CN113881354A - Bonding repair method for carbon fiber reinforced carbon-based composite material, adhesive used by bonding repair method and preparation method of adhesive - Google Patents

Bonding repair method for carbon fiber reinforced carbon-based composite material, adhesive used by bonding repair method and preparation method of adhesive Download PDF

Info

Publication number
CN113881354A
CN113881354A CN202111151677.1A CN202111151677A CN113881354A CN 113881354 A CN113881354 A CN 113881354A CN 202111151677 A CN202111151677 A CN 202111151677A CN 113881354 A CN113881354 A CN 113881354A
Authority
CN
China
Prior art keywords
powder
adhesive
meshes
organic silicon
silicon resin
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202111151677.1A
Other languages
Chinese (zh)
Other versions
CN113881354B (en
Inventor
罗瑞盈
罗浩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hubei Ruiyu Kongtian High Tech Co ltd
Original Assignee
Hubei Ruiyu Kongtian High Tech Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hubei Ruiyu Kongtian High Tech Co ltd filed Critical Hubei Ruiyu Kongtian High Tech Co ltd
Priority to CN202111151677.1A priority Critical patent/CN113881354B/en
Publication of CN113881354A publication Critical patent/CN113881354A/en
Application granted granted Critical
Publication of CN113881354B publication Critical patent/CN113881354B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • 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
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83Carbon fibres in a carbon matrix
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/06Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving heating of the applied adhesive
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/085Copper
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc

Landscapes

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

Abstract

The repairing method comprises the following steps of stirring and mixing 10-15 wt.% of diamond powder, 12-15 wt.% of zinc oxide powder, 6-12 wt.% of copper powder, 10-15 wt.% of titanium powder, 32-37 wt.% of low-melting-point glass powder and 20-25 wt.% of organic silicon resin solution to complete preparation of the adhesive; then uniformly coating the adhesive on the surface CfAdhering the surface of the bonding surface of the/C composite material, heating to 250 ℃ in a blast oven at the speed of 5 ℃/hour, and then preserving heat for 2 hoursCuring the adhesive, wherein the thickness of the adhesive layer is controlled to be 0.08-0.3 mu m by applying pressure to the material during curing; finally, the temperature is raised to 1200 ℃ at the speed of 100 ℃/hour under the vacuum environment of-0.1 MPa, and then the temperature is preserved for 2 hours to finish the carbonization of the adhesive. The adhesive provided by the invention has excellent room-temperature and high-temperature adhesive strength and thermal shock resistance, the room-temperature thermal conductivity of the material after adhesive repair is higher than 22.31W/(m.k), and the coefficient of thermal conductivity is higher than CfThe composite material has wide practical value and application prospect in the field of the/C composite material.

