh felt layer is a preset first thickness.
Specifically, the density of the densified crucible with the first preset density is 1.1-1.2cm3The breaking strength is 105-110 MPa.
In this embodiment, the density of the preform of the preset second thickness is 0.45 to 0.5g/cm3。
In some possible embodiments, the step S7 includes:
s71: thinning the inner surface and the outer surface of the densified crucible by a preset third thickness to realize surface treatment;
s72: dipping the densified crucible after surface treatment in an inert atmosphere environment to obtain a dipped densified crucible; wherein the pressure of the impregnation treatment is 1.2-1.8MPa, the impregnation time is 1.5-3h, and the impregnation resin is furfuryl ketone resin/phenolic resin;
s73: carbonizing the impregnated densified crucible to obtain a carbonized densified crucible;
s74: and detecting the density of the carbonized densified crucible, and if the density is less than the second preset density, repeating the steps S71-S73 until the density is more than or equal to the second preset density to obtain the carbon-carbon crucible.
It should be noted that: for carbon/carbon composite materials, the higher bulk density means that more pores in the material are filled with matrix carbon, and the matrix carbon can bear certain stress action, which is beneficial to improving the mechanical strength of the carbon/carbon composite material. The market verifies that the density of the current carbon/carbon crucible finished product is more than 1.35g/cm3, and the carbon/carbon crucible finished product has longer service life. The general densification process is difficult to realize to reach the required density at one time, especially the chemical vapor deposition process; however, after a certain density is reached, because the pores on the surface of the carbon/carbon crucible are blocked, mechanical processing is needed to remove the 'skin', so that a certain processing allowance is needed to be provided for the inner diameter and the outer diameter of the densified crucible, and generally 4-5mm is reserved for a single side. Taking a 36-inch carbon/carbon crucible as an example, the wall thickness of a finished product is generally 15-20mm, and the machining allowance reaches more than 30% of the wall thickness of a blank, so that the waste of expensive carbon fiber raw materials is caused, and the production cost is increased; and this application uses the carbon fiber preform of retrieving, can reduce carbon fiber raw and other materials cost by more than 13%, and solved the recovery problem of enterprise's carbon fiber rim charge to a certain extent.
In some possible embodiments, the carrier gas for the densification process in the step S6 is an inert gas, the flow rate of the carrier gas is 13-23l/min, the deposition temperature is 800-.
Specifically, the pressure of the dipping treatment is 0.5-1.1MPa, and the temperature of the dipping treatment is 55-70 ℃.
In some possible embodiments, the curing process and the carbonizing process include:
controlling the temperature of the curing oven to be 60-120 ℃, and keeping for at least 4 h; wherein, the temperature is increased by 1 ℃ every 3-5 min;
controlling the temperature of the curing furnace at 120-; wherein, the temperature is increased by 1 ℃ every 5-8 min;
controlling the temperature of the curing oven to be 180 ℃, and preserving heat for 1h to finish curing.
After the solidification is finished, the mixture is transferred into a carbonization furnace for carbonization under normal pressure, and the temperature is programmed and raised according to the following temperature raising system:
controlling the temperature in the carbonization furnace to be-200 +/-10 ℃, and keeping for at least 3 h;
controlling the temperature in the carbonization furnace to be (200-;
controlling the temperature in the carbonization furnace to be (600-;
controlling the temperature in the carbonization furnace to be 850 +/-10 ℃, keeping the temperature for at least 1h continuously, cooling along with the furnace, and discharging below 300 ℃.
In some possible embodiments, the step of S7 is further followed by:
s8: and carrying out high-temperature purification treatment and machining treatment on the carbon-carbon crucible to obtain the finished carbon-carbon crucible.
Specifically, controlling the reaction device to vacuumize to more than 50Pa, closing a valve and a vacuum pump, and keeping the vacuum for 3 hours, wherein the pressure rise rate is less than 0.002MPa/3 hours;
controlling the temperature of the reaction device to 2000-2600 ℃; wherein, after the temperature reaches 1800 ℃, argon is filled for protection, and the furnace is continuously vacuumized, the pressure in the furnace is always kept about 3000pa until the heat preservation is finished for 5-6 days, and then the vacuumizing is stopped, and the temperature is freely reduced.
