CN117089921A - Integrated carbon/carbon crucible supporting rod - Google Patents
Integrated carbon/carbon crucible supporting rod Download PDFInfo
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- CN117089921A CN117089921A CN202310881551.2A CN202310881551A CN117089921A CN 117089921 A CN117089921 A CN 117089921A CN 202310881551 A CN202310881551 A CN 202310881551A CN 117089921 A CN117089921 A CN 117089921A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 101
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000004744 fabric Substances 0.000 claims abstract description 26
- 238000000280 densification Methods 0.000 claims abstract description 21
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 17
- 239000004917 carbon fiber Substances 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000003754 machining Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 25
- 230000008569 process Effects 0.000 claims description 19
- 239000003292 glue Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000010410 layer Substances 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 12
- 238000003763 carbonization Methods 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 239000011229 interlayer Substances 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 239000003345 natural gas Substances 0.000 claims description 6
- 239000005011 phenolic resin Substances 0.000 claims description 6
- 229920001568 phenolic resin Polymers 0.000 claims description 6
- 239000002296 pyrolytic carbon Substances 0.000 claims description 6
- 235000005074 zinc chloride Nutrition 0.000 claims description 6
- 239000011592 zinc chloride Substances 0.000 claims description 6
- 239000011300 coal pitch Substances 0.000 claims description 5
- 230000008595 infiltration Effects 0.000 claims description 5
- 238000001764 infiltration Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- WIEXMPDBTYDSQF-UHFFFAOYSA-N 1,3-bis(furan-2-yl)propan-2-one Chemical compound C=1C=COC=1CC(=O)CC1=CC=CO1 WIEXMPDBTYDSQF-UHFFFAOYSA-N 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 2
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 239000007849 furan resin Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 2
- 229960001124 trientine Drugs 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 10
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 239000000835 fiber Substances 0.000 abstract description 4
- 238000010923 batch production Methods 0.000 abstract description 2
- XBWAZCLHZCFCGK-UHFFFAOYSA-N 7-chloro-1-methyl-5-phenyl-3,4-dihydro-2h-1,4-benzodiazepin-1-ium;chloride Chemical compound [Cl-].C12=CC(Cl)=CC=C2[NH+](C)CCN=C1C1=CC=CC=C1 XBWAZCLHZCFCGK-UHFFFAOYSA-N 0.000 description 13
- 238000005520 cutting process Methods 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 239000002131 composite material Substances 0.000 description 9
- 238000012545 processing Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 238000010000 carbonizing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000010439 graphite Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000010354 integration Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 241001149930 Protura <class> Species 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
-
- 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
- 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
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- 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
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- 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
- C04B2235/02—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
- C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
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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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- 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
- C04B2235/61—Mechanical properties, e.g. fracture toughness, hardness, Young's modulus or strength
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Ceramic Products (AREA)
Abstract
The application relates to an integrated carbon/carbon crucible supporting rod, and belongs to the technical field of crucible supporting rods. The integrated carbon/carbon crucible supporting rod is an integrated hollow revolving body structure consisting of a supporting rod body and a supporting rod cone head, wherein a first central through hole is formed in the supporting rod body part along the axial direction, a second central through hole is formed in the supporting rod cone head part along the axial direction, and the diameter of the second central through hole is smaller than that of the first central through hole; the integrated hollow revolving body structure is formed by alternately layering and needling a carbon fiber woven cloth and a carbon net tire to form a prefabricated body of the integrated hollow revolving body structure, and then performing carbon densification and machining treatment. The integrated carbon/carbon crucible supporting rod provided by the application has the advantages that the integrity of fibers is greatly reserved, the transmission and bearing performances of products are guaranteed, the preparation is easy, the preparation flow is less, the preparation period is short, the utilization rate of raw materials is high, the cost is low, and the integrated carbon/carbon crucible supporting rod is suitable for batch production.
Description
Technical Field
The application relates to an integrated carbon/carbon crucible supporting rod, and belongs to the technical field of crucible supporting rods.