Description

Bonding repair method for carbon fiber reinforced carbon-based composite material, adhesive used by bonding repair method and preparation method of adhesive
Technical Field
The invention belongs to the technical field of carbon/carbon composite materials, and particularly relates to a carbon fiber reinforced carbon-based (C)f/C) a method for repairing the composite material by bonding.
Background
The carbon/carbon composite material has the characteristics of low density, high heat capacity, small thermal deformation, good ablation resistance, excellent room temperature and high temperature mechanical properties and the like, and is widely applied to high temperature parts such as advanced brake systems, thermal protection systems, space shuttles, rocket engines and the like. However, due to CfThe preparation period of the/C composite material is long, the cost is high, and the process is complex, so that the composite material is used for treating C which is damaged or reaches the service lifefthe/C composite material component is necessary to be repaired and reused. The traditional repair technology (riveting, welding or mechanical connection) easily causes damage to the material, so that the strength of the material is reduced, and meanwhile, the weight of the used repair material is large, so that the effective load is reduced. The adhesive bonding is a technology for connecting the surfaces of homogeneous or heterogeneous objects together, has the characteristics of continuous stress distribution, light weight and the like, can effectively avoid the problems of the traditional mechanical connection method, and is very effective CfA method for repairing/C composite material.
CfThe high temperature application field of the/C composite material determines that the adhesive has good heat resistance and toughness to meet the structural adhesive performance requirement, and also has excellent thermal conductivity to meet the heat transfer requirement. C has been developed so farfThe adhesives for the/C composite materials are mainly divided into organic and inorganic adhesives. The organic adhesive forms a carbon bonding layer or a silicon bonding layer after high-temperature heat treatment, has higher bonding strength at room temperature and low temperature, but has certain limitation, low fracture toughness and poor thermal shock resistance due to a single-phase structure. The inorganic adhesive can be reacted with CfThe C/C matrix reacts to form a carbide bonding layer with higher bonding strength, the temperature resistance is excellent, but the ceramic layer and the C arefThe thermal expansion coefficient and the elastic modulus of the/C composite material are greatly mismatched, and residual stress is generated in the cooling process at the preparation temperature, so that the bonding is strongThe degree decreases. In addition, the heat conductivity of the two adhesives is rarely reported. Therefore, the conventional adhesive hardly satisfies CfThe bonding repair requirement of the/C composite material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a bonding repair method of a carbon fiber reinforced carbon-based composite material, a used adhesive and a preparation method thereof.
The above purpose can be realized by the following technical scheme:
in a first aspect, the invention provides a bonding repair method for a carbon fiber reinforced carbon-based composite material, which comprises the following steps:
(1) adhesive preparation:
at the room temperature of 25 ℃, firstly, adding 10-15 wt.% of diamond powder, 12-15 wt.% of zinc oxide powder, 6-12 wt.% of copper powder, 10-15 wt.% of titanium powder and 32-37 wt.% of low-melting-point glass powder into a mortar, mixing and grinding for 30 minutes to prepare mixed powder;
adding the mixed powder and 20-25 wt.% of organic silicon resin solution into a container (beaker) simultaneously, and mechanically stirring for 1 hour to complete the preparation of the adhesive; the organic silicon resin solution is prepared by stirring and mixing organic silicon resin and dimethylbenzene, and the viscosity is 65-100 cps;
(2) curing of the adhesive:
uniformly coating the prepared adhesive on the surfaces of two bonding surfaces of a material to be repaired, then bonding the two surfaces, controlling the pressure applied to the surface of the material in the atmospheric environment, controlling the thickness of the adhesive layer to be 0.08-0.3 mu m, then placing the material into a blast oven, heating to 250 ℃ at the speed of 5 ℃/h, preserving the temperature for 2 hours to complete the curing of the adhesive, and controlling the thickness of the adhesive layer to be 0.08-0.3 mu m by applying pressure to the material during the whole curing period;
