CN111570192A - High-pressure impregnation pressurization carbonization process and equipment for carbon fiber preform - Google Patents

High-pressure impregnation pressurization carbonization process and equipment for carbon fiber preform Download PDF

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Publication number
CN111570192A
CN111570192A CN202010547410.3A CN202010547410A CN111570192A CN 111570192 A CN111570192 A CN 111570192A CN 202010547410 A CN202010547410 A CN 202010547410A CN 111570192 A CN111570192 A CN 111570192A
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pressure
carbon fiber
fiber preform
impregnation
carbonization
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Chinese (zh)
Inventor
王金铎
杨海春
邵河
李童
郭宾
陶国新
啜艳明
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Hebei Shuntian Electrode Co ltd
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Hebei Shuntian Electrode Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C3/00—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material
    • B05C3/02—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material
    • B05C3/09—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating separate articles
    • B05C3/109—Passing liquids or other fluent materials into or through chambers containing stationary articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
    • B05D3/0486—Operating the coating or treatment in a controlled atmosphere
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10—Crucibles or containers for supporting the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
    • D06C7/00—Heating or cooling textile fabrics
    • D06C7/04—Carbonising or oxidising

Abstract

The invention relates to a high-pressure impregnation pressure carbonization process and equipment for a carbon fiber preform, wherein the equipment comprises an outer liner and an inner liner, a cavity is formed between the inner liner and the outer liner, the carbon fiber preform is placed in the cavity, the pressure and the temperature in the cavity are controlled by the pressure and the temperature, and the integrated high-pressure impregnation and pressure carbonization are completedThe production process can be completed. The product cycle is less than 45 days, and the product density is more than 1.50g/cm3The provided equipment is designed integrally, is scientific and reasonable, and greatly reduces energy consumption.

Description

High-pressure impregnation pressurization carbonization process and equipment for carbon fiber preform
Technical Field
The invention relates to the field of carbon material preparation, in particular to a high-pressure impregnation pressurization carbonization process and equipment for a carbon fiber preform.
Background
The carbon/carbon crucible is a necessary consumable material for pulling monocrystalline silicon in the photovoltaic industry, and the method for manufacturing the carbon/carbon crucible at present in China is to densify the carbon fiber preform by vapor deposition to the density of 1.0g/cm3Then soaking in soaking equipment, transferring to other equipment for carbonization and densification, repeatedly soaking and carbonizing for 4-5 times to make product density reach 1.5g/cm3Above, the whole production cycle needs 90 days, the production procedures are more and less efficient, the energy loss is more, and the automation degree is lower.
In order to solve the problems, CN104446588A in the prior art discloses a liquid-phase impregnation densification method for a carbon fiber preform, which comprises an impregnation step, a low-temperature treatment step and a high-temperature carbonization step, wherein the carbon fiber preform is used as a reinforcement, high-temperature modified asphalt is used as a matrix impregnant, a pressurized impregnation device is used for carrying out liquid-phase impregnation densification treatment on a C/C material, and the density of the C/C material reaches 1.5 g-cm by adopting the conventional liquid-phase impregnation method-3The above requires 8 to 10 cycles of densification.
Although the above technical solutions shorten the number of cycles, they cannot solve the problem that a single cycle is long and a complex process of switching devices is required, so that a new process method needs to be invented to meet the requirements of shortening the production cycle and improving efficiency without affecting the product quality.