Background
The single crystal furnace is equipment for drawing single crystal silicon, and mainly comprises a furnace chamber, a quartz crucible, a crucible tray, a crucible supporting rod and a driving device, wherein the crucible tray is arranged in the furnace chamber and is used for supporting a crucible for containing silicon materials, the top end of the crucible supporting rod is connected with the crucible tray in the furnace chamber, the middle section of the crucible supporting rod is exposed out of the furnace chamber, the bottom end of the crucible supporting rod penetrates through the furnace chamber and is connected with the driving device, and the driving device drives the crucible to rotate or move up and down in the furnace chamber through the crucible supporting rod. Besides bearing the environment of huge temperature difference inside and outside the single crystal furnace chamber, the crucible supporting rod also needs to have transmission capacity while bearing the weight of the crucible, the silicon material and the crucible tray. At present, most crucible supporting rods of a single crystal furnace are graphite rods, so that the brittleness of graphite is high, and the increasing bearing capacity cannot be met; in addition, the graphite has large heat conductivity and expansion coefficient, so that heat is conducted to the outside of the furnace chamber, energy consumption is increased, and the carbon/carbon composite material becomes a substitute material of the graphite crucible supporting rod by virtue of excellent mechanical and thermal properties.
Chinese patent CN102619863 a discloses a single crystal furnace supporting rod, which has two structures, one adopts a carbon/carbon composite material integral structure, and is manufactured into a final size by densification and post-machining of a needled preform, but the patent only outlines the density of the needled preform, and does not further describe the structural design of the preform; the other is a carbon/carbon composite material and graphite stack structure, the connecting part of the top of the shaft body of the support rod and the crucible in the furnace is made of graphite materials, the connecting part of the bottom of the shaft body of the support rod and the driving device outside the furnace is made of carbon/carbon composite materials, the carbon/carbon composite materials and the driving device outside the furnace are connected into a support rod product by screw threads or mortise and tenon joints, the top of the support rod of the structure is made of graphite materials with excellent heat conducting performance, so that heat is externally transmitted to cause fluctuation of an internal heating field in the furnace and additional energy consumption, and the shaft body of the support rod is formed by screw threads or mortise and tenon joints. Chinese patent CN115141029 a discloses a method for preparing crucible supporting rod by separating and densifying cylindrical supporting rod body and supporting rod head, and finally assembling and preparing, in which the supporting rod head and supporting rod body are fastened by screw thread, so that there is a risk of loosening and potential safety hazard, in addition, the supporting rod head adopts large-block thick carbon plate material to densify, and then adopts cutting-cutting processing to prepare the reducing crucible supporting rod, and the prefabricated body has the problems of uneven material density and long densification period, and the carbon plate consumption is high and the yield is low in cutting processing. Chinese patent CN114560715 a discloses a method for preparing solid crucible supporting rod, which comprises bonding the prepared carbon fiber composite rod with needled net tyre to form carbon fiber composite rod/carbon transition layer structure, needling and compounding carbon material layer on the periphery of several composite rod/carbon transition layers to form integral supporting rod preform, wherein the structural preform has solid structure, low densification efficiency and uneven density, and in addition, the preparation method of the preform is complex, and has the problem of long production period
Disclosure of Invention
Aiming at the defects of the prior crucible supporting rod, the application provides an integrated carbon/carbon crucible supporting rod, wherein a supporting rod body and a supporting rod cone head are prefabricated bodies with integrated hollow structures formed by alternately layering and needling carbon fiber woven cloth and a carbon net tire, and then the integrated crucible supporting rod with the required size is formed through densification and machining treatment, the integrated structure greatly maintains the integrity of fibers, the transmission and bearing performance of products are ensured, and the utilization rate of raw materials is high; meanwhile, the design of the hollow structure ensures the strength of the product and simultaneously reduces the weight effectively, thereby being beneficial to improving the densification efficiency, shortening the production period and reducing the preparation cost.
The aim of the application is achieved by the following technical scheme.