(3) carbonization of the adhesive:
and (3) putting the cured material into high-temperature vacuum equipment, heating to 1200 ℃ at the speed of 100 ℃/hour under the vacuum environment of-0.1 MPa, and then preserving heat for 2 hours to finish the carbonization of the adhesive.
The granularity of the diamond powder in the step (1) is 460-650 meshes; the granularity of the zinc oxide powder is 270-325 meshes; the mesh number of the copper powder is 200-325 meshes; the mesh number of the titanium powder is 200-325 meshes; the low-melting point glass powder has a mesh number of 1500-3000 meshes and a melting point of 700-750 ℃.
The organic silicon resin is polymethylphenylsiloxane; the purity of the xylene was analytical grade.
In a second aspect, the present invention provides a high thermal conductivity and high temperature resistant adhesive, which is prepared by the following method:
at the room temperature of 25 ℃, firstly, adding 10-15 wt.% of diamond powder, 12-15 wt.% of zinc oxide powder, 6-12 wt.% of copper powder, 10-15 wt.% of titanium powder and 32-37 wt.% of low-melting-point glass powder into a mortar, mixing and grinding for 30 minutes to prepare mixed powder;
adding the mixed powder and 20-25 wt.% of organic silicon resin solution into a container (beaker) simultaneously, and mechanically stirring for 1 hour to complete the preparation of the adhesive; the organic silicon resin solution is prepared by stirring and mixing organic silicon resin and dimethylbenzene, and the viscosity of the organic silicon resin solution is 65-100 cps.
The particle size of the diamond powder is 460-650 meshes; the granularity of the zinc oxide powder is 270-325 meshes; the mesh number of the copper powder is 200-325 meshes; the mesh number of the titanium powder is 200-325 meshes; the low-melting point glass powder has a mesh number of 1500-3000 meshes and a melting point of 700-750 ℃.
The organic silicon resin is polymethylphenylsiloxane; the purity of the xylene was analytical grade.
The adhesive has excellent room temperature and high temperature adhesive strength and thermal shock resistance, and the heat conductivity coefficient of the material after adhesive repair is higher than 22.31W/(m.k) at room temperature, and the coefficient is CfThe composite material has wide practical value and application prospect in the field of the/C composite material.
In a third aspect, the invention provides a preparation method of a high-thermal-conductivity high-temperature-resistant adhesive, which comprises the following steps:
at the room temperature of 25 ℃, firstly, adding 10-15 wt.% of diamond powder, 12-15 wt.% of zinc oxide powder, 6-12 wt.% of copper powder, 10-15 wt.% of titanium powder and 32-37 wt.% of low-melting-point glass powder into a mortar, mixing and grinding for 30 minutes to prepare mixed powder;
adding the mixed powder and 20-25 wt.% of organic silicon resin solution into a container (beaker) simultaneously, and mechanically stirring for 1 hour to complete the preparation of the adhesive; the organic silicon resin solution is prepared by stirring and mixing organic silicon resin and dimethylbenzene, and the viscosity of the organic silicon resin solution is 65-100 cps.
The particle size of the diamond powder is 460-650 meshes; the granularity of the zinc oxide powder is 270-325 meshes; the mesh number of the copper powder is 200-325 meshes; the mesh number of the titanium powder is 200-325 meshes; the low-melting point glass powder has a mesh number of 1500-3000 meshes and a melting point of 700-750 ℃.
The organic silicon resin is polymethylphenylsiloxane; the purity of the xylene was analytical grade.
In a fourth aspect, the invention provides an application of the high-thermal-conductivity high-temperature-resistant adhesive in repairing a carbon fiber reinforced carbon-based composite material.
The high-heat-conductivity high-temperature-resistant adhesive has the advantages and positive effects that the adhesive not only has good room-temperature and high-temperature adhesive strength, but also has excellent heat-conducting property, and is particularly shown in the following steps:
1) the carbon fiber reinforced carbon base (C) bonded and repaired by the methodfThe room-temperature bonding strength of the/C) composite material is 11.6-13.0 MPa, and the failure mode is that the body is broken;
2) c bonded by the inventionfAfter the/C composite material is subjected to accumulated treatment for 50 hours at 300 ℃, 700 ℃, 1100 ℃ and 1500 ℃ respectively, no defects such as pores, cracks and the like are found at the adhesive layer, the adhesive strength is 11.6-13.0 MPa, the adhesive strength is not attenuated compared with the adhesive strength at room temperature, and the failure mode is still that the body material is broken;
