CN114057486A - Method for preparing carbon/carbon split-type structure crucible support at low cost - Google Patents

Method for preparing carbon/carbon split-type structure crucible support at low cost Download PDF

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Publication number
CN114057486A
CN114057486A CN202111364001.0A CN202111364001A CN114057486A CN 114057486 A CN114057486 A CN 114057486A CN 202111364001 A CN202111364001 A CN 202111364001A CN 114057486 A CN114057486 A CN 114057486A
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China
Prior art keywords
carbon
crucible support
graphite
preparing
low cost
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Application number
CN202111364001.0A
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Chinese (zh)
Inventor
邵忠
李国强
于守洪
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Inner Mongolia Kang Carbon Composite Material Technology Co ltd
Shanghai Kangtan Composite Material Technology Co ltd
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Inner Mongolia Kang Carbon Composite Material Technology Co ltd
Shanghai Kangtan Composite Material Technology Co ltd
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Application filed by Inner Mongolia Kang Carbon Composite Material Technology Co ltd, Shanghai Kangtan Composite Material Technology Co ltd filed Critical Inner Mongolia Kang Carbon Composite Material Technology Co ltd
Priority to CN202111364001.0A priority Critical patent/CN114057486A/en
Publication of CN114057486A publication Critical patent/CN114057486A/en
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L9/00—Supporting devices; Holding devices
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/522—Graphite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time

Abstract

The invention discloses a method for preparing a crucible support with a carbon/carbon split structure at low cost, which comprises a carbon/carbon tool, wherein a plurality of convex grooves are uniformly formed in the carbon/carbon tool from top to bottom, and the crucible support is vertically arranged in the convex grooves in multiple layers.