An integrated carbon/carbon crucible supporting rod is an integrated hollow revolving body structure consisting of a supporting rod body and a supporting rod cone head, wherein a first central through hole is formed in the supporting rod body part along the axial direction, a second central through hole is formed in the supporting rod cone head part along the axial direction, and the diameter of the second central through hole is smaller than that of the first central through hole;
the integrated hollow revolving body structure is formed by alternately layering and needling a carbon fiber woven cloth and a carbon net tire to form a prefabricated body of the integrated hollow revolving body structure, and then performing carbon densification and machining treatment.
Further, the diameter of the first central through hole is 50-75 mm, the diameter of the second central through hole is 5-15 mm, and the outer diameter of the stopper rod body part is 125-140 mm.
Further, the density of the prefabricated body of the integrated hollow revolving body structure is 0.35-0.55 g/cm 3 The density of the compact carbon is 1.45-1.75 g/cm 3 。
Further, the specific preparation steps of the integrated carbon/carbon crucible supporting rod are as follows:
preparing a mandrel with a corresponding shape and size according to the shape and size of an inner molded surface of the integrated hollow revolving body structure, alternately layering a carbon fiber woven cloth and a carbon net tire according to a required proportion, continuously needling a vertical layering surface, circulating the layering-needling operation to obtain a prefabricated body of the integrated hollow revolving body structure (the prefabricated body comprises a prefabricated body of a straight-cylinder-shaped integrated hollow revolving body structure or a prefabricated body of a variable-diameter cylinder-shaped integrated hollow revolving body structure), wherein the difference is that the shape of a corresponding part of a supporting rod cone head is cylindrical, the shape of the supporting rod cone head is required to be processed into a supporting rod cone head with a required shape through a later machine, the shape of the supporting rod cone head is required to be a profiling cone structure, then performing carbon densification treatment on the prefabricated body to form a supporting rod blank, and then performing machining on the supporting rod blank to obtain an integrated carbon/carbon crucible supporting rod with a required size;
the carbon fiber woven cloth is laid in whole or integrally woven with carbon fibers, and continuous fibers in the longitudinal circumferential direction are ensured, including but not limited to carbon fiber plain cloth, warp-weft woven cloth or weft-free cloth.
Further, the surface density of the carbon fiber woven cloth is 200-420 g/m 2 The surface density of the carbon net tire is 30-120 g/m 2 The mass ratio of the carbon fiber woven cloth to the carbon net tire in the preform is 3:1-5:1, and the needling density is 20-40 needles/cm 2 The interlayer density is 7-15 layers/cm, the needling depth is 0.3-1 cm, so that carbon fibers brought into the interlayer in the needling process form a pin structure, and the connection strength between the circumferential layers can be further enhanced.
Further, the specific steps of carbon densification treatment of the preform are as follows:
firstly, pre-curing the surface of a preform, spraying a curing glue solution on the surface of the preform, and then placing the preform in 60-120 o C, curing for 2-6 hours to finish the pre-curing treatment of the preform; for the pre-solidified preform, chemical Vapor Infiltration (CVI) is adopted to deposit pyrolytic carbon to densify the preform to 0.8-1.3 g/cm 3 Then, resin carbon is formed by adopting an impregnant impregnation-carbonization process to continuously densify to 1.45-1.75 g/cm 3 Finally, in a protective atmosphere and 1600-2500 o C, performing high-temperature treatment in a furnace chamber for 2-6 hours;
wherein the curing glue solution is prepared from resin, a curing agent and ethanol according to (8-12): (0.8 to 1.5): (2-3) the resin comprises but not limited to phenolic resin, the curing agent comprises but not limited to zinc chloride, toluene sulfonic acid or triethylene tetramine, and the liquid amount of the spraying curing adhesive on the surface of the preform is 0.5-1.8 mL/cm 2 。
In addition, the CVI process adopts conventional carbon source gas, such as natural gas and olefin with 1-4 carbon atoms, and the carbon source gas can be mixed with protective gas (such as nitrogen gas); the impregnating agent is prepared by conventional impregnating agent such as furan resin, furfuryl ketone resin, and coal pitch.