3) c bonded by the inventionfThe adhesive sample of the/C composite material is not cracked after accumulated treatment for 20 hours at 1800 ℃, and the adhesive strength is 6.8-7.5 MPa, which shows that the adhesiveThe heat resistance is excellent;
4) c bonded by the inventionfThe thermal conductivity coefficients of the/C composite material at room temperature (25 ℃), 700 ℃ and 1000 ℃ are respectively 22.31-25.35W/(m.k), 20.86-21.56W/(m.k) and 17.68-19.15W/(m.k), and CfThe thermal conductivity of the/C composite material is equivalent.
Drawings
FIG. 1 is a flow chart of the bond repair method of the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
Example 1:
the embodiment provides a bonding repair method for a carbon fiber reinforced carbon-based composite material, which comprises the following steps:
(1) at the room temperature of 25 ℃, 10 wt.% of diamond powder, 12wt.% of zinc oxide powder, 10 wt.% of copper powder, 15wt.% of titanium powder and 33 wt.% of low-melting glass powder are added into a mortar and ground for 30 minutes to prepare mixed powder, then the organic silicon resin is stirred and mixed with a proper amount of xylene to prepare an organic silicon resin solution with the viscosity of 80cps, and finally the 20 wt.% organic silicon resin solution and the mixed powder are added into a beaker at the same time and mechanically stirred for 1 hour. Wherein the particle size of the diamond powder is 460 meshes; the granularity of the zinc oxide powder is 325 meshes; the mesh number of the copper powder is 325 meshes; the mesh number of the titanium powder is 325 meshes; the mesh number of the low-melting-point glass powder is 1500-3000 meshes, and the melting point is 700-750 ℃; the organic silicon resin is polymethylphenylsiloxane; the xylene purity was analytical.
(2) Uniformly coating the adhesive on the surfaces of the two bonding surfaces, then bonding the two surfaces, controlling the pressure applied to the surface of the material under the atmospheric environment to control the thickness of the adhesive layer to be 0.12 mu m, then placing the material into a blast oven, heating to 250 ℃ at the speed of 5 ℃/h, and then preserving heat for 2 hours.
(3) And (3) putting the cured material into high-temperature vacuum equipment, heating to 1200 ℃ at the speed of 100 ℃/hour under the vacuum environment of-0.1 MPa, and then preserving heat for 2 hours.
Using the adhesive of example 1C after grafting repairfthe/C composite material:
the room-temperature bonding strength is 12.5MPa, and the failure mode is Cfthe/C composite material body is broken;
after accumulated treatment is carried out for 50 hours at 300 ℃, 700 ℃, 1100 ℃ and 1500 ℃, no defects such as pores, cracks and the like are found at the glue layer, the bonding strength is 12.6MPa, the bonding strength is not attenuated compared with the bonding strength at room temperature, and the failure mode is that the body material is still broken;
the bonded sample does not crack after accumulated treatment for 20 hours at 1800 ℃, the bonding strength is 7.2MPa, and the bonded sample has excellent heat resistance;
thermal conductivities at room temperature (25 ℃), 700 ℃ and 1000 ℃ of 23.54W/(m.k), 21.23W/(m.k) and 18.56W/(m.k), respectively, and CfThe thermal conductivity of the/C composite material is equivalent.
The test method of the bonding performance is as follows:
room temperature adhesive strength: the shear performance of a sample is tested by adopting a short beam method on a universal electronic testing machine to measure;
heat resistance: placing the bonded sample into a tube furnace, preserving heat for a corresponding time at a test temperature point under the protection of argon, and then cooling the sample to room temperature for bonding performance test;
coefficient of thermal conductivity: the bonded sample was placed in an LFA427HT laser thermal conductivity meter manufactured by KASS Germany, and the thermal conductivity was measured under vacuum.
Example 2:
the embodiment provides a bonding repair method for a carbon fiber reinforced carbon-based composite material, which comprises the following steps:
(1) at the room temperature of 25 ℃, 10 wt.% of diamond powder, 10 wt.% of zinc oxide powder, 10 wt.% of copper powder, 10 wt.% of titanium powder and 35 wt.% of low-melting glass powder are added into a mortar and ground for 30 minutes to prepare mixed powder, then the organic silicon resin and a proper amount of dimethylbenzene are stirred and mixed to prepare an organic silicon resin solution with the viscosity of 100cps, and finally the 25wt.% of organic silicon resin solution and the mixed powder are simultaneously added into a beaker and mechanically stirred for 1 hour to complete the preparation of the adhesive. Wherein the particle size of the diamond powder is 460 meshes; the granularity of the zinc oxide powder is 325 meshes; the mesh number of the copper powder is 325 meshes; the mesh number of the titanium powder is 325 meshes; the mesh number of the low-melting-point glass powder is 1500 meshes; the organic silicon resin is polymethylphenylsiloxane; the xylene purity was analytical.