Specifically, the reaction device comprises at least one of a vacuum melting furnace, a vacuum sintering furnace, an ultrahigh temperature graphitization furnace and a carbonization furnace.
Specifically, the carbon-carbon crucible is purified at high temperature, which has little influence on density and mainly removes some metal and nonmetal impurities in the carbon-carbon crucible, for example, when the carbon-carbon crucible is used for matching a thermal field in the photovoltaic industry, the resistivity of a silicon single crystal at a client side is greatly influenced when the content of impurities such as aluminum, phosphorus, boron and the like is too high, and generally, the content of the metal impurities is required to be less than or equal to 300ppm by a client, so that the content of the metal impurities is reduced by high-temperature purification.
In some possible embodiments, the first predetermined density is 1.1-1.2g/cm3The second predetermined density is 1.35g/cm3-1.5g/cm3。
In some possible embodiments, the first angle is 30 ° -45 °; the second angle is-30 to-45.
It should be noted that: in the process of pulling the single crystal, the carbon-carbon crucible is a key core component and plays a role in high-temperature bearing, the carbon-carbon crucible bears the weight of raw materials such as the quartz crucible and the polycrystalline silicon, the raw materials are prevented from leaking out after the high-temperature quartz crucible is softened, and the carbon-carbon crucible bears the raw materials to rotate in the crystal pulling process, so that the requirement on the mechanical property of the crystal pulling furnace is high. In an emergency shutdown, the carbon-carbon crucible is subjected to a large stress for a short time due to the volume expansion of about 10% when the polysilicon cools, and in this case, the carbon-carbon crucible is generally cracked and discarded, and particularly, the stress is the greatest at the arc transition part.
Preferably, the strength at the arc-shaped transition part is increased by winding the first filament winding layer at 30 ℃ on the annular carbon filament layer and the arc-shaped transition part and the bottom of the composite carbon cloth layer, and winding the second filament winding layer at-30 ℃ on the first filament winding layer.
Preferably, the strength at the arc-shaped transition part is increased by winding the first filament winding layer at 45 ℃ on the annular carbon filament layer and the arc-shaped transition part and the bottom of the composite carbon cloth layer, and winding the second filament winding layer at-45 ℃ on the first filament winding layer.
In some possible embodiments, sequentially performing a pre-curing process, a carbonization process, and a densification process on the preform to obtain a densified crucible having a first predetermined density includes:
sleeving the prefabricated body on a profiling tool, coating resin, standing for 2-4h, demolding and carbonizing to obtain a low-density crucible;
and carrying out densification treatment on the low-density crucible, and obtaining a densified crucible with a first preset density when the density reaches a first preset density.
Specifically, the carbonization treatment includes:
before power transmission and temperature rise, vacuumizing to more than-0.094 MPa, closing a valve and a vacuum pump, keeping the vacuum for 1h, filling protective gas to normal pressure when the pressure rise rate is less than 0.002MPa/h, and opening a vent valve;
controlling the temperature of the carbonization furnace to be (220 +/-10) DEG C, and keeping for at least 1.5 h;
controlling the temperature of the carbonization furnace to be 230 +/-10 ℃ and keeping the temperature for 2 hours;
controlling the temperature of the carbonization furnace to be 220-650 ℃, and uniformly heating within 30 h;
controlling the temperature of the carbonization furnace to be 650-850 ℃, and uniformly heating within 15 h;
controlling the temperature of the carbonization furnace to be 850 +/-10 ℃ and keeping the temperature for 6 h;
and after the heat preservation is finished, controlling the carbonization furnace to cut off the power and freely cooling. Wherein, protective gas is continuously introduced for protection in the stages of temperature rise and temperature reduction.