Further, when the preform is placed in a chemical vapor deposition furnace for pyrolytic carbon deposition, the axial direction of the preform is parallel to the flow direction of the air flow, and the flow direction of the air flow is the direction from the first central through hole to the second central through hole, so that the reaction time of carbon source gas and the inner wall of the preform adopted in the CVI process is prolonged, and the densification efficiency is improved.
The beneficial effects are that:
(1) The integrated carbon/carbon crucible supporting rod designed by the application greatly reserves the integrity of fibers and ensures the transmission and bearing performance of products.
(2) The prefabricated body of the straight-tube-shaped integrated hollow revolving body structure, which is designed by the application, has a cylindrical shape at the moment, and the corresponding part of the supporting rod cone head can be processed by subsequent machining to obtain supporting rod cone heads with different shapes, so that different application requirements are met, and compared with the existing whole plate cutting, the raw material utilization rate is improved by more than 30%; the prefabricated body of the designed reducing cylinder-shaped integrated hollow revolving body structure has the advantages that the shape of the corresponding part of the taper head of the support rod is a profiling taper, the later cutting processing is avoided, and the utilization rate of raw materials reaches more than 80 percent.
(3) The two central through holes designed in the integrated carbon/carbon crucible supporting rod can effectively reduce weight while guaranteeing the strength of a product, avoid later punching processing, simplify the processing process and reduce the processing difficulty; meanwhile, the design of the hollow structure enlarges the contact area between the carbon source gas and the impregnant in the later densification treatment and the preform, thereby being beneficial to improving the densification efficiency.
(4) In the preparation process of the prefabricated body of the integrated carbon/carbon crucible supporting rod, the pore formed in the needling process provides a channel for diffusion and infiltration of carbon source gas and impregnant into the prefabricated body in the later densification treatment, thereby being beneficial to improving the density uniformity and the densification efficiency; in addition, the carbon fiber brought into the interlayer in the needling process forms a pin structure, so that the connection strength between the circumferential layers can be further enhanced.
(5) The integrated carbon/carbon crucible supporting rod has the advantages of simple structure, easy preparation, less preparation flow, short preparation period, high raw material utilization rate and low cost, and is suitable for batch production.
Drawings
Fig. 1 is a schematic structural view of a preform of a straight cylindrical integrated hollow revolution body structure.
Fig. 2 is a schematic structural view of a preform of a variable diameter cylindrical integrated hollow revolution structure.
Wherein, 1-die-pin body, 2-first central through-hole, 3-die-pin conical head, 4-second central through-hole.
Detailed Description
The present application will be further described with reference to the following detailed description, wherein the processes are conventional, and wherein the starting materials are commercially available from the open market, unless otherwise specified.
Example 1
The utility model provides an integration charcoal/charcoal crucible die-pin, is the integration cavity solid of revolution structure that comprises die-pin body of rod 1 and die-pin conical head 3, and the external diameter of die-pin body of rod 1 part is 140mm and inside along the axial be equipped with the internal diameter be 70 mm's first central through-hole 2, and die-pin conical head 3 part is equipped with the internal diameter along the axial be 15 mm's second central through-hole 4, and specific preparation step is as follows:
(1) Preparing a mandrel with a corresponding shape and size according to the shape and size of the inner molded surface of the integrated hollow rotary body structure, alternately layering the non-woven cloth and the carbon net tire according to the mass ratio of 3:1, continuously needling the vertical layering surface, and circulating the layering-needling operation until reaching the required thickness to form the hollow rotary body structure with the density of 0.40 g/cm 3 A preform of a straight cylindrical integrated hollow revolution structure as shown in fig. 1;
wherein the surface density of the laid fabric is 305g/m 2 The laid cloth is laid in the direction of 0 degree/90 degrees; the surface density of the carbon net tire is 100g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The needling density is 20 needles/cm 2 The interlayer density is 9 layers/cm, and the needling depth is 0.8cm;