(2) Uniformly coating the adhesive on the surfaces of the two bonding surfaces, then bonding the two surfaces, controlling the pressure applied to the surface of the material under the atmospheric environment to control the thickness of the adhesive layer to be 0.15 mu m, then placing the material into a blast oven, heating to 250 ℃ at the speed of 5 ℃/h, and then preserving heat for 2 hours.
(3) And (3) putting the cured material into high-temperature vacuum equipment, heating to 1200 ℃ at the speed of 100 ℃/hour under the vacuum environment of-0.1 MPa, and then preserving heat for 2 hours to finish the carbonization of the adhesive.
C after adhesive repair in example 2fthe/C composite material:
the room-temperature bonding strength is 13.0MPa, and the failure mode is Cfthe/C composite material body is broken;
after accumulated treatment is carried out for 50 hours at 300 ℃, 700 ℃, 1100 ℃ and 1500 ℃, no defects such as pores, cracks and the like are found at the glue layer, the bonding strength is 13.0MPa, the bonding strength is not attenuated compared with the bonding strength at room temperature, and the failure mode is that the body material is still broken;
the bonded sample does not crack after accumulated treatment for 20 hours at 1800 ℃, the bonding strength is 7.1MPa, and the bonded sample has excellent heat resistance;
thermal conductivities at room temperature (25 ℃), 700 ℃ and 1000 ℃ of 22.31W/(m.k), 20.97W/(m.k) and 17.90W/(m.k), respectively, and CfThe thermal conductivity of the/C composite material is equivalent.
The above test method for the adhesion property was the same as in example 1.
Example 3:
the embodiment provides a bonding repair method for a carbon fiber reinforced carbon-based composite material, which comprises the following steps:
(1) at the room temperature of 25 ℃, 13 wt.% of diamond powder, 12wt.% of zinc oxide powder, 8 wt.% of copper powder, 10 wt.% of titanium powder and 32 wt.% of low-melting glass powder are added into a mortar and ground for 30 minutes to prepare mixed powder, then the organic silicon resin and a proper amount of dimethylbenzene are stirred and mixed to prepare an organic silicon resin solution with the viscosity of 85cps, and finally the 25wt.% of organic silicon resin solution and the mixed powder are simultaneously added into a beaker and mechanically stirred for 1 hour to complete the preparation of the adhesive. Wherein the particle size of the diamond powder is 650 meshes; the granularity of the zinc oxide powder is 270 meshes; the mesh number of the copper powder is 200 meshes; the mesh number of the titanium powder is 325 meshes; the mesh number of the low-melting-point glass powder is 1500 meshes; the organic silicon resin is polymethylphenylsiloxane; the xylene purity was analytical.
(2) Uniformly coating the adhesive on the surfaces of the two bonding surfaces, then bonding the two surfaces, controlling the thickness of an adhesive layer to be 0.08 mu m by controlling the pressure applied to the surface of the material in an atmospheric environment, then placing the material into a blast oven, heating to 250 ℃ at the speed of 5 ℃/h, and then preserving heat for 2 hours.
(3) And (3) putting the cured material into high-temperature vacuum equipment, heating to 1200 ℃ at the speed of 100 ℃/hour under the vacuum environment of-0.1 MPa, and then preserving heat for 2 hours.
C after adhesive repair in example 3fthe/C composite material:
the room-temperature bonding strength is 12.9MPa, and the failure mode is Cfthe/C composite material body is broken;
after accumulated treatment is carried out for 50 hours at 300 ℃, 700 ℃, 1100 ℃ and 1500 ℃, no defects such as pores, cracks and the like are found at the glue layer, the bonding strength is 12.9MPa, the bonding strength is not attenuated compared with the bonding strength at room temperature, and the failure mode is that the body material is still broken;
the bonded sample does not crack after accumulated treatment for 20 hours at 1800 ℃, the bonding strength is 7.1MPa, and the bonded sample has excellent heat resistance;
thermal conductivities at room temperature (25 ℃), 700 ℃ and 1000 ℃ of 24.68W/(m.k), 21.12W/(m.k) and 19.03W/(m.k), respectively, and CfThe thermal conductivity of the/C composite material is equivalent.
The above test method for the adhesion property was the same as in example 1.