Wherein, the temperature of the carbonization furnace is controlled to be (220 +/-10) DEG C, and the step of keeping the temperature for 2h is carried out, so as to prevent incomplete curing in the shaping process. The step-by-step uniform temperature rise can uniformly exhaust gas although the time is long, and the slow release of the thermal stress is ensured, so that the low-density crucible with small deformation is obtained.
Specifically, the protective gas is nitrogen or argon, and the purity of the nitrogen or argon is 99-99.999%.
In some possible embodiments, the resin includes 9-10 parts by weight of a phenolic resin, 1-1.5 parts by weight of an alcohol, and 1-2 parts by weight of a curing agent.
In some possible embodiments, the resin includes 3 to 4 parts by weight of the epoxy colloid and 1 part by weight of the curing agent;
sleeving the prefabricated body on a profiling tool, coating resin, standing for a period of time, demolding and carbonizing to obtain the low-density crucible, wherein the low-density crucible comprises the following steps:
s61: after demolding treatment, detecting the deformation of the prefabricated body, and judging whether the deformation meets the preset deformation;
s62: if the deformation does not meet the preset deformation, placing the prefabricated body in a high-temperature environment with the temperature of more than 200 ℃ and removing the resin;
s63: performing orthopedic treatment on the prefabricated body after the resin is removed;
s64: sleeving the reshaped prefabricated body on a profiling tool, coating resin, standing for a period of time, demolding, and carbonizing to obtain the low-density crucible.
It should be noted that: at present, the market takes an integral crucible as a mainstream, the straight wall end of the integral crucible is in a cylindrical shape, an R arc area exists at the bottom of the integral crucible, the integral crucible is easily influenced by a mould and a needling process after demoulding, the straight wall end can be deformed elliptically, the R arc shape is mainly repaired according to a contour guiding rule at present, experience difference of individual operation of staff exists, and a certain error is easily caused when the R arc shape is compared with a standard shape; therefore, after deformation is detected, the shape correction treatment is carried out, the deformation amount of the obtained low-density crucible can be ensured to be in a reasonable range, and the appearance attractiveness of the carbon-carbon crucible is improved to a certain extent.
In some possible embodiments, the epoxy colloid is epoxy E44 or epoxy E51, and the curing agent is an aliphatic amine or an aromatic amine.
In some possible embodiments, the pre-formed mat layer has a grammage of 60-100g/m2The first thickness is preset to be 2-3mm, and the third thickness is preset to be 1-2 mm.
As shown in FIG. 2, the invention also provides a carbon-carbon crucible, which is prepared by the preparation method of the carbon-carbon crucible.
The density of the carbon-carbon crucible in the application is more than or equal to 1.35g/cm3The breaking strength is 120-135 MPa.
It should be noted that: the carbon-carbon crucible prepared by the preparation method of the carbon-carbon crucible has the advantages of high strength, light weight, high density, small thermal expansion coefficient and good thermal shock resistance, and does not crack when used in an environment of rapid heating and rapid cooling, thereby prolonging the service life of the carbon-carbon crucible.