Disclosure of Invention
The invention aims to solve the problems in the prior art, provides a high-pressure impregnation and pressurization carbonization process for a carbon fiber preform, and also provides equipment for implementing the process.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a high-pressure impregnation pressurization carbonization device for a carbon fiber preform, which comprises an outer liner and an inner liner which are matched with each other, wherein the upper ends of the outer liner and the inner liner are provided with openings, and a sealing cavity for placing the carbon fiber preform is formed between the outer liner and the inner liner; a shell is arranged on the outer side of the outer container, a heat insulation material is arranged in the shell, and an electric heating pipe is arranged between the outer side of the outer container and the heat insulation material; the upper end of the inner container is provided with an upper cover, the inner side of the upper cover is provided with a heat insulation material, and the inner side of the inner container is provided with an electric heating pipe; the sealing cavity is connected with a pressure regulating chamber through a vent pipeline, and the pressure regulating chamber is provided with an automatic pressure relief control valve, an automatic pressure increasing control valve and a pressure gauge; the sealed cavity is connected with the steeping liquor pool through a liquor inlet pipeline, and a high-pressure pump and an electric valve are arranged on the liquor inlet pipeline.
As a further improvement of the invention, temperature sensors are arranged between the outer side of the outer liner and the heat insulation material and on the inner side of the inner liner.
As a further improvement of the invention, the shell and the upper cover are both provided with temperature control instruments which are respectively and electrically connected with temperature sensors arranged between the outer side of the outer liner and the heat insulation material and the inner side of the inner liner.
As a further improvement of the invention, the upper ends of the outer liner and the inner liner are both provided with annular outer edges, the outer edges of the outer liner and the inner liner are provided with corresponding threaded holes, and the outer liner and the inner liner are connected together through connecting bolts.
As a further improvement of the invention, a sealing ring is arranged between the outer edge of the outer liner and the outer edge of the inner liner.
As a further improvement of the invention, the sealing ring is made of high-temperature-resistant aluminum silicate fiber felt.
As a further improvement of the invention, the top of the sealed cavity is provided with a vent connected with the vent pipeline, and the bottom of the sealed cavity is provided with an immersion liquid inlet connected with the liquid inlet pipeline.
As a further improvement of the invention, the clearance at any place of the sealed cavity is 2-3mm larger than the thickness of the carbon fiber preform.
As a further improvement of the invention, the heat-insulating material adopts rock wool.
The invention also provides a process for carrying out high-pressure impregnation pressure carbonization on the carbon fiber preform by using the equipment, which comprises the following steps:
(1) weaving the prefabricated body: adopting T700 protofilament to produce carbon cloth and net tyre, calculating dosage according to size density, cross-layer knitting, 30 needles/cm2Obtaining a carbon fiber preform;
(2) preparing an impregnation liquid: adding 0.5-1.0 wt% of one-dimensional or two-dimensional nano carbon material into coal tar pitch, and heating and mixing uniformly for later use;
(3) high-pressure impregnation: the impregnation liquid prepared in the step (2) has the density of the carbon fiber preform from 0.45g/cm according to the step (1)3Increase to 1.5g/cm3Adding the calculated amount of the carbon fiber preform, immersing the carbon fiber preform, and keeping the temperature of 140-160 ℃ for 1-2 hours under the condition of 5-8 MPa;
(4) pressure carbonization: after the treatment in the step (3) is completed, reducing the pressure to 2-4 MPa, and carrying out temperature programming to 850 +/-10 ℃ for carbonization for 3-4 h, wherein the temperature programming curve is as follows: heating to 230 ℃ for 3 h; 230 ℃ for 2 h; 230 to 650 ℃ for 18 h; 650 to 850 ℃ for 9 h; 850 ℃ for 4 h;
(5) discharging the product out of the furnace: cooling to room temperature, reducing the pressure to atmospheric pressure, and taking out the carbon fiber preform to obtain the carbon fiber preform.
As some embodiments of the invention, the coal tar pitch in the step (2) has a softening point of 90-100 ℃ and a coking value of more than 45%.