Claims (10)

1. A bonding repair method for a carbon fiber reinforced carbon-based composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) adhesive preparation:
at the room temperature of 25 ℃, firstly, adding 10-15 wt.% of diamond powder, 12-15 wt.% of zinc oxide powder, 6-12 wt.% of copper powder, 10-15 wt.% of titanium powder and 32-37 wt.% of low-melting-point glass powder into a mortar, mixing and grinding for 30 minutes to prepare mixed powder;
simultaneously adding the mixed powder and 20-25 wt.% of organic silicon resin solution into a container, and mechanically stirring for 1 hour to complete the preparation of the adhesive; the organic silicon resin solution is prepared by stirring and mixing organic silicon resin and dimethylbenzene, and the viscosity is 65-100 cps;
(2) curing of the adhesive:
uniformly coating the prepared adhesive on the surfaces of two bonding surfaces of a material to be repaired, then bonding the two surfaces, controlling the pressure applied to the surface of the material in the atmospheric environment, controlling the thickness of the adhesive layer to be 0.08-0.3 mu m, then placing the material into a blast oven, heating to 250 ℃ at the speed of 5 ℃/h, preserving the temperature for 2 hours to complete the curing of the adhesive, and controlling the thickness of the adhesive layer to be 0.08-0.3 mu m by applying pressure to the material during the whole curing period;
(3) carbonization of the adhesive:
and (3) putting the cured material into high-temperature vacuum equipment, heating to 1200 ℃ at the speed of 100 ℃/hour under the vacuum environment of-0.1 MPa, and then preserving heat for 2 hours to finish the carbonization of the adhesive.
2. The method for repairing the adhesion of the carbon fiber reinforced carbon-based composite material according to claim 1, wherein: the granularity of the diamond powder in the step (1) is 460-650 meshes; the granularity of the zinc oxide powder is 270-325 meshes; the mesh number of the copper powder is 200-325 meshes; the mesh number of the titanium powder is 200-325 meshes; the low-melting point glass powder has a mesh number of 1500-3000 meshes and a melting point of 700-750 ℃.
3. The method for repairing the adhesion of the carbon fiber reinforced carbon-based composite material according to claim 1, wherein: the organic silicon resin is polymethylphenylsiloxane; the purity of the xylene was analytical grade.
4. The high-heat-conductivity high-temperature-resistant adhesive is characterized in that: the adhesive is prepared by the following method:
at the room temperature of 25 ℃, firstly, adding 10-15 wt.% of diamond powder, 12-15 wt.% of zinc oxide powder, 6-12 wt.% of copper powder, 10-15 wt.% of titanium powder and 32-37 wt.% of low-melting-point glass powder into a mortar, mixing and grinding for 30 minutes to prepare mixed powder;
simultaneously adding the mixed powder and 20-25 wt.% of organic silicon resin solution into a container, and mechanically stirring for 1 hour to complete the preparation of the adhesive; the organic silicon resin solution is prepared by stirring and mixing organic silicon resin and dimethylbenzene, and the viscosity of the organic silicon resin solution is 65-100 cps.
5. The high thermal conductivity and high temperature resistance adhesive according to claim 4, wherein: the particle size of the diamond powder is 460-650 meshes; the granularity of the zinc oxide powder is 270-325 meshes; the mesh number of the copper powder is 200-325 meshes; the mesh number of the titanium powder is 200-325 meshes; the low-melting point glass powder has a mesh number of 1500-3000 meshes and a melting point of 700-750 ℃.
6. The high thermal conductivity and high temperature resistance adhesive according to claim 4, wherein: the organic silicon resin is polymethylphenylsiloxane; the purity of the xylene was analytical grade.
7. A preparation method of a high-heat-conductivity high-temperature-resistant adhesive is characterized by comprising the following steps: the method comprises the following steps:
at the room temperature of 25 ℃, firstly, adding 10-15 wt.% of diamond powder, 12-15 wt.% of zinc oxide powder, 6-12 wt.% of copper powder, 10-15 wt.% of titanium powder and 32-37 wt.% of low-melting-point glass powder into a mortar, mixing and grinding for 30 minutes to prepare mixed powder;
simultaneously adding the mixed powder and 20-25 wt.% of organic silicon resin solution into a container, and mechanically stirring for 1 hour to complete the preparation of the adhesive; the organic silicon resin solution is prepared by stirring and mixing organic silicon resin and dimethylbenzene, and the viscosity of the organic silicon resin solution is 65-100 cps.
8. The preparation method of the high-thermal-conductivity high-temperature-resistant adhesive according to claim 7, characterized in that: the particle size of the diamond powder is 460-650 meshes; the granularity of the zinc oxide powder is 270-325 meshes; the mesh number of the copper powder is 200-325 meshes; the mesh number of the titanium powder is 200-325 meshes; the low-melting point glass powder has a mesh number of 1500-3000 meshes and a melting point of 700-750 ℃.
9. The preparation method of the high-thermal-conductivity high-temperature-resistant adhesive according to claim 7, characterized in that: the organic silicon resin is polymethylphenylsiloxane; the purity of the xylene was analytical grade.
10. The application of the high-thermal-conductivity high-temperature-resistant adhesive as defined in any one of claims 4 to 6 in repairing carbon fiber reinforced carbon-based composite materials.
CN202111151677.1A 2021-09-29 2021-09-29 Bonding repair method for carbon fiber reinforced carbon-based composite material, used bonding agent and preparation method thereof Active CN113881354B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111151677.1A CN113881354B (en) 2021-09-29 2021-09-29 Bonding repair method for carbon fiber reinforced carbon-based composite material, used bonding agent and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111151677.1A CN113881354B (en) 2021-09-29 2021-09-29 Bonding repair method for carbon fiber reinforced carbon-based composite material, used bonding agent and preparation method thereof