Example 1
S1: sequentially carrying out shredding treatment and net tire treatment on the recycled carbon fiber prefabricated body to obtain a prefabricated carbon fiber net tire;
s2: carrying out needling molding on the prefabricated carbon fiber net tire to obtain a first prefabricated net tire felt layer with a preset first thickness;
s3: placing the composite carbon cloth layer on the first prefabricated net felt layer, and performing needling molding to obtain a prefabricated shell with an arc-shaped transition part between the side wall and the bottom;
s4: winding the annular carbon wire layer on the side wall of the prefabricated shell, and winding the first wire winding layer on the annular carbon wire layer, the bottom of the composite carbon cloth layer and the arc transition part at a first angle; winding the second silk winding layer on the first silk winding layer at a second angle to obtain a target prefabricated shell;
s5: sequentially needling the carbon fiber net tire layer and the prefabricated carbon fiber net tire to a target preset shell to obtain a prefabricated body with a preset second thickness;
s6: sleeving the prefabricated body on a profiling tool, coating resin, standing for 2 hours, demolding and carbonizing to obtain a low-density crucible; carrying out densification treatment on the low-density crucible, and obtaining a densified crucible with a first preset density when the density reaches a first preset density;
s71: thinning the inner surface and the outer surface of the densified crucible by a preset third thickness to realize surface treatment;
s72: dipping the densified crucible after surface treatment in an inert atmosphere environment to obtain a dipped densified crucible; wherein the pressure of the impregnation treatment is 1.5MPa, the impregnation time is 1.5h, and the impregnation resin is furfuryl ketone resin/phenolic resin;
s73: carbonizing the impregnated densified crucible to obtain a carbonized densified crucible;
s74: detecting the density of the carbonized densified crucible, and if the density is less than the second preset density, repeating the steps S71-S73 until the density is more than or equal to the second preset density to obtain a carbon-carbon crucible;
s8: and carrying out high-temperature purification treatment and machining treatment on the carbon-carbon crucible to obtain the finished carbon-carbon crucible.
In the embodiment, the operations of surface treatment, impregnation and carbonization of the densified crucible are repeated for 1-2 times, and the density of the prepared carbon-carbon crucible is 1.30-1.32g/cm3, at which time the breaking strength of the carbon-carbon crucible is 120-124 MPa.
Example 2
S1: sequentially carrying out shredding treatment and net tire treatment on the recycled carbon fiber prefabricated body to obtain a prefabricated carbon fiber net tire;
s2: carrying out needling molding on the prefabricated carbon fiber net tire to obtain a first prefabricated net tire felt layer with a preset first thickness;
s3: placing the composite carbon cloth layer on the first prefabricated net felt layer, and performing needling molding to obtain a prefabricated shell with an arc-shaped transition part between the side wall and the bottom;
s4: winding the annular carbon wire layer on the side wall of the prefabricated shell, and winding the first wire winding layer on the annular carbon wire layer, the bottom of the composite carbon cloth layer and the arc transition part at a first angle; winding the second silk winding layer on the first silk winding layer at a second angle to obtain a target prefabricated shell;
s5: sequentially needling the carbon fiber net tire layer and the prefabricated carbon fiber net tire to a target preset shell to obtain a prefabricated body with a preset second thickness;
s6: sleeving the prefabricated body on a profiling tool, coating resin, standing for 3 hours, demolding and carbonizing to obtain a low-density crucible; carrying out densification treatment on the low-density crucible, and obtaining a densified crucible with a first preset density when the density reaches a first preset density;
s71: thinning the inner surface and the outer surface of the densified crucible by a preset third thickness to realize surface treatment;
s72: dipping the densified crucible after surface treatment in an inert atmosphere environment to obtain a dipped densified crucible; wherein the pressure of the impregnation treatment is 1.6MPa, the impregnation time is 2h, and the impregnation resin is furfuryl ketone resin/phenolic resin;
s73: carbonizing the impregnated densified crucible to obtain a carbonized densified crucible;
s74: detecting the density of the carbonized densified crucible, and if the density is less than the second preset density, repeating the steps S71-S73 until the density is more than or equal to the second preset density to obtain a carbon-carbon crucible;
s8: and carrying out high-temperature purification treatment and machining treatment on the carbon-carbon crucible to obtain the finished carbon-carbon crucible.
In the embodiment, the operations of surface treatment, impregnation and carbonization of the densified crucible are repeated for 1-2 times, and the density of the prepared carbon-carbon crucible is 1.32-1.34g/cm3, at which time the breaking strength of the carbon-carbon crucible is 124-128 MPa.
