CN111187076A - Ultra-high temperature adhesive and preparation method thereof - Google Patents

Ultra-high temperature adhesive and preparation method thereof Download PDF

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CN111187076A
CN111187076A CN202010067896.0A CN202010067896A CN111187076A CN 111187076 A CN111187076 A CN 111187076A CN 202010067896 A CN202010067896 A CN 202010067896A CN 111187076 A CN111187076 A CN 111187076A
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adhesive
powder
carbon
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high temperature
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CN111187076B (en
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史萌
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Yantai Kaibo Composite Material Technology Co ltd
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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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303—Inorganic additives
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63472—Condensation polymers of aldehydes or ketones
    • C04B35/63476—Phenol-formaldehyde condensation polymers
    • 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
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
    • 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
    • C04B2235/02—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
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C04B2235/424—Carbon black
    • 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
    • C04B2235/02—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
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon
    • 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
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Composite Materials (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses an ultrahigh-temperature adhesive and a preparation method thereof. The key point is that the components of the adhesive comprise the following components in percentage by weight: 40-60% of liquid phenolic resin, 20-40% of carbon felt powder, 5-20% of carbon black powder, 10-25% of silicon powder, 5-15% of aluminum powder, 0.1-0.5% of coupling agent, 0.1-0.6% of n-ethane and 10-20% of short carbon fiber. The invention has excellent fusion performance, ensures that the thermal internal stress of the large carbon/carbon composite material member is extremely small, has high connection strength, and simultaneously, the adhesive layer formed after high-temperature treatment also has excellent mechanical property.