As some embodiments of the invention, the mixing temperature in the step (2) is 150-180 ℃, and ultrasonic mixing and stirring are adopted.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
the method provided by the invention does not need to adopt vapor deposition for densification, and can complete the production process by optimizing the impregnation liquid, carrying out one-step high-pressure impregnation and carrying out two-step pressure carbonization. The product cycle is less than 10 daysThe product density is more than 1.5g/cm3。
According to the carbon fiber preform high-pressure impregnation pressurization carbonization all-in-one machine, vapor deposition densification is not needed, the high-pressure impregnation and pressurization carbonization processes can be completed on one device, automatic control and safe production are achieved through the pressure gauge and the temperature control instrument, rapid densification and carbonization are achieved, production procedures are reduced, energy consumption is reduced, production efficiency is improved, the internal structure of a product can be guaranteed to be uniform, and the service life of the product is prolonged.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural view of the present invention.
Wherein: the device comprises an outer container 1, a steeping liquid inlet 1-1, an inner container 2, an air vent 2-1, a sealing cavity 3, a carbon fiber preform 4, a shell 5, an upper cover 6, a heat insulation material 7, an electric heating pipe 8, an air vent pipeline 9, a pressure adjusting chamber 10, an automatic pressure relief control valve 11, an automatic pressure increasing control valve 12, a pressure gauge 13, a liquid inlet pipeline 14, a steeping liquid pool 15, a high-pressure pump 16, an electric valve 17, a temperature control instrument 18, a connecting bolt 19, a sealing ring 20 and a power supply lead 21.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail and fully with reference to the following embodiments.
Example 1
The utility model provides a carbon fiber preform high pressure impregnation pressurization carbonization equipment, as shown in figure 1, it includes outer courage 1 and the inner bag 2 of the metal material of mutually supporting, outer courage 1 and inner bag 2 are cylinder and upper end opening, form the sealed chamber 3 that is used for placing carbon fiber preform 4 between the two, the clearance in sealed chamber 3 any place is than here carbon fiber preform 4's thickness is 2-3mm big, guarantees carbon fiber preform 4 does not take place too big deformation, plays the effect of fixed shape.
A shell 5 made of metal is arranged on the outer side of the outer container 1, a heat insulation material 7 is arranged in the shell 5, and an electric heating pipe 8 is arranged between the outer side of the outer container 1 and the heat insulation material 7; an upper cover 6 made of metal is arranged at the upper end of the inner container 2, a heat insulation material 7 is arranged on the inner side of the upper cover 6, and an electric heating pipe 8 is arranged on the inner side of the inner container 2. The heat insulation material 7 is rock wool. Temperature sensors are arranged between the outer side of the outer container 1 and the heat insulation material 7 and on the inner side of the inner container 2. All be equipped with temperature control instrument 18 on shell 1 and the upper cover 6, temperature control instrument 18 respectively with locate between outer courage 1 outside and the insulation material 7 and the inboard temperature sensor electric connection of inner bag 1. The sealed cavity 3 is connected with a pressure regulating chamber 10 through a vent pipeline 9, the pressure regulating chamber 10 is a cavity made of forged steel materials and is connected with an air pump, an automatic pressure relief control valve 11, an automatic pressure increasing control valve 12 and a pressure gauge 13 are arranged on the pressure regulating chamber 10, and a pressure transmitter and a safety valve can be further arranged. The electric heating pipes 8 are uniformly arranged along the outer side of the outer container 1 and the inner side of the inner container 2 in the circumferential direction, radiate heat energy to the outer container 1 and the inner container 2, and then transmit the heat energy to the carbon fiber prefabricated body 4 in the sealing cavity 3 in a heat conduction mode to heat. The temperature in the sealed cavity 3 is regulated and controlled by the temperature sensor and the temperature control instrument 18, so that the temperature required by the process is guaranteed to be maintained. The pressure in the sealed cavity 3 is regulated and controlled through the pressure regulating chamber 10 and the pressure gauge 12, and the pressure required by the process is guaranteed to be maintained.
The sealed cavity 3 is connected with an immersion liquid pool 15 through a liquid inlet pipeline 14, and a high-pressure pump 16 and an electric valve 17 are arranged on the liquid inlet pipeline 14. The impregnation liquid tank 15 contains the impregnation liquid with a measured volume, the impregnation liquid is just the amount of the carbon fiber preform 4 which is completely immersed, the impregnation liquid is pumped into the sealing cavity 3 through the high-pressure pump 16, and then the electric valve 17 is closed.
