CN112358232A - Manufacturing method of mould pressing needling carbon crucible support - Google Patents

Manufacturing method of mould pressing needling carbon crucible support Download PDF

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Publication number
CN112358232A
CN112358232A CN202011386952.3A CN202011386952A CN112358232A CN 112358232 A CN112358232 A CN 112358232A CN 202011386952 A CN202011386952 A CN 202011386952A CN 112358232 A CN112358232 A CN 112358232A
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China
Prior art keywords
carbon fiber
crucible support
phenolic resin
carbon
needled
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Pending
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CN202011386952.3A
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Chinese (zh)
Inventor
裴洋
樊乾国
侯光远
李晓天
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Xi'an Meilan New Material Co ltd
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Xi'an Meilan New Material Co ltd
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Priority to CN202011386952.3A priority Critical patent/CN112358232A/en
Publication of CN112358232A publication Critical patent/CN112358232A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • C04B26/10Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B26/12Condensation polymers of aldehydes or ketones
    • C04B26/122Phenol-formaldehyde condensation polymers
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10Crucibles or containers for supporting the melt
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/20Mortars, concrete or artificial stone characterised by specific physical values for the density

Abstract

The invention discloses a method for manufacturing a molded needled carbon crucible support, which relates to the technical field of crucible supports and comprises the following steps: carbon fiber felt, carbon fiber cloth and liquid phenolic resin; the method comprises the following steps: forming a blank body by needling the carbon fiber felt and the carbon fiber cloth through carbon fibers; pouring 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; placing the blank into a processed graphite mold tool, then placing the whole mold into a flat vulcanizing machine to carry out hot press molding on the blank, wherein the formed blank can form a crucible support; the method is characterized in that demoulding treatment is carried out on the crucible support, then chemical vapor deposition densification and liquid phenolic resin impregnation-carbonization process densification are respectively carried out on the crucible support, and the crucible support is prepared by adding liquid phenolic resin on the needled crucible support and carrying out hot pressing, so that the crucible support is not easy to bulge, crack and stab and detach when the crucible support is used at a high temperature.