Description

Method for preparing carbon/carbon split-type structure crucible support at low cost
Technical Field
The invention relates to a method for preparing a carbon/carbon split-type structure crucible support at low cost.
Background
The problem that the service life of the graphite crucible support is not up to standard is greatly solved due to the appearance of the carbon/carbon crucible support. However, the preparation cost is high and is not competitive, the furnace deposition is a popular scheme, but a plurality of cycles are needed in the furnace, and the preparation can be successfully prepared by machining the furnace 1 to 2 times in the middle. Besides, the crucible support is prepared by a mould pressing impregnation and carbonization method, and the mechanical property of the crucible support is enhanced by vapor deposition.
Patent "a manufacturing method of mould pressing acupuncture carbon pot holder" (CN 112358232A) discloses a manufacturing method of mould pressing acupuncture carbon pot holder, which comprises the following basic steps: (1) preparing a laminated 2.5D needling preform blank; (2) pouring the liquid phenolic resin on the surface of the blank body to enable the liquid phenolic resin to completely penetrate through the blank body, and then pre-baking; (3) placing the blank into a processed graphite mold tool, and then placing the whole mold into a flat vulcanizing machine to carry out hot press molding on the blank, wherein the molded blank can form a pot support; (4) and demolding the pot support, respectively carrying out chemical vapor deposition densification and liquid phenolic resin impregnation-carbonization process densification on the pot support, adding liquid phenolic resin on the needled pot support, and manufacturing the pot support in a hot pressing mode. The method adopts resin impregnation, then carbonization and high-temperature heat treatment are carried out after compression molding, and finally the carbon crucible support is prepared by vapor deposition reinforcement and multi-period impregnation carbonization process. However, the preparation period is long, the raw material cost is high, the mechanical property of the crucible support prepared by the pure vapor deposition method is poor, and the fracture toughness is represented by brittle or pseudoplastic fracture.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for preparing a carbon/carbon split-type structure crucible support at low cost, which adopts a scheme of opening a hole at the core part of a prefabricated body of the crucible support and independently supplying air in multiple layers, can prepare the crucible support with high strength and high density in a short time, has short preparation period and low cost, and is suitable for mass production.
The invention can be realized by the following technical scheme:
a method for preparing a carbon/carbon split structure crucible support at low cost comprises a carbon/carbon tool, wherein a plurality of protruding grooves are uniformly formed in the carbon/carbon tool from top to bottom, and the method comprises the following steps:
1) preparing a crucible support prefabricated body, and opening a hole in the center of the crucible support prefabricated body;
2) loading a crucible support prefabricated body into a furnace, sequentially arranging the crucible support prefabricated body in a protruding groove of a carbon/carbon tool, inserting a plurality of graphite pipes from the bottom of the crucible support, wherein each graphite pipe meets multilayer independent gas supply in height, plugging holes between gas outlets of the plurality of graphite pipes and the crucible support, and adjusting the number of the graphite pipes and the outlet positions of the graphite pipes according to the number of the crucible support prefabricated body arranged in the height direction in the deposition furnace, wherein the plugging material is soft felt;
3) respectively introducing a certain amount of mixed gas of natural gas and propane into the graphite pipe, and depositing for a certain time at low pressure and high temperature to prepare a carbon/carbon crucible support body;
4) and processing the carbon/carbon crucible support body to the net size of the product, and then plugging the hole in the center by using a plug.
Further, in the step 1), the diameter of the opening of the hole is 30-100 mm.
Further, in the step 2), after the crucible support preforms are charged, the gap between the crucible support preforms is kept at 10-30 mm.
Further, adjusting the number of graphite tubes to arrange a graphite tube air inlet position every 3-10 crucible support preforms according to the number of the crucible support preforms arranged in the height direction in the deposition furnace.
Further, the diameter size of the graphite tube is 10-25 mm.
Further, in the step 3), the mixed gas of the natural gas and the propane is introduced in a range of 5-10m3H, volume ratio 1: 10-1: 5, the low pressure is 3-8kPa, the high temperature is 1050 ℃, and the deposition time is 200-300 h.
Further, the plug is made of carbon/carbon or graphite, the plug is circular or rectangular, and the crucible support main body and the plug are connected in a concave-convex, conical or threaded mode.
Advantageous effects
According to the invention, the middle of the crucible support preform is provided with a hole, and the multilayer furnace charging scheme can effectively utilize the space of the deposition furnace and ensure the maximum furnace charging amount in the furnace; the uniformity and consistency of product deposition can be guaranteed by the aid of the multiple layers of independent gas supply, and the product can be qualified by one-time deposition, so that the crucible support is short in preparation period and low in cost.
Drawings
FIG. 1 is a schematic structural view of a pot support preform in the invention;
FIG. 2 is a schematic view of charging of a crucible support preform in the invention;
FIG. 3 is a schematic diagram of a matching structure of a crucible support body and a central plug in the invention.
In the figure, A-carbon/carbon tooling, B-crucible support prefabricated body, C-graphite tube and D-soft felt
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification.
Example 1
A method for preparing a carbon/carbon split-type structure crucible support at low cost comprises the following steps:
1. preparing a crucible support prefabricated body, and opening a circular hole at the center of the crucible support prefabricated body, wherein the diameter of the opening is 30mm, as shown in figure 1;
2. the crucible holds in the palm preform B and loads onto the stove according to the mode of drawing 2, and the crucible holds in the palm and holds in the palm to support through carbon/carbon frock A, makes its crucible hold in the palm the clearance between keep 10mm interval, and graphite pipe C holds in the palm the bottom from the crucible and inserts, satisfies the independent air feed of multilayer in height, and graphite pipe C gas outlet department and crucible hold in the palm the interorifice and will carry out the shutoff, and sealing material is soft felt D, and wherein the diameter size of graphite pipe is 10 mm. Adjusting the quantity of inlet graphite and the outlet position of an inlet graphite pipe according to the quantity of the crucible support preforms arranged in the height direction of the deposition furnace, wherein in the embodiment, the quantity of the graphite pipes is that one inlet position of the graphite pipe is arranged every 3 crucible support preforms, namely, one graphite pipe is arranged every 3 crucible support preforms;
3. respectively introducing 5m of graphite tubes C3H mixed gas of natural gas and propane, volume ratio is 1: 10, depositing for 200 hours at the temperature of 1000 ℃ and under the pressure of 3kPa to prepare a carbon/carbon crucible support body;
4. the carbon/carbon crucible support body is processed to the net size of the product, the hole at the center is blocked by a plug after the product is obtained, and the plug and the carbon crucible support body are matched in a conical surface manner, as shown in figure 3.
Example 2
A method for preparing a carbon/carbon split-type structure crucible support at low cost comprises the following steps:
1. preparing a crucible support prefabricated body, and opening a circular hole at the central position of the crucible support prefabricated body, wherein the diameter of the opening is 100 mm;
2. the crucible holds in the palm preform B and loads onto the stove according to the mode of drawing 2, and the crucible holds in the palm and holds in the palm to support through carbon/carbon frock A, makes its crucible hold in the palm the clearance between the interval and keep 30mm, and graphite tube C holds in the palm the bottom from the crucible and inserts, satisfies the independent air feed of multilayer in height, and graphite tube C gas outlet department and crucible hold in the palm the interorifice and will carry out the shutoff, and sealing material is soft felt D, and wherein the diameter size of graphite tube is 25 mm. Adjusting the quantity of inlet graphite and the outlet position of an inlet graphite pipe according to the quantity of the crucible support preforms arranged in the height direction of the deposition furnace, wherein in the embodiment, the quantity of the graphite pipes is that one inlet position of the graphite pipe is arranged every 3 crucible support preforms, namely, one graphite pipe is arranged every 4 crucible support preforms;
3. respectively introducing 10m of graphite tubes C3H mixed gas of natural gas and propane, volume ratio is 1: 5, depositing for 300 hours at the high temperature of 1050 ℃ under 8kPa to prepare a carbon/carbon crucible support body;
4. the carbon/carbon crucible support body is processed to the net size of a product, a hole in the center is blocked by a plug after the product is made to pass through, and the plug and the carbon crucible support body are matched in a concave-convex mode.
Example 3
A method for preparing a carbon/carbon split-type structure crucible support at low cost comprises the following steps:
1. preparing a crucible support prefabricated body, and opening a circular hole at the central position of the crucible support prefabricated body, wherein the diameter of the opening is 80 mm;
2. the crucible holds in the palm preform B and loads onto the stove according to the mode of drawing 2, and the crucible holds in the palm and holds in the palm to support through carbon/carbon frock A, makes its crucible hold in the palm the clearance between 25mm interval, and graphite pipe C holds in the palm the bottom from the crucible and inserts, satisfies the independent air feed of multilayer in height, and graphite pipe C gas outlet department and crucible hold in the palm the interpore and will carry out the shutoff, and sealing material is soft felt D, and wherein the diameter size of graphite pipe is 20 mm. Adjusting the quantity of inlet graphite and the outlet position of an inlet graphite pipe according to the quantity of the arranged crucible support preforms in the height direction of the deposition furnace, wherein in the embodiment, the quantity of the graphite pipes is that one inlet position of the graphite pipe is arranged every 3 crucible support preforms, namely, one graphite pipe is arranged every 8 crucible support preforms;
3. respectively introducing 6m of graphite tubes C3H mixed gas of natural gas and propane, volume ratio is 1: 8, depositing for 220 hours at the high temperature of 1020 ℃ under the condition of 5kPa to prepare a carbon/carbon crucible support body;
4. the carbon/carbon crucible support body is processed to the net size of a product, a hole in the center is blocked by a plug, and the plug is matched with the carbon crucible support body in a threaded mode.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (7)