The upper ends of the outer liner 1 and the inner liner 2 are both provided with annular outer edges, the outer edges of the outer liner 1 and the inner liner 2 are provided with corresponding threaded holes, and the outer liner 1 and the inner liner 2 are connected together through connecting bolts 19. And a sealing ring 20 is arranged between the outer edge of the outer liner 1 and the outer edge of the inner liner 2 for sealing to prevent air leakage and liquid leakage. The sealing ring 20 is made of high-temperature-resistant aluminum silicate fiber felt.
The top of the sealed cavity 3 is provided with a vent hole 2-1 connected with the vent pipeline 9, and the vent hole 2-1 is arranged on the outer edge of the inner container 2; the bottom of the sealed cavity 3 is provided with an immersion liquid inlet 1-1 connected with the liquid inlet pipeline 14, and the immersion liquid inlet 1-1 is arranged at the bottom of the outer container 1.
The working process of the device is as follows:
weaving the prefabricated body: adopting T700 carbon fiber to produce carbon cloth and net body, calculating the use amount of the carbon cloth and the net body according to the size and the density, and calculating the use amount of the carbon cloth and the net body according to the needle/cm2And (5) interweaving layers to weave to obtain the carbon fiber preform.
Preparing an impregnation liquid: adding 0.5-1.0 wt% of one-dimensional nano carbon material or two-dimensional nano carbon material into coal tar pitch with the softening point of 95 ℃ and the coking value of more than 45%, and ultrasonically mixing uniformly at 150-180 ℃, wherein the ultrahigh sound wave frequency is 30 Khz. The mixture is injected into the impregnation liquid pool 15 after being mixed evenly.
Charging a product: cleaning the outer container 1, placing the prepared carbon fiber preform 4 on the inner side of the outer container 1, inserting the inner container 2 into the outer container 1, fixing the outer edges of the outer container 1 and the inner container 2 through the connecting bolt 19 to form a sealing cavity 3 filled with the carbon fiber preform 4, and finishing furnace charging of a product to be processed.
Pumping the impregnation liquid: starting the high-pressure pump 16, and enabling the impregnation liquid with the carbon residue rate of 45% to be 0.45g/cm from the carbon fiber preform 43Increase to 1.5g/cm3The calculated amount is added to the sealed chamber 3, and then the electric valve 17 is automatically closed and the high pressure pump 16 is automatically stopped.
High-pressure impregnation: starting automatic heating, introducing electric energy into the electric heating pipe 8 through a power supply lead 21, starting heating to 140-160 ℃, completing temperature monitoring through a temperature control instrument 18, wherein the heat preservation time is 1-2 hours, realizing that the impregnation liquid is fully and uniformly distributed in the sealed cavity 3, and realizing automatic heating, heat preservation and cooling. In the heating process, gas is generated due to volatilization of the impregnation liquid, so that the pressure of the closed space is increased, the automatic pressure relief control valve 11 is automatically started through detection of the pressure gauge 13 and control of the PLC control system, and the pressure is controlled within the range of 5-8 MPa of the process requirement.
Pressure carbonization: after the high-pressure impregnation process is finished, continuously keeping the temperature for 4 hours at 850 ℃ according to the carbonization process curve requirement in the embodiment 1, automatically heating, keeping the temperature and cooling, wherein the pressure of a closed space is increased due to gas generated by volatilization in the process, automatically starting the automatic pressure relief control valve 11 through the detection of the pressure gauge 13 and the control of the PLC control system, and controlling the pressure within the range of 2-4 MPa of the process requirement until the carbonization process is finished.
Discharging the product out of the furnace: the pressure is reduced to zero through the automatic pressure relief control valve 11, so that the air pressure in the sealed cavity 3 is the same as the external atmospheric pressure, the connecting bolt 19 is unscrewed, the inner container 2 and the carbon fiber preform 4 are taken out, and the product is discharged.
Example 2
The process for the high-pressure impregnation pressure carbonization of carbon fiber preforms using the apparatus as described in example 1 comprises the following steps and parameters:
(1) weaving the prefabricated body: adopting T700 protofilament to produce carbon cloth and net body, calculating the carbon cloth and net body dosage according to size density, according to 30 needles/cm2And (5) interweaving layers to weave to obtain the carbon fiber preform.
(2) Preparing an impregnation liquid: adding 0.8wt% of one-dimensional nano carbon material into coal tar pitch with the softening point of 95 ℃ and the coking value of more than 45%, and ultrasonically mixing uniformly at 165 ℃ with the ultrahigh sound wave frequency of 30 Khz.
(3) High-pressure impregnation: the impregnation liquid prepared in the step (2) is used for preparing the carbon fiber preform from 0.45g/cm according to the step (1)3Increase to 1.5g/cm3Adding the calculated amount of the carbon fiber preform, immersing the carbon fiber preform, keeping the temperature at 150 ℃ for 1.5h under the condition of 6.5MPa, and cooling to room temperature;
(4) pressure carbonization: after the treatment in the step (3) is finished, reducing the pressure to 2.0MPa, and carrying out temperature programming to 850 ℃ for carbonization for 4h, wherein the temperature programming curve is as follows: heating to 230 ℃ for 3 h; 230 ℃ for 2 h; 230 to 650 ℃ for 18 h; 650 to 850 ℃ for 9 h; 850 ℃ and 4 h.
(5) Discharging the product out of the furnace: cooling to room temperature, reducing the pressure to atmospheric pressure, and taking out the carbon fiber preform to obtain the carbon fiber preform.
Example 3
The process for the high-pressure impregnation pressure carbonization of carbon fiber preforms using the apparatus as described in example 1 comprises the following steps and parameters:
(1) weaving the prefabricated body: adopting T700 protofilament to produce carbon cloth and net body, calculating the consumption of the carbon cloth and the net body according to the size density, and calculating the consumption of the carbon cloth and the net body according to 30 needles/cm2And (5) interweaving layers to weave to obtain the carbon fiber preform.
(2) Preparing an impregnation liquid: adding 1.0wt% of two-dimensional nano carbon material into coal tar pitch with the softening point of 95 ℃ and the coking value of more than 45%, and ultrasonically mixing uniformly at 165 ℃ with the ultrahigh sound wave frequency of 25 Khz.
(3) High-pressure impregnation: the impregnation liquid prepared in the step (2) is used for preparing the carbon fiber preform from 0.45g/cm according to the step (1)3Increase to 1.5g/cm3Adding the calculated amount of the carbon fiber preform, immersing the carbon fiber preform, keeping the temperature at 160 ℃ for 1h under the condition of 5.0MPa, and cooling to room temperature;
(4) pressure carbonization: after the treatment in the step (3) is finished, reducing the pressure to 3.5MPa, and carrying out temperature programming to 850 ℃ for carbonization for 4h, wherein the temperature programming curve is as follows: the temperature programming curve is as follows: heating to 230 ℃ for 3 h; 230 ℃ for 2 h; 230 to 650 ℃ for 18 h; 650 to 850 ℃ for 9 h; 850 ℃ and 4 h.
(5) Discharging the product out of the furnace: cooling to room temperature, reducing the pressure to atmospheric pressure, and taking out the carbon fiber preform to obtain the carbon fiber preform.
Example 4
A high-pressure impregnation pressure carbonization process of a carbon fiber preform is produced according to the equipment of the embodiment 2, and the specific parameters are as follows:
(1) weaving the prefabricated body: adopting T700 protofilament to produce carbon cloth and net body, calculating the consumption of the carbon cloth and the net body according to the size density, and calculating the consumption of the carbon cloth and the net body according to 30 needles/cm2And (5) interweaving layers to weave to obtain the carbon fiber preform.