Description

Manufacturing method of mould pressing needling carbon crucible support
Technical Field
The invention belongs to the technical field of crucible supports, and particularly relates to a manufacturing method of a molded needled carbon crucible support.
Background
At present, a graphite thermal field and a carbon-carbon composite material thermal field are generally used in domestic high thermal fields (such as silicon single crystal pulling furnaces), however, graphite products are easy to crack by heating, have short service life, poor friction resistance and low corrosion resistance, and further a crucible support in a needling forming mode is hoped to replace a graphite piece to reduce the production cost;
the needling technology of the common crucible support also has the problems of long time consumption, easy internal protrusion, cracking, stabbing and the like of the product.
Disclosure of Invention
The invention aims to provide a method for manufacturing a mould pressing needling carbon crucible support, which aims to solve the problems in the background technology.
The technical scheme adopted by the invention is as follows:
a method for manufacturing a molded needled carbon crucible support comprises the following steps
Raw materials: carbon fiber felt, carbon fiber cloth and liquid phenolic resin;
the method comprises the following steps:
forming a blank body by needling the carbon fiber felt and the carbon fiber cloth through carbon fibers;
pouring 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;
placing the blank into a processed graphite mold tool, then placing the whole mold into a flat vulcanizing machine to carry out hot press molding on the blank, wherein the formed blank can form a crucible support;
demoulding the crucible support, and respectively carrying out chemical vapor deposition densification and liquid phenolic resin impregnation-carbonization process densification on the crucible support.
Preferably, in the hot pressing process of the plate vulcanizing machine:
raising the temperature of the plate vulcanizing machine from room temperature to 80 ℃ for preheating treatment, keeping the temperature for 30min, and intermittently exhausting gas for one to two times in the process;
adding initial pressure of 1Mpa and supplementary pressure of 0.5Mpa, and maintaining the pressure for 20 min;
heating to 100 deg.C, maintaining the temperature for 30min, and pressurizing to 10 Mpa;
continuously heating to 140 deg.C, and pressurizing to 12 Mpa;
continuously heating to 160 ℃, pressurizing to 16Mpa, preserving heat for 1h and maintaining pressure for 30 min.
Preferably, when the carbon fiber felt and the carbon fiber cloth are subjected to carbon fiber needling, the carbon fiber felt and the carbon fiber cloth are subjected to needling according to the quantity ratio of 5: 1.
Preferably, the areas of the carbon fiber cloth and the carbon fiber felt are both 500mm by 500 mm.
Preferably, the density of the carbon fiber needle-punched embryo body is 35-40 needle/cm < year >.
Preferably, the liquid phenolic resin is ammonia phenolic resin, the curing carbon residue rate of the ammonia phenolic resin is 96%, and the fluid viscosity is 300mPa.s at room temperature.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
according to the invention, the pot support is prepared by adding the liquid phenolic resin on the needled pot support and performing hot pressing, and the pot support is not easy to bulge, crack and stab off when used at a high temperature.
Drawings
FIG. 1 is a block flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
Referring to fig. 1, a method for manufacturing a molded needled carbon crucible support comprises the steps of
Raw materials: carbon fiber felt, carbon fiber cloth and liquid phenolic resin;
the method comprises the following steps:
forming a blank body by needling the carbon fiber felt and the carbon fiber cloth through carbon fibers;
pouring 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;
placing the blank into a processed graphite mold tool, then placing the whole mold into a flat vulcanizing machine to carry out hot press molding on the blank, wherein the formed blank can form a crucible support;
demoulding the crucible support, and respectively carrying out chemical vapor deposition densification and liquid phenolic resin impregnation-carbonization process densification on the crucible support.
In the hot pressing process of the plate vulcanizing machine:
raising the temperature of the plate vulcanizing machine from room temperature to 80 ℃ for preheating treatment, keeping the temperature for 30min, and intermittently exhausting gas for one to two times in the process;
adding initial pressure of 1Mpa and supplementary pressure of 0.5Mpa, and maintaining the pressure for 20 min;
heating to 100 deg.C, maintaining the temperature for 30min, and pressurizing to 10 Mpa;
continuously heating to 140 deg.C, and pressurizing to 12 Mpa;
continuously heating to 160 ℃, pressurizing to 16Mpa, preserving heat for 1h and maintaining pressure for 30 min.
When the carbon fiber felt and the carbon fiber cloth are needled, the carbon fiber felt and the carbon fiber cloth are needled according to the quantity ratio of 5: 1.
The areas of the carbon fiber cloth and the carbon fiber felt are both 500mm multiplied by 500 mm.
The density of the carbon fiber needled embryo is 35-40 needle/. cm.
The liquid phenolic resin is ammonia phenolic resin, the curing carbon residue rate of the ammonia phenolic resin is 96%, and the fluid viscosity is 300mPa.s at room temperature.
Example two
A method for manufacturing a molded needled carbon crucible support comprises the following steps
Raw materials: carbon fiber felt, carbon fiber cloth and liquid phenolic resin;
the method comprises the following steps:
forming a blank body by needling the carbon fiber felt and the carbon fiber cloth through carbon fibers;
pouring 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;
when the carbon fiber felt and the carbon fiber cloth are needled, the carbon fiber felt and the carbon fiber cloth are needled according to the quantity ratio of 5: 1.
The areas of the carbon fiber cloth and the carbon fiber felt are both 500mm multiplied by 500 mm.
The density of the carbon fiber needled embryo is 35-40 needle/. cm.
EXAMPLE III
A method for manufacturing a molded needled carbon crucible support comprises the following steps
Raw materials: carbon fiber felt, carbon fiber cloth and liquid phenolic resin;
the method comprises the following steps:
forming a blank body by needling the carbon fiber felt and the carbon fiber cloth through carbon fibers;
when the carbon fiber felt and the carbon fiber cloth are needled, the carbon fiber felt and the carbon fiber cloth are needled according to the quantity ratio of 5: 1.
The areas of the carbon fiber cloth and the carbon fiber felt are both 500mm multiplied by 500 mm.
The density of the carbon fiber needled embryo is 35-40 needle/. cm.
The three groups of embodiments are tested, in order to ensure the accuracy of the test result in the test process, under the technical requirements of the three groups of embodiments, five crucible supports are manufactured by utilizing each group of technology respectively, then the five crucible supports are tested under the state of high temperature respectively, then the test is carried out on the crucible supports after the test, the damage detection content comprises protrusion, cracking and stabbing, and the test result is as shown in the following table 1:
Figure DEST_PATH_IMAGE001
TABLE 1
To sum up, in the first embodiment, liquid phenolic resin is added to a needled crucible support and then the crucible support is subjected to hot pressing, in the second embodiment, the liquid phenolic resin is added to the crucible support and is baked and formed, in the third embodiment, the prior art is adopted, and the crucible support is directly subjected to needling and forming;
as can be seen from the experimental data in Table 1, the crucible support processed by the technical scheme of the first embodiment has the highest quality, the crucible support processed by the technical scheme of the second embodiment has the second highest quality, and the crucible support processed by the technical scheme of the third embodiment has the worst quality;
therefore, the crucible support prepared by adding the liquid phenolic resin on the needled crucible support and performing hot pressing has the highest quality, so that the crucible support is not easy to bulge, crack and stab off when being used at a high temperature.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (6)