Description

Ultra-high temperature adhesive and preparation method thereof
The technical field is as follows:
the invention relates to an adhesive, in particular to an ultrahigh temperature resistant adhesive for bonding carbon/carbon composite materials.
Background art:
the C/C composite material is the most advanced high-temperature structure/function composite material in the present generation, has excellent high-temperature mechanical properties and thermophysical properties such as light specific gravity, heat resistance, high strength, ablation resistance and the like, and is widely applied to the aerospace field. But is limited to small components with simple shapes and medium-high temperatures. However, with the rapid development of aerospace technology, ultrahigh temperature (> 2200 ℃) is urgently needed, and a large-sized C/C component with a complex shape is urgently needed. For example, new strategic missiles in the future require C/C components to meet ultra-high temperature (> 2200 ℃) service conditions. Meanwhile, the development of space technology needs large-scale and ultra-stable C/C components to meet the requirement of long-term use in space heat exchange environment. With the development of engineering technology, the civil fields of metallurgy, machinery, chemical industry and the like have urgent needs for C/C composite materials. The existing production process of the C/C composite material cannot meet the requirements of the aerospace field and the modern industry on ultrahigh-temperature large-scale complex C/C components. Therefore, the preparation method for solving the problem of the preparation of the ultrahigh-temperature large-scale complex C/C component becomes an important subject for meeting the urgent need of aerospace and modern industry on the C/C composite material.
The invention content is as follows:
the invention aims to disclose an ultra-high temperature adhesive for preparing a large-scale carbon/carbon component with a complex structure and a preparation method thereof.
The technical solution for realizing the invention is as follows: the ultrahigh-temperature adhesive comprises the following components in percentage by weight:
Figure BSA0000201081110000021
the ultrahigh-temperature adhesive comprises the following components in percentage by weight:
Figure BSA0000201081110000022
the particle size of the carbon felt powder is 50-100 meshes, the particle size of the carbon black powder is 500 meshes, the particle size of the silicon powder is 350 meshes, the particle size of the aluminum powder is 1600 meshes, and the length of the short carbon fiber filament is 3-10 mm.
The preparation method of the ultra-high temperature adhesive comprises the following steps: sequentially adding carbon felt powder, carbon black powder, silicon powder, aluminum powder, a coupling agent, n-ethane and short carbon fiber into liquid phenolic resin, adding the next component after adding one component and stirring uniformly, finally adding the short carbon fiber, stirring for 10-25 minutes, grinding for 20-40 minutes in a ball mill, putting into a closed container, and standing for 12-24 hours to obtain the adhesive.
The ultrahigh-temperature adhesive disclosed by the invention has excellent fusion with a carbon/carbon composite material prefabricated body, a structural layer is penetrated between adhesive layer carbon/carbon composite material members after high-temperature treatment, the densities of the adhesive layer carbon/carbon composite material members are basically equivalent, the thermal internal stress of the large carbon/carbon composite material members is extremely small, the connection strength is high, the adhesive layer formed after high-temperature treatment also has excellent mechanical properties, and particularly, the adhesive is subjected to high-temperature treatment at the temperature of more than 2500 ℃.
The specific implementation mode is as follows:
the following detailed description of the present invention is given in detail, and it should be noted that the description of the embodiments of the present invention is made for the purpose of facilitating a comprehensive understanding of the technical contents of the present invention, and should not be construed as limiting the scope of the claims of the present invention.
The technical solution of the specific embodiment of the ultra-high temperature adhesive is as follows: the adhesive comprises the following components in percentage by weight: 40-60% of liquid phenolic resin, 20-40% of carbon felt powder, 5-20% of carbon black powder, 10-25% of silicon powder, 5-15% of aluminum powder, 0.1-0.5% of coupling agent, 0.1-0.6% of n-ethane and 10-20% of short carbon fiber. The adhesive is placed between the contact parts of two carbon/carbon composite preforms when in use, and the two carbon/carbon composite preforms are bonded to form a preform with a larger size, or three or more carbon/carbon composite preforms form a preform with a large size and a complex structure. In order to achieve the fusion and combination, the adhesive contains various carbon materials of different types, and the various carbon materials of different types are combined with the short carbon fiber in the adhesive and also combined with the carbon material in the prefabricated body, and meanwhile, after the adhesive is bonded with the prefabricated body, the adhesive also penetrates into the inner part of the surface of the prefabricated body, and the different carbon materials also react with silicon powder and aluminum powder to generate silicon carbide and metal ceramics with complex structures; the adhesive is sintered with the preform into a whole after high-temperature treatment, and the density and the expansion coefficient of the sintered adhesive layer are close to those of the sintered preform due to the specific formula and the specific proportion, so that when the carbon/carbon composite material member with a large-scale complex structure is used at a high temperature, the thermal stress caused by the difference of the expansion coefficients and the micro cracks generated in the member can not be generated.
In order to further improve the bonding performance of the adhesive and the carbon/carbon composite material member, the adhesive comprises the following components in percentage by weight: 45-55% of liquid phenolic resin, 20-32% of carbon felt powder, 5-15% of carbon black powder, 6-15% of silicon powder, 8-12% of aluminum powder, 0.3-0.4% of coupling agent, 0.3-0.4% of n-ethane and 12-16% of short carbon fiber. The optimization of the proportion of the adhesive enables the adhesive to have better performance of penetrating a prefabricated body and better bonding capability, and further improves the mechanical property of the adhesive, and tests show that the mechanical property of the adhesive can achieve that the interlaminar shear strength is more than or equal to 12MPa, the elastic modulus is more than or equal to 20GPa, the compressive strength is more than or equal to 150MPa, and the tensile strength is more than or equal to 60MPa after the adhesive is treated at high temperature.
In order to further improve the performance of the adhesive, the granularity of carbon felt powder in the adhesive is preferably 50-100 meshes, the granularity of carbon black powder is 500 meshes, the granularity of silicon powder is 350 meshes, the granularity of aluminum powder is 1600 meshes, and the length of short carbon fiber filaments is 3-10 mm; the optimization of the component particle size in the adhesive is obtained based on a large number of tests and detections, the matching of the component particle sizes enables the mixed adhesive to have better density, that is, the component particles are embedded with each other to achieve better mutual embedding of the space main bodies, so that the adhesive achieves the density as high as possible, and the mutual matching of the component particles of the adhesive achieves the space main bodies as high as possible, so that the reaction speed and crystallization during high-temperature sintering are also beneficial.
The composition of the adhesive of the present invention has been described above, and the preparation method of the adhesive is: sequentially adding carbon felt powder, carbon black powder, silicon powder, aluminum powder, a coupling agent, n-ethane and short carbon fiber into liquid phenolic resin, adding the next component after adding one component and stirring uniformly, finally adding the short carbon fiber, stirring for 10-25 minutes, grinding for 20-40 minutes in a ball mill, putting into a closed container, and standing for 12-24 hours to obtain the adhesive. Through the processes of sequentially adding the components, repeatedly stirring for many times and finally ball milling, the components of the adhesive are fully mixed, the optimal space of the particles of the components is embedded, the space gap among the particles of the components of the adhesive is minimized, and the compactness of the adhesive is realized as far as possible.
After a plurality of carbon/carbon composite material prefabricated bodies are bonded into a large prefabricated body with a larger size and a complex structure by the adhesive, the large prefabricated body is placed into a high-temperature furnace and subjected to high-temperature treatment to obtain a carbon/carbon composite material member.
The components of the adhesive are purchased from the market, the liquid phenolic resin is under the trade name of PF-51, the coupling agent is under the trade name of KH-792, the n-ethane is industrially pure, and the carbon black powder is industrially pure.