Example 3
S1: sequentially carrying out shredding treatment and net tire treatment on the recycled carbon fiber prefabricated body to obtain a prefabricated carbon fiber net tire;
s2: performing needling molding on the prefabricated carbon fiber net tire to obtain a first prefabricated net tire felt layer with a preset first thickness;
s3: placing the composite carbon cloth layer on the first prefabricated net felt layer, and performing needling molding to obtain a prefabricated shell with an arc-shaped transition part between the side wall and the bottom;
s4: winding the annular carbon wire layer on the side wall of the prefabricated shell, and winding the first wire winding layer on the annular carbon wire layer, the bottom of the composite carbon cloth layer and the arc transition part at a first angle; winding the second silk winding layer on the first silk winding layer at a second angle to obtain a target prefabricated shell;
s5: sequentially needling the carbon fiber net tire layer and the prefabricated carbon fiber net tire to a target preset shell to obtain a prefabricated body with a preset second thickness;
s6: sleeving the prefabricated body on a profiling tool, coating resin, standing for 3 hours, demolding and carbonizing to obtain a low-density crucible; carrying out densification treatment on the low-density crucible, and obtaining a densified crucible with a first preset density when the density reaches a first preset density;
s71: thinning the inner surface and the outer surface of the densified crucible by a preset third thickness to realize surface treatment;
s72: dipping the densified crucible after surface treatment in an inert atmosphere environment to obtain a dipped densified crucible; wherein the pressure of the impregnation treatment is 1.8MPa, the impregnation time is 3h, and the impregnation resin is furfuryl ketone resin/phenolic resin;
s73: carbonizing the impregnated densified crucible to obtain a carbonized densified crucible;
s74: detecting the density of the carbonized densified crucible, and if the density is less than the second preset density, repeating the steps S71-S73 until the density is more than or equal to the second preset density to obtain a carbon-carbon crucible;
s8: and carrying out high-temperature purification treatment and machining treatment on the carbon-carbon crucible to obtain the finished carbon-carbon crucible.
In this example, the surface treatment, impregnation and carbonization treatment of the densified crucible were repeated 3 times, and the density of the prepared carbon-carbon crucible was 1.35-1.5g/cm3, at which time the flexural strength of the carbon-carbon crucible was 128-135 MPa.
In conclusion, the application has the following beneficial effects:
(1) this application carries out the acupuncture shaping through using electronic acupuncture head, reduction in production cost to improve production efficiency, do benefit to industrial production, have higher market application scene.
(2) This application makes the prefabricated net child felt layer of two first thickness of predetermineeing again with the carbon fiber preform of retrieving, and with two prefabricated net child felt layers acupuncture to composite carbon fiber cloth respectively, first twine the silk layer, the both sides of the composite bed of the formation of second twine silk layer and carbon fiber net child, this can be when using densification back carbon crucible surface hole to be blockked up, get rid of the prefabricated net child felt layer of certain thickness, this has avoided extravagant carbon fiber raw and other materials, and then reduced manufacturing cost, and also need not complicated preparation technology, be favorable to the industrial production, make the carbon crucible of this application have good market perspective.
The foregoing description has disclosed fully embodiments of the present application. It should be noted that those skilled in the art can make modifications to the embodiments of the present application without departing from the scope of the claims of the present application. Accordingly, the scope of the claims of the present application is not to be limited to the particular embodiments described above.
Claims (10)
1. A method of making a carbon-carbon crucible, the method comprising:
s1: sequentially carrying out shredding treatment and net tire treatment on the recycled carbon fiber prefabricated body to obtain a prefabricated carbon fiber net tire;
s2: performing needling molding on the prefabricated carbon fiber net tire to obtain a first prefabricated net tire felt layer with a preset first thickness;
s3: placing the composite carbon cloth layer on the first prefabricated net felt layer, and performing needling molding to obtain a prefabricated shell with an arc-shaped transition part between the side wall and the bottom;
s4: winding an annular carbon wire layer on the side wall of the prefabricated shell, and winding a first winding wire layer on the annular carbon wire layer, the bottom of the composite carbon cloth layer and the arc transition part at a first angle; winding a second filament winding layer on the first filament winding layer at a second angle to obtain a target prefabricated shell;
s5: sequentially needling the carbon fiber net tire layer and the prefabricated carbon fiber net tire to the target preset shell to obtain a prefabricated body with a preset second thickness;
s6: sequentially carrying out pre-curing treatment, carbonization treatment and densification treatment on the prefabricated body to obtain a densified crucible with a first preset density;
s7: performing surface treatment, impregnation and carbonization treatment on the densified crucible until the density of the densified crucible reaches a second preset density to obtain a carbon-carbon crucible; wherein, the surface treatment is to thin the inner and outer surfaces of the densified crucible.
2. The method of manufacturing a carbon-carbon crucible as recited in claim 1, wherein said step of S7 comprises:
s71: thinning the inner surface and the outer surface of the densified crucible by a preset third thickness to realize surface treatment;
s72: dipping the densified crucible after surface treatment in an inert atmosphere environment to obtain a dipped densified crucible; wherein the pressure of the impregnation treatment is 1.2-1.8MPa, the impregnation time is 1.5-3h, and the impregnation resin is furfuryl ketone resin/phenolic resin;
s73: carbonizing the impregnated densified crucible to obtain a carbonized densified crucible;
s74: and detecting the density of the carbonized densified crucible, and if the density is less than the second preset density, repeating the steps S71-S73 until the density is more than or equal to the second preset density to obtain the carbon-carbon crucible.
3. The method as claimed in claim 2, wherein the carrier gas for densification in step S6 is an inert gas, the flow rate of the carrier gas is 13-23l/min, the deposition temperature is 800-1050 ℃, and the deposition time is 180-230 h.
4. The method of claim 1, wherein the first predetermined density is 1.1-1.2g/cm3The second preset density is 1.35g/cm3-1.5g/cm3。
5. The method of making a carbon-carbon crucible as recited in claim 1, wherein said first angle is between 30 ° and 45 °; the second angle is-30 ° -45 °.
6. The method for preparing a carbon-carbon crucible as recited in claim 1, wherein the sequentially performing the pre-curing treatment, the carbonizing treatment and the densifying treatment on the preform to obtain a densified crucible with a first predetermined density comprises:
sleeving the prefabricated body on a profiling tool, coating resin, standing for a period of time, demolding and carbonizing to obtain a low-density crucible;
and carrying out densification treatment on the low-density crucible, and obtaining the densified crucible with the first preset density when the density reaches the first preset density.
7. The method of manufacturing a carbon-carbon crucible as recited in claim 6, wherein the resin comprises 9 to 10 parts by weight of a phenol resin, 1 to 1.5 parts by weight of alcohol and 1 to 2 parts by weight of a curing agent.
8. The method of manufacturing a carbon-carbon crucible as recited in claim 6, wherein the resin comprises 3 to 4 parts by weight of epoxy colloid and 1 part by weight of curing agent;
sleeving the prefabricated body on a profiling tool, coating resin, standing for a period of time, demolding and carbonizing to obtain the low-density crucible, wherein the method comprises the following steps:
s61: after demolding treatment, detecting the deformation of the preform, and judging whether the deformation meets a preset deformation or not;
s62: if the deformation does not meet the preset deformation, placing the prefabricated body in a high-temperature environment with the temperature of more than 200 ℃ and removing the resin;
s63: performing orthopedic treatment on the prefabricated body after the resin is removed;
s64: sleeving the preform subjected to the shape correction treatment on the profiling tool, coating resin, standing for a period of time, demolding, and performing carbonization treatment to obtain the low-density crucible.
9. The method of claim 2, wherein the pre-formed batt layer has a grammage of 60 to 100g/m2The preset first thickness is 2-3mm, and the preset third thickness is 1-2 mm.
10. A carbon-carbon crucible, characterized by being produced by the method for producing a carbon-carbon crucible according to any one of claims 1 to 9.
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| CN116003151A (en) * | 2022-07-18 | 2023-04-25 | 浙江星辉新材料科技有限公司 | Carbon-carbon composite material crucible and preparation method thereof |
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