1. A method for manufacturing a mould pressing needling carbon crucible support is characterized by comprising the following steps: comprises that
Raw materials: carbon fiber felt, carbon fiber cloth and liquid phenolic resin;
the method comprises the following steps:
forming a blank body by needling the carbon fiber felt and the carbon fiber cloth through carbon fibers;
pouring 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;
placing the blank into a processed graphite mold tool, then placing the whole mold into a flat vulcanizing machine to carry out hot press molding on the blank, wherein the formed blank can form a crucible support;
demoulding the crucible support, and respectively carrying out chemical vapor deposition densification and liquid phenolic resin impregnation-carbonization process densification on the crucible support.
2. The manufacturing method of the molded needled carbon crucible support according to claim 1, characterized in that: in the hot pressing process of the vulcanizing press:
raising the temperature of the plate vulcanizing machine from room temperature to 80 ℃ for preheating treatment, keeping the temperature for 30min, and intermittently exhausting gas for one to two times in the process;
adding initial pressure of 1Mpa and supplementary pressure of 0.5Mpa, and maintaining the pressure for 20 min;
heating to 100 deg.C, maintaining the temperature for 30min, and pressurizing to 10 Mpa;
continuously heating to 140 deg.C, and pressurizing to 12 Mpa;
continuously heating to 160 ℃, pressurizing to 16Mpa, preserving heat for 1h and maintaining pressure for 30 min.
3. The manufacturing method of the molded needled carbon crucible support according to claim 1, characterized in that: when the carbon fiber felt and the carbon fiber cloth are needled, the carbon fiber felt and the carbon fiber cloth are needled according to the quantity ratio of 5: 1.
4. The manufacturing method of the molded needled carbon crucible support according to claim 1, characterized in that: the areas of the carbon fiber cloth and the carbon fiber felt are both 500mm multiplied by 500 mm.
5. The manufacturing method of the molded needled carbon crucible support according to claim 1, characterized in that: the density of the carbon fiber needled embryo body is 35-40 cm/cm.
6. The manufacturing method of the molded needled carbon crucible support according to claim 1, characterized in that: the liquid phenolic resin is ammonia phenolic resin, the curing carbon residue rate of the ammonia phenolic resin is 96%, and the fluid viscosity is 300mPa.s at room temperature.
CN202011386952.3A 2020-12-01 2020-12-01 Manufacturing method of mould pressing needling carbon crucible support Pending CN112358232A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113896561A (en) * 2021-11-18 2022-01-07 杭州幄肯新材料科技有限公司 Liquid phase-vapor deposition carbon fiber/carbon composite thermal field material and preparation method thereof
CN114379115A (en) * 2021-12-31 2022-04-22 浙江德鸿碳纤维复合材料有限公司 Carbon crucible support and preparation method thereof
CN115160010A (en) * 2022-07-18 2022-10-11 浙江星辉新材料科技有限公司 Manufacturing method of mould pressing needling carbon crucible support
CN116375488A (en) * 2023-02-17 2023-07-04 贵州省紫安新材料科技有限公司 Mould pressing manufacturing method of carbon-carbon crucible support

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102826867A (en) * 2012-09-13 2012-12-19 湖南省鑫源新材料股份有限公司 Carbon/carbon composite material flat plate preparation method
CN109721377A (en) * 2019-01-30 2019-05-07 湖南兴晟新材料科技有限公司 Ceramic Matrix Composites Reinforced by Carbon Fibers and preparation method thereof
CN111960841A (en) * 2020-08-31 2020-11-20 陕西美兰德炭素有限责任公司 Preparation method of crucible tray of single crystal furnace

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102826867A (en) * 2012-09-13 2012-12-19 湖南省鑫源新材料股份有限公司 Carbon/carbon composite material flat plate preparation method
CN109721377A (en) * 2019-01-30 2019-05-07 湖南兴晟新材料科技有限公司 Ceramic Matrix Composites Reinforced by Carbon Fibers and preparation method thereof
CN111960841A (en) * 2020-08-31 2020-11-20 陕西美兰德炭素有限责任公司 Preparation method of crucible tray of single crystal furnace

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113896561A (en) * 2021-11-18 2022-01-07 杭州幄肯新材料科技有限公司 Liquid phase-vapor deposition carbon fiber/carbon composite thermal field material and preparation method thereof
CN113896561B (en) * 2021-11-18 2022-09-16 杭州幄肯新材料科技有限公司 Liquid phase-vapor deposition carbon fiber/carbon composite thermal field material and preparation method thereof
CN114379115A (en) * 2021-12-31 2022-04-22 浙江德鸿碳纤维复合材料有限公司 Carbon crucible support and preparation method thereof
CN115160010A (en) * 2022-07-18 2022-10-11 浙江星辉新材料科技有限公司 Manufacturing method of mould pressing needling carbon crucible support
CN116375488A (en) * 2023-02-17 2023-07-04 贵州省紫安新材料科技有限公司 Mould pressing manufacturing method of carbon-carbon crucible support

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