Claims (4)

1. The ultra-high temperature adhesive is characterized by comprising the following components in percentage by weight:
Figure FSA0000201081100000011
2. the ultra-high temperature adhesive according to claim 1, characterized in that the components of the adhesive are, by weight:
Figure FSA0000201081100000012
3. the ultra-high temperature adhesive according to claim 1 or 2, wherein the particle size of the carbon felt powder is 50-100 meshes, the particle size of the carbon black powder is 500 meshes, the particle size of the silicon powder is 350 meshes, the particle size of the aluminum powder is 1600 meshes, and the length of the short carbon fiber filament is 3-10 mm.
4. The method for preparing the ultra-high temperature adhesive according to claim 1, 2 or 3, wherein the method for preparing the adhesive comprises the following steps: sequentially adding carbon felt powder, carbon black powder, silicon powder, aluminum powder, a coupling agent, n-ethane and short carbon fiber into liquid phenolic resin, adding the next component after adding one component and stirring uniformly, finally adding the short carbon fiber, stirring for 10-25 minutes, grinding for 20-40 minutes in a ball mill, putting into a closed container, and standing for 12-24 hours to obtain the adhesive.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115139590A (en) * 2022-08-01 2022-10-04 江苏中矿大正表面工程技术有限公司 Preparation method of aerogel fiber composite board for bridge fire resistance

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101157566A (en) * 2007-09-13 2008-04-09 北京航空航天大学 Deep regenerative restoring technique for charcoal/charcoal composite material
CN101486588A (en) * 2009-03-04 2009-07-22 中南大学 Preparation of carbon fiber reinforced carbon-silicon carbide double matrix friction material
CN104139572A (en) * 2014-07-21 2014-11-12 烟台凯泊复合材料科技有限公司 Preparation process of carbon/ceramic-graphite composite material and carbon/ceramic-graphite composite material prepared through preparation process
CN104342079A (en) * 2013-08-01 2015-02-11 甘肃郝氏炭纤维有限公司 Preparation method and application method of high-temperature bonding agent used for bonding carbon felts
CN104974697A (en) * 2015-07-21 2015-10-14 中国科学院上海应用物理研究所 Carbon/carbon composite material binder, bonding method and carbon/carbon composite material member
US20160176764A1 (en) * 2014-09-17 2016-06-23 Baker Hughes Incorporated Carbon composites

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101157566A (en) * 2007-09-13 2008-04-09 北京航空航天大学 Deep regenerative restoring technique for charcoal/charcoal composite material
CN101486588A (en) * 2009-03-04 2009-07-22 中南大学 Preparation of carbon fiber reinforced carbon-silicon carbide double matrix friction material
CN104342079A (en) * 2013-08-01 2015-02-11 甘肃郝氏炭纤维有限公司 Preparation method and application method of high-temperature bonding agent used for bonding carbon felts
CN104139572A (en) * 2014-07-21 2014-11-12 烟台凯泊复合材料科技有限公司 Preparation process of carbon/ceramic-graphite composite material and carbon/ceramic-graphite composite material prepared through preparation process
US20160176764A1 (en) * 2014-09-17 2016-06-23 Baker Hughes Incorporated Carbon composites
CN104974697A (en) * 2015-07-21 2015-10-14 中国科学院上海应用物理研究所 Carbon/carbon composite material binder, bonding method and carbon/carbon composite material member

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115139590A (en) * 2022-08-01 2022-10-04 江苏中矿大正表面工程技术有限公司 Preparation method of aerogel fiber composite board for bridge fire resistance

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