1. The method for preparing the carbon/carbon split-type structure crucible support at low cost comprises a carbon/carbon tool, wherein a plurality of protruding grooves are uniformly formed in the carbon/carbon tool from top to bottom, and the method is characterized by comprising the following steps of:
1) preparing a crucible support prefabricated body, and opening a hole in the center of the crucible support prefabricated body;
2) loading a crucible support prefabricated body into a furnace, sequentially arranging the crucible support prefabricated body in a protruding groove of a carbon/carbon tool, inserting a plurality of graphite pipes from the bottom of the crucible support, wherein each graphite pipe meets multilayer independent gas supply in height, plugging holes between gas outlets of the plurality of graphite pipes and the crucible support, and adjusting the number of the graphite pipes and the outlet positions of the graphite pipes according to the number of the crucible support prefabricated body arranged in the height direction in the deposition furnace, wherein the plugging material is soft felt;
3) respectively introducing a certain amount of mixed gas of natural gas and propane into the graphite pipe, and depositing for a certain time at low pressure and high temperature to prepare a carbon/carbon crucible support body;
4) and processing the carbon/carbon crucible support body to the net size of the product, and then plugging the hole in the center by using a plug.
2. The method for preparing the carbon/carbon split-structure pot holder at low cost according to claim 1, wherein in the step 1), the opening diameter of the hole is 30-100 mm.
3. The method for preparing a carbon/carbon split-structure pot holder at low cost according to claim 1, wherein in the step 2), the gap between the pot precursor is maintained at 10-30mm after the pot precursor is charged.
4. The method for preparing a carbon/carbon split-structure pot holder at low cost according to claim 1, wherein the number of graphite tubes is adjusted to every 3 to 10 pot holder preforms in the gas inlet position according to the number of the pot holder preforms arranged in the height direction in the deposition furnace.
5. The method for preparing the carbon/carbon split-structure pot holder at low cost according to claim 1, wherein the diameter of the graphite tube is 10-25 mm.
6. The method for preparing the carbon/carbon split-structure pot holder at low cost according to claim 1, wherein in the step 3), the mixed gas of the natural gas and the propane is introduced in a range of 5-10m3H, volume ratio 1: 10-1: 5, the low pressure is 3-8kPa, the high temperature is 1050 ℃, and the deposition time is 200-300 h.
7. The method for preparing the carbon/carbon split-structure pot holder at low cost according to claim 1, wherein the plug is made of carbon/carbon or graphite, the plug is round or rectangular, and the pot holder body and the plug are connected in a concave-convex, conical or threaded manner.
CN202111364001.0A 2021-11-17 2021-11-17 Method for preparing carbon/carbon split-type structure crucible support at low cost Withdrawn CN114057486A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115141029A (en) * 2022-08-31 2022-10-04 浙江德鸿碳纤维复合材料有限公司 Preparation method of carbon/carbon crucible supporting rod

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109354508A (en) * 2018-12-13 2019-02-19 上海康碳复合材料科技有限公司 A kind of CVI process of batch preparing carbon/carbon composite material crucible side
CN109400198A (en) * 2018-12-13 2019-03-01 上海康碳复合材料科技有限公司 A kind of carbon/carbon (pottery) composite material brake disc Preparation equipment and preparation method thereof based on quick sedimentation process
CN109503188A (en) * 2018-12-14 2019-03-22 上海康碳复合材料科技有限公司 It is a kind of that carbon/carbon crucible CVI process is prepared based on flow fieldoptimization

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109354508A (en) * 2018-12-13 2019-02-19 上海康碳复合材料科技有限公司 A kind of CVI process of batch preparing carbon/carbon composite material crucible side
CN109400198A (en) * 2018-12-13 2019-03-01 上海康碳复合材料科技有限公司 A kind of carbon/carbon (pottery) composite material brake disc Preparation equipment and preparation method thereof based on quick sedimentation process
CN109503188A (en) * 2018-12-14 2019-03-22 上海康碳复合材料科技有限公司 It is a kind of that carbon/carbon crucible CVI process is prepared based on flow fieldoptimization

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115141029A (en) * 2022-08-31 2022-10-04 浙江德鸿碳纤维复合材料有限公司 Preparation method of carbon/carbon crucible supporting rod
CN115141029B (en) * 2022-08-31 2022-11-11 浙江德鸿碳纤维复合材料有限公司 Preparation method of carbon/carbon crucible support rod

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Application publication date: 20220218