(2) Phenolic resin, zinc chloride and ethanol were mixed according to a ratio of 10:1:2.5 mass ratio, and preparing into solidified glue solution; according to 0.8mL/cm 2 Spraying a curing glue solution on the surface of the preform obtained in the step (1), and then placing the preform in a baking oven at 120 ℃ for curing for 2 hours to harden the surface of the preform, thus finishing the pre-curing treatment of the preform;
(3) Loading the pre-cured preform into an isothermal chemical vapor deposition furnace, placing the preform axially parallel to the airflow direction, introducing 90% natural gas and 10% nitrogen in the airflow direction from the first central through hole to the second central through hole, setting the deposition temperature at 1100 ℃ and the deposition pressure at 6kPa to obtain a density of 0.98g/cm 3 Is a first pin blank;
(4) Using furfuryl ketone resin as impregnant, setting the impregnating pressure at 1.5MPa, immersing the first die-pin blank in the impregnant for 10h, carbonizing at 900 deg.C for 4h, and circulating the impregnant impregnating-carbonizing process for 2 periods to obtain the final product with density of 1.57g/cm 3 Is a second pin blank;
(5) Placing the second support rod blank at 1650 ℃ for high-temperature treatment for 6 hours to obtain a third support rod blank;
(6) And (3) machining the third support rod blank to a final size, cutting one end corresponding to the second central hole 4 to finally prepare a tapered support rod conical head 3, and finish turning the rest parts of the third support rod blank to obtain the integrated carbon/carbon crucible support rod.
Example 2
An integrated carbon/carbon crucible supporting rod is an integrated hollow revolving body structure consisting of a supporting rod body 1 and a supporting rod cone head 3, wherein the outer diameter of the supporting rod body 1 is 130mm, a first central through hole 2 with the inner diameter of 60mm is axially arranged in the supporting rod body 1, and a second central through hole 4 with the inner diameter of 10mm is axially arranged in the supporting rod cone head 3, and the concrete preparation steps are as follows:
(1) Preparing a mandrel with a corresponding shape and size according to the shape and size of the inner molded surface of the integrated hollow rotary body structure, alternately layering the non-woven cloth and the carbon net tire according to the mass ratio of 4:1, and continuously needling the vertical layering surfaceThe above layering-needling operation is cycled until the desired thickness is achieved, resulting in a density of 0.50g/cm 3 A preform of a straight cylindrical integrated hollow revolution structure as shown in fig. 1;
wherein the surface density of the laid fabric is 400g/m 2 The laid cloth is laid in the direction of 0 degree/90 degrees; the surface density of the carbon net tire is 100g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The needling density is 38 needles/cm 2 The interlayer density is 12 layers/cm, and the needling depth is 1.0cm;
(2) Phenolic resin, zinc chloride and ethanol were mixed according to a ratio of 10:1:2.5 mass ratio, and preparing into solidified glue solution; according to 1.0mL/cm 2 Spraying a curing glue solution on the surface of the preform obtained in the step (1), and then placing the preform in a baking oven at 120 ℃ for curing for 2 hours to harden the surface of the preform, thus finishing the pre-curing treatment of the preform;
(3) Placing the pre-cured preform in an isothermal chemical vapor deposition furnace, placing the preform axially parallel to the airflow direction, introducing 90% natural gas, 3% propylene and 7% nitrogen in the airflow direction from the first central through hole to the second central through hole, setting the deposition temperature at 1050 ℃ and the deposition pressure at 4kPa to obtain a density of 1.15g/cm 3 Is a first pin blank;
(4) Adopting coal pitch as an impregnant, setting the impregnating pressure to be 2.0MPa, immersing a first support rod blank in the impregnant for 8 hours, then carbonizing at 900 ℃ for 8 hours, and circulating the impregnant impregnating-carbonizing process for 2 periods to obtain the material with the density of 1.48g/cm 3 Is a second pin blank;
(5) Placing the second support rod blank at 2500 ℃ for high-temperature treatment for 2 hours to obtain a third support rod blank;
(6) And (3) machining the third support rod blank to a final size, cutting one end corresponding to the second central hole 4 to finally prepare a tapered support rod conical head 3, and finish turning the rest parts of the third support rod blank to obtain the integrated carbon/carbon crucible support rod.
Example 3
The utility model provides an integration charcoal/charcoal crucible die-pin, is the profile modeling integration cavity solid of revolution structure that comprises die-pin body of rod 1 and die-pin conical head 3, and the external diameter of die-pin body of rod 1 part is 125mm and its inside is equipped with the first central through-hole 2 that the internal diameter is 55mm along the axial, and die-pin conical head 3 part is equipped with the second central through-hole 4 that the internal diameter is 5mm along the axial, and specific preparation steps are as follows:
(1) Preparing a mandrel with a corresponding shape and size according to the shape and size of the inner molded surface of the integrated hollow rotary body structure, alternately layering the non-woven cloth and the carbon net tire according to the mass ratio of 5:1, continuously needling the vertically layered surface, preparing a supporting rod cone head 3 with the taper of 45 degrees by changing the laying size of the net tire, and circulating the layering-needling operation until the required thickness is reached, thereby forming the hollow rotary body structure with the density of 0.55g/cm 3 A preform of a variable diameter cylindrical integrated hollow revolution structure as shown in fig. 2;
wherein the surface density of the laid fabric is 409g/m 2 The laid cloth is laid in the direction of 0 degree/90 degrees; the surface density of the carbon net tire is 82g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Needling density of 28 needles/cm 2 The interlayer density is 15 layers/cm, and the needling depth is 0.8cm;
(2) Phenolic resin, zinc chloride and ethanol were mixed according to a ratio of 10:1:2.5 mass ratio, and preparing into solidified glue solution; according to 1.0mL/cm 2 Spraying a curing glue solution on the surface of the preform obtained in the step (1), and then placing the preform in a 100 ℃ oven for curing for 5 hours to harden the surface of the preform, thereby completing the pre-curing treatment of the preform;
(3) Placing the pre-cured preform in an isothermal chemical vapor deposition furnace, placing the preform axially parallel to the airflow direction, introducing 80% natural gas, 13% propane and 7% nitrogen in the airflow direction from the first central through hole to the second central through hole, setting the deposition temperature at 1050 ℃ and the deposition pressure at 6kPa to obtain a density of 1.28g/cm 3 Is a first pin blank;
(4) Adopting coal pitch as an impregnant, setting the impregnating pressure to be 2.0MPa, immersing a first support rod blank in the impregnant for 8 hours, then carbonizing at 900 ℃ for 8 hours, and circulating the impregnant impregnating-carbonizing process for 2 periods to obtain the material with the density of 1.60g/cm 3 Is a second pin blank;
(5) Placing the second support rod blank at 2300 ℃ for high-temperature treatment for 4 hours to obtain a third support rod blank;
(6) And (5) performing final sizing machining on the third support rod blank to obtain the integrated carbon/carbon crucible support rod.
Comparative example 1
(1) Alternately laying the laid cloth and the carbon net tire according to the mass ratio of 3:1, needling in the direction perpendicular to the laying direction, and circulating the laying-needling operation until the required thickness is reached, thereby forming the composite material with the length, width and thickness of 1250, mm, 270, mm, 130, mm and the density of 0.45g/cm 3 Is a plate-like preform of (a);
wherein the surface density of the laid fabric is 305g/m 2 The laid cloth is laid in the direction of 0 degree/90 degrees; the surface density of the carbon net tire is 100g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The needling density is 20 needles/cm 2 The interlayer density is 9 layers/cm, and the needling depth is 1.0cm;
(2) Phenolic resin, zinc chloride and ethanol were mixed according to a ratio of 10:1:2.5 mass ratio, and preparing into solidified glue solution; according to 1.5mL/cm 2 Spraying a curing glue solution on the surface of the preform obtained in the step (1), and then placing the preform in a baking oven at 120 ℃ for curing for 6 hours to harden the surface of the preform, thus finishing the pre-curing treatment of the preform;