Publications (2)

Publication Number Publication Date
CN113881354A true CN113881354A (en) 2022-01-04
CN113881354B CN113881354B (en) 2022-07-22

Family

ID=79007973

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111151677.1A Active CN113881354B (en) 2021-09-29 2021-09-29 Bonding repair method for carbon fiber reinforced carbon-based composite material, used bonding agent and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113881354B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115403400A (en) * 2022-08-19 2022-11-29 宏德新材料科技(葫芦岛)股份有限公司 Aircraft carbon/carbon composite material brake disc repairing method and adhesive used in method

Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5180532A (en) * 1989-02-27 1993-01-19 Mitsubishi Denki Kabushiki Kaisha Process for preparing mica-containing ceramic composite
JPH11218605A (en) * 1998-01-30 1999-08-10 Toppan Printing Co Ltd Color filter and its production
JP2004200322A (en) * 2002-12-17 2004-07-15 Dainippon Printing Co Ltd Rear surface protective sheet for solar cell module and solar cell module using the same
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
JP2008169265A (en) * 2007-01-10 2008-07-24 Kaneka Corp Electrically insulating and highly thermally conductive thermoplastic resin composition and highly thermally conductive molded article
CN101671194A (en) * 2009-09-23 2010-03-17 北京航空航天大学 Preparation method of high temperature adhesive used for carbon-based composite material
CN101671530A (en) * 2009-09-23 2010-03-17 北京航空航天大学 Preparation method of cryogenic adhesive used for carbon-based composite material
CN101851478A (en) * 2010-04-29 2010-10-06 黄文迎 Rapid-curing conductive adhesive composition and method for preparing same
CN101921489A (en) * 2010-08-24 2010-12-22 烟台德邦电子材料有限公司 Macromolecule thermal-conducting composite material and preparation method thereof
US20110024675A1 (en) * 2008-02-29 2011-02-03 Shin-Etsu Chemical Co., Ltd. Heat conductive cured product and making method
CN102491783A (en) * 2011-11-21 2012-06-13 西北工业大学 Repairing method of carbon ceramic brake-disc coating
CN102746032A (en) * 2012-06-25 2012-10-24 西北工业大学 Method for repairing medium temperature coating (1000 to 1400 DEG C) of silicon carbide base composite material toughened by carbon fiber
CN103894694A (en) * 2014-04-17 2014-07-02 哈尔滨工业大学 Method for connection between composite type green low-melting solder glass and silicon carbide reinforced aluminum matrix composites
CN104028749A (en) * 2014-06-05 2014-09-10 浙江大学 High-thermal-stability insulated coating treatment method of metal soft magnetic composite material
US20180134925A1 (en) * 2016-11-11 2018-05-17 Polyonics, Inc. High temperature resistant pressure sensitive adhesive with low thermal impedance
CN108329048A (en) * 2018-02-26 2018-07-27 陕西科技大学 A kind of connection method of carbon/carbon compound material
CN108912683A (en) * 2018-06-13 2018-11-30 中国科学院金属研究所 Based on low-melting-point metal conductive particle composite heat-conducting network thermal interfacial material and preparation method thereof
CN111662558A (en) * 2020-07-17 2020-09-15 无锡恒尚装饰工程有限公司 High-strength flame-retardant heat-insulation composite door and window

Patent Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5180532A (en) * 1989-02-27 1993-01-19 Mitsubishi Denki Kabushiki Kaisha Process for preparing mica-containing ceramic composite
JPH11218605A (en) * 1998-01-30 1999-08-10 Toppan Printing Co Ltd Color filter and its production
JP2004200322A (en) * 2002-12-17 2004-07-15 Dainippon Printing Co Ltd Rear surface protective sheet for solar cell module and solar cell module using the same
JP2008169265A (en) * 2007-01-10 2008-07-24 Kaneka Corp Electrically insulating and highly thermally conductive thermoplastic resin composition and highly thermally conductive molded article
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
US20110024675A1 (en) * 2008-02-29 2011-02-03 Shin-Etsu Chemical Co., Ltd. Heat conductive cured product and making method
CN101671194A (en) * 2009-09-23 2010-03-17 北京航空航天大学 Preparation method of high temperature adhesive used for carbon-based composite material
CN101671530A (en) * 2009-09-23 2010-03-17 北京航空航天大学 Preparation method of cryogenic adhesive used for carbon-based composite material
CN101851478A (en) * 2010-04-29 2010-10-06 黄文迎 Rapid-curing conductive adhesive composition and method for preparing same
CN101921489A (en) * 2010-08-24 2010-12-22 烟台德邦电子材料有限公司 Macromolecule thermal-conducting composite material and preparation method thereof
CN102491783A (en) * 2011-11-21 2012-06-13 西北工业大学 Repairing method of carbon ceramic brake-disc coating
CN102746032A (en) * 2012-06-25 2012-10-24 西北工业大学 Method for repairing medium temperature coating (1000 to 1400 DEG C) of silicon carbide base composite material toughened by carbon fiber
CN103894694A (en) * 2014-04-17 2014-07-02 哈尔滨工业大学 Method for connection between composite type green low-melting solder glass and silicon carbide reinforced aluminum matrix composites
CN104028749A (en) * 2014-06-05 2014-09-10 浙江大学 High-thermal-stability insulated coating treatment method of metal soft magnetic composite material
US20180134925A1 (en) * 2016-11-11 2018-05-17 Polyonics, Inc. High temperature resistant pressure sensitive adhesive with low thermal impedance
CN108329048A (en) * 2018-02-26 2018-07-27 陕西科技大学 A kind of connection method of carbon/carbon compound material
CN108912683A (en) * 2018-06-13 2018-11-30 中国科学院金属研究所 Based on low-melting-point metal conductive particle composite heat-conducting network thermal interfacial material and preparation method thereof
CN111662558A (en) * 2020-07-17 2020-09-15 无锡恒尚装饰工程有限公司 High-strength flame-retardant heat-insulation composite door and window