(2) Preparing an impregnation liquid: adding 0.5wt% of two-dimensional nano carbon material into coal tar pitch with the softening point of 95 ℃ and the coking value of more than 45%, and ultrasonically mixing uniformly at 165 ℃ with the ultrahigh sound wave frequency of 30 Khz.
(3) High-pressure impregnation: the impregnation liquid prepared in the step (2) is used for preparing the carbon fiber preform from 0.45g/cm according to the step (1)3Increase to 1.5g/cm3Adding the calculated amount of the carbon fiber preform, immersing the carbon fiber preform, keeping the temperature at 140 ℃ for 1.5h under the condition of 8.0MPa, and cooling to room temperature;
(4) pressure carbonization: after the treatment in the step (3) is finished, reducing the pressure to 2.0MPa, and carrying out temperature programming to 850 ℃ for carbonization for 4h, wherein the temperature programming curve is as follows: heating to 230 ℃ for 3 h; 230 ℃ for 2 h; 230 to 650 ℃ for 18 h; 650 to 850 ℃ for 9 h; 850 ℃ and 4 h.
(5) Discharging the product out of the furnace: cooling to room temperature, reducing the pressure to atmospheric pressure, and taking out the carbon fiber preform to obtain the carbon fiber preform.
Comparative example 1
The difference from the example 2 is that the one-dimensional nano carbon material is not added in the impregnation liquid.
Comparative example 2
The difference from example 2 is that the pressure in the high pressure impregnation step was 3.0MPa and the pressure in the pressure carbonization step was 1 MPa.
Effect example 1
The products obtained in example 2, example 3, example 4, comparative example 1 and comparative example 2 were subjected to the performance measurement of graphitization degree, tensile strength, thermal conductivity and thermal diffusivity, which is specifically shown in table 1.
TABLE 1 Properties
Figure RE-269268DEST_PATH_IMAGE001
The process provided by the invention not only shortens the production period by 90 percent and improves the production efficiency, but also ensures the excellent performance of the product, can ensure the uniform internal structure of the product and prolong the service life of the product, and can reduce the production cost by at least 1.1 million yuan/year according to the calculation of average using 3 ten thousand crucibles per year in the domestic monocrystalline silicon industry at present, thereby promoting the continuous cost reduction of the photovoltaic industry and realizing the flat price surfing quickly.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. The high-pressure impregnation pressurization carbonization equipment for the carbon fiber preforms is characterized by comprising an outer liner (1) and an inner liner (2) which are matched with each other, wherein the upper ends of the outer liner (1) and the inner liner (2) are provided with openings, and a sealing cavity (3) for placing the carbon fiber preforms (4) is formed between the outer liner (1) and the inner liner; a shell (5) is arranged on the outer side of the outer container (1), a heat insulation material (7) is arranged in the shell (5), and an electric heating pipe (8) is arranged between the outer side of the outer container (1) and the heat insulation material (7); an upper cover (6) is arranged at the upper end of the inner container (2), a heat insulation material (7) is arranged on the inner side of the upper cover (6), and an electric heating pipe (8) is arranged on the inner side of the inner container (2); the sealing cavity (3) is connected with a pressure regulating chamber (10) through a vent pipeline (9), and an automatic pressure relief control valve (11), an automatic pressure increasing control valve (12) and a pressure gauge (13) are arranged on the pressure regulating chamber (10); the sealed cavity (3) is connected with an impregnation liquid pool (15) through a liquid inlet pipeline (14), and a high-pressure pump (16) and an electric valve (17) are arranged on the liquid inlet pipeline (14).
2. The carbon fiber preform high-pressure impregnation pressure carbonization apparatus as claimed in claim 1, wherein a temperature sensor is provided between the outer side of the outer liner (1) and the heat insulating material (7) and inside the inner liner (2).
3. The carbon fiber preform high-pressure impregnation and pressure carbonization apparatus as claimed in claim 1, wherein the outer shell (1) and the upper cover (6) are both provided with temperature control instruments (18), and the temperature control instruments (18) are respectively electrically connected with temperature sensors arranged between the outer side of the outer container (1) and the heat insulation material (7) and the inner side of the inner container (1).
4. The carbon fiber preform high-pressure impregnation pressure carbonization device as claimed in claim 1, wherein the upper ends of the outer liner (1) and the inner liner (2) are provided with annular outer edges, the outer edges of the outer liner (1) and the inner liner (2) are provided with corresponding threaded holes, and the outer liner (1) and the inner liner (2) are connected together through connecting bolts (19).
5. The carbon fiber preform high-pressure impregnation pressure carbonization apparatus according to claim 1, characterized in that a sealing ring (20) is provided between the outer edge of the outer container (1) and the outer edge of the inner container (2).
6. The carbon fiber preform high-pressure impregnation and pressure carbonization apparatus according to claim 1, wherein the top of the sealed chamber (3) is provided with a vent (2-1) connected to the vent line (9), and the bottom of the sealed chamber (3) is provided with an impregnation liquid inlet (1-1) connected to the liquid inlet line (14).
7. A carbon fiber preform high-pressure impregnation pressure carbonization apparatus according to claim 1, characterized in that the clearance at any of the seal cavities (3) is 2-3mm larger than the thickness of the carbon fiber preform (4) at that point.
8. A process for high-pressure impregnation pressure carbonization of carbon fiber preforms using the apparatus according to any one of claims 1 to 7, characterized in that it comprises the steps of:
(1) weaving the prefabricated body: adopting T700 protofilament to produce carbon cloth and net tyre, calculating dosage according to size density, cross-layer knitting, 30 needles/cm2Obtaining a carbon fiber preform;
(2) preparing an impregnation liquid: adding 0.5-1.0 wt% of one-dimensional or two-dimensional nano carbon material into coal tar pitch, and heating and mixing uniformly for later use;
(3) high-pressure impregnation: the impregnation liquid prepared in the step (2) has the density of the carbon fiber preform from 0.45g/cm according to the step (1)3Increase to 1.5g/cm3Adding the calculated amount of the carbon fiber preform, immersing the carbon fiber preform, and keeping the temperature of 140-160 ℃ for 1-2 hours under the condition of 5-8 MPa;
(4) pressure carbonization: after the treatment in the step (3) is completed, reducing the pressure to 2-4 MPa, and carrying out temperature programming to 850 +/-10 ℃ for carbonization for 3-4 h, wherein the temperature programming curve is as follows: heating to 230 ℃ for 3 h; 230 ℃ for 2 h; 230 to 650 ℃ for 18 h; 650 to 850 ℃ for 9 h; 850 ℃ for 4 h;
(5) discharging the product out of the furnace: cooling to room temperature, reducing the pressure to atmospheric pressure, and taking out the carbon fiber preform to obtain the carbon fiber preform.
9. The high-pressure impregnation pressure carbonization process of the carbon fiber preform as claimed in claim 8, wherein the softening point of the coal tar pitch in the step (2) is 90-100 ℃ and the coking value is more than 45%.
10. The high-pressure impregnation pressure carbonization process of the carbon fiber preform as claimed in claim 8, wherein the heating temperature in the step (2) is 150-180 ℃, and ultrasonic uniform mixing and stirring are adopted.
CN202010547410.3A 2020-06-16 2020-06-16 High-pressure impregnation pressurization carbonization process and equipment for carbon fiber preform Pending CN111570192A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115369592A (en) * 2022-08-31 2022-11-22 安徽天富环保科技材料有限公司 Carbon fiber cloth felt preparation equipment and preparation process

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115369592A (en) * 2022-08-31 2022-11-22 安徽天富环保科技材料有限公司 Carbon fiber cloth felt preparation equipment and preparation process

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