(3) Placing the pre-cured preform in an isothermal chemical vapor deposition furnace, placing the preform axially parallel to the airflow direction, introducing 90% natural gas and 10% nitrogen in the airflow direction from the first central through hole to the second central through hole, setting the deposition temperature at 1100 ℃ and the deposition pressure at 6kPa to obtain a density of 1.1g/cm 3 Is a first pin blank;
(4) Cutting the first support rod blank, cutting the first support rod blank into two parts along the width, then carrying out impregnant impregnation-carbonization densification treatment, specifically adopting coal asphalt as impregnant, setting the impregnation pressure to be 1.5MPa, impregnating the first support rod blank in the impregnant for 8 hours, then carrying out carbonization treatment at 900 ℃ for 8 hours, and circulating the resin impregnation-carbonization process for 2 periods to obtain the support rod with the density of 1.43g/cm 3 Is a second pin blank;
(5) Coring and cutting the second support rod blank to obtain a third support rod blank;
(6) Placing the third support rod blank at 2300 ℃ for high-temperature treatment for 4 hours to obtain a fourth support rod blank;
(7) Continuously carrying out impregnant impregnation-carbonization densification treatment on the fourth support rod blank, specifically, adopting coal pitch as impregnant, setting the impregnation pressure to be 1.5MPa, immersing the fourth support rod blank in the impregnant for 8 hours, then carrying out carbonization treatment at 900 ℃ for 8 hours, and recycling the impregnant impregnation-carbonization process for 2 periods to obtain the support rod blank with the density of 1.63g/cm 3 A fifth pin blank;
(8) Placing the fifth die-pin blank at 2300 ℃ for high-temperature treatment for 4 hours to obtain a sixth die-pin blank;
(9) And (5) performing final sizing machining on the sixth support rod blank to obtain the carbon/carbon crucible support rod.
The crucible support rods prepared in examples 1 to 3 and comparative example 1 were tested separately, and the material parameter test method adopted was as follows: (1) Density test: adopting a volume density test method; (2) density uniformity test sample and calculation method: slicing the parts of the support rod body 1 and the support rod cone head 3 after the crucible support rod is subjected to high-temperature treatment, wherein the thickness of a slice is 10mm, and the total number of the slices is 2; taking 6 samples near the outer surface, the middle and the near inner surface along the radial direction of the thin sheet, wherein the sizes of the samples are density samples with the length of 10mm multiplied by the width of 10mm multiplied by the thickness of 2 mm, and the total number of the samples is 12 for each crucible supporting rod, and calculating the relative standard value (RSD) of the 12 samples; density uniformity= (1-RSD) ×100%; (3) Mechanical test, adopting a universal tester to test compression performance, and selecting standard GB/T5350-2005 for test samples and tests; (4) raw material utilization rate calculation method: and the finished carbon/carbon crucible supporting rod and the supporting rod blank volume after the high-temperature treatment of different embodiments are read by CAD drawing software, wherein the raw material utilization rate is = (supporting rod blank volume-supporting rod finished product volume)/supporting rod blank volume multiplied by 100%.
TABLE 1
| Density (g/cm 3) | Density uniformity | Compressive Strength (MPa) | Raw material utilization rate | |
| Comparative example 1 | 1.63 | 65% | 130.6 | 48% |
| Example 1 | 1.57 | 82% | 131.5 | 85% |
| Example 2 | 1.48 | 85% | 124.8 | 87% |
| Example 3 | 1.60 | 92% | 122.9 | 92% |
As can be seen from the test results of Table 1, the present application is designed withThe two-stage hollow structure of the straight cylinder-shaped and variable diameter cylinder-shaped support rod prefabricated body, wherein the part corresponding to the second center through hole in the straight cylinder-shaped support rod prefabricated body can meet the processing of crucible support rod conical heads with different shapes, and compared with the existing whole plate cutting, the raw material utilization rate is improved by 37%; the other reducing cylindrical support rod preform avoids later cutting processing, and the utilization rate of raw materials reaches 92 percent. And the density of the prepared carbon/carbon crucible supporting rod can reach 1.48g/cm 3 The compression strength reaches more than 120 MPa.
In summary, the above embodiments are only preferred embodiments of the present application, and are not intended to limit the scope of the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (9)
1. An integrated carbon/carbon crucible supporting rod which is characterized in that: the integrated hollow revolution solid structure consists of a support rod body and a support rod cone head, wherein a support rod body part is axially provided with a first central through hole, a support rod cone head part is axially provided with a second central through hole, and the diameter of the second central through hole is smaller than that of the first central through hole;
the integrated hollow revolving body structure is formed by alternately layering and needling a carbon fiber woven cloth and a carbon net tire to form a prefabricated body of the integrated hollow revolving body structure, and then performing carbon densification and machining treatment.
2. The integrated char/char crucible pin according to claim 1, wherein: the diameter of the first central through hole is 50-75 mm, the diameter of the second central through hole is 5-15 mm, and the outer diameter of the stopper rod body part is 125-140 mm.
3. The integrated char/char crucible pin according to claim 1, wherein: the density of the prefabricated body of the integrated hollow revolving body structure is 0.35-0.55 g/cm 3 The density of the compact carbon is 1.45-1.75 g/cm 3 。
4. An integrated char/char crucible pin according to any one of claims 1 to 3, wherein: the specific preparation steps of the integrated carbon/carbon crucible supporting rod are as follows:
preparing a mandrel with a corresponding shape and size according to the shape and size of the inner molded surface of the integrated hollow revolving body structure, alternately layering carbon fiber woven cloth and a carbon net tire according to a required proportion, continuously needling the layer vertically, circulating the layering-needling operation to obtain a prefabricated body of the integrated hollow revolving body structure, performing carbon densification treatment on the prefabricated body to form a support rod blank, and performing machining on the support rod blank to obtain the integrated carbon/carbon crucible support rod with a required size.
5. The integrated char/char crucible pin according to claim 4, wherein: the surface density of the carbon fiber woven cloth is 200-420 g/m 2 The surface density of the carbon net tire is 30-120 g/m 2 The mass ratio of the carbon fiber woven cloth to the carbon net tire in the preform is 3:1-5:1, and the needling density is 20-40 needles/cm 2 The interlayer density is 7-15 layers/cm, and the needling depth is 0.3-1 cm.
6. The integrated char/char crucible pin according to claim 4, wherein: the concrete steps of the carbon densification treatment of the preform are as follows:
firstly, pre-curing the surface of a preform, spraying a curing glue solution on the surface of the preform, and then placing the preform in 60-120 o C, curing for 2-6 hours to finish the pre-curing treatment of the preform; for the pre-cured preform, firstly adopting a chemical vapor infiltration process to deposit pyrolytic carbon for densification, then adopting an impregnant impregnation-carbonization process to form resin carbon for continuous densification, and finally, carrying out protective atmosphere and 1600-2500 ℃ to obtain the resin carbon o C, performing high-temperature treatment in a furnace chamber for 2-6 hours;
wherein the curing glue solution is prepared from resin, a curing agent and ethanol according to (8-12): (0.8 to 1.5): (2-3) a resin including but not limited to phenolic resin, a curing agent including but not limited to zinc chloride,Toluene sulfonic acid or triethylene tetramine, and the surface spraying and curing glue liquid amount of the prefabricated body is 0.5-1.8 mL/cm 2 。
7. The integrated char/char crucible pin of claim 6, wherein: for a density of 0.35-0.55 g/cm 3 Firstly, adopting a chemical vapor infiltration process to deposit pyrolytic carbon so as to densify the pyrolytic carbon to 0.8-1.3 g/cm 3 Then, resin carbon is formed by adopting an impregnant impregnation-carbonization process to continuously densify to 1.45-1.75 g/cm 3 。
8. The integrated char/char crucible pin of claim 6, wherein: the carbon source gas adopted in the chemical vapor infiltration process is at least one of natural gas and olefin with 1-4 carbon atoms; the impregnant used in the impregnant impregnation-carbonization process is furan resin, furfuryl ketone resin or coal pitch.
9. The integrated char/char crucible pin according to claim 4, wherein: when the preform is placed in a chemical vapor deposition furnace for pyrolytic carbon deposition, the axial direction of the preform is parallel to the flow direction of the air flow, and the flow direction of the air flow is the direction from the first central through hole to the second central through hole.
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