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
WANG, XZ等: "Preparation of high-temperature organic adhesives and their performance for joining SiC ceramic", 《CERAMICS INTERNATIONAL 》 *
王小宙: "耐高温有机硅胶粘剂的制备及性能研究", 《《万方数据库》》 *
陈玉峰等: "空天飞行器用热防护陶瓷材料", 《现代技术陶瓷》 *
高晓云: "纤维增强陶瓷复合材料的制造技术", 《化工新型材料》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115403400A (en) * 2022-08-19 2022-11-29 宏德新材料科技(葫芦岛)股份有限公司 Aircraft carbon/carbon composite material brake disc repairing method and adhesive used in method
CN115403400B (en) * 2022-08-19 2023-03-21 宏德新材料科技(葫芦岛)股份有限公司 Aircraft carbon/carbon composite material brake disc repairing method and adhesive used in method

Also Published As

Publication number Publication date
CN113881354B (en) 2022-07-22

Similar Documents

Publication Publication Date Title
He et al. Debonding of CFRP-to-steel joints with CFRP delamination
Reedy Jr et al. Comparison of butt tensile strength data with interface corner stress intensity factor prediction
CN113881354B (en) Bonding repair method for carbon fiber reinforced carbon-based composite material, used bonding agent and preparation method thereof
CN112225458B (en) High-temperature-resistant low-expansion-coefficient bonding slurry for ceramic matrix composite and preparation method thereof
JP2023549545A (en) Bonding solder and its manufacturing method, bonding method for silicon carbide coating
CN108950463B (en) High-temperature environment barrier coating structure and preparation method thereof
CN103738000B (en) Fibre composite reinforcement and the concrete method of protection
US11780781B2 (en) Bonding dissimilar ceramic components
CN108822792B (en) Preparation method of high-temperature adhesive suitable for nickel-based alloy
CN111517795A (en) Thermal protection material structural damage repair patch and preparation and use method thereof
CN110105904A (en) The glue applying method of resistance to 1500 DEG C of high temperature adhesives
CN113735609A (en) Remanufacturing method of carbon/carbon friction material
CN108329055B (en) Method for repairing SiC setter plate or sagger and repairing bonding material
CN115816926B (en) Reusable heat-proof and heat-proof structure based on ceramic tile and preparation method thereof
CN114561152B (en) Room-temperature-curing inorganic-organic composite adhesive with temperature resistance of 400 ℃ and preparation method thereof
CN103786382A (en) Method for reinforcing and protecting concrete through inorganic adhesive fiber composite material
CN114958259B (en) High-temperature-resistant phenolic aldehyde adhesive for composite material and preparation method thereof
CN108611047A (en) A method of preparing the wide organopolysiloxane base adhesive in temperature in use domain
Petrova et al. Adhesives for aviation equipment
Mayer et al. Impact and adhesion tests of composite polymer coatings on steel substrate
CN115305019B (en) High-temperature adhesive and preparation method and application method thereof
Sarker et al. Bond strength of fly ash geopolymer with CFRP fabric after exposure to high temperature
CN117285372A (en) Repairing agent for ceramic-based heat-proof material of aircraft and repairing method thereof
Cerny et al. Adhesive Bonding of Titanium to Carbon‐Carbon Composites for Heat Rejection Systems
Bagcı et al. An Investigation On the Use Of Geopolymer As An Alternative Adhesive For Aluminum Panels

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant