CN105967714A - Preparation method of composite carbon pottery material - Google Patents

Preparation method of composite carbon pottery material Download PDF

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Publication number
CN105967714A
CN105967714A CN201610344300.0A CN201610344300A CN105967714A CN 105967714 A CN105967714 A CN 105967714A CN 201610344300 A CN201610344300 A CN 201610344300A CN 105967714 A CN105967714 A CN 105967714A
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carbon
temperature
composite
gained
carbon fiber
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不公告发明人
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Suzhou Sichuang Yuanbo Electronic Technology Co Ltd
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Suzhou Sichuang Yuanbo Electronic Technology Co Ltd
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    • C04B35/806—
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—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
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248—Carbon, e.g. graphite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/614—Gas infiltration of green bodies or pre-forms
    • 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
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/616—Liquid infiltration of green bodies or pre-forms
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

The invention discloses a preparation method of a composite carbon pottery material. By adopting the composite carbon fiber material, the carbon-carbon composite material has higher mechanical properties. By adopting the specific technique and parameters, the composite material has the advantages of low density, favorable mechanical properties and favorable ablation resistance.

Description

A kind of preparation method of composite carbon ceramic material
Technical field
The present invention relates to the preparation method of a kind of composite carbon ceramic material.
Background technology
The brake disc being presently used on aircraft mainly has carbon-carbon material and powdered metallurgical material two class.Powder metallurgy brake material has the disadvantage that: the most bonding under high temperature, and weight is big, and heat fading is obvious, and elevated temperature strength declines, and thermal shock resistance is poor, and the life-span is short.And carbon-carbon composite brake disc is developed as far back as 20 century 70s, it has light weight under hot conditions, can carry the features such as strong, the length in service life of energy high, high temperature resistant, but has oxidizable due to it, the easy moisture absorption, the shortcomings such as hygrometric state coefficient of friction is low, and static friction coefficient is little.Meanwhile, along with science and technology and the update of aircraft, carbon-to-carbon brake composite is increasingly difficult to meet the demand of aircraft brake.It is therefore necessary to develop one to avoid disadvantages described above, the new brake dish composite of high comprehensive performance.
Carbon pottery brake material is as a kind of new brake material, compared with traditional metal and semi-metallic brake pad, it has that density is low, stable friction factor, brake percentage greatly, the advantage such as not corrosion and length in service life, heat fading will not be produced during especially long-time brake continuously.And compared with carbon carbon brake material, it has excellent antioxygenic property and the decay of hygrometric state frictional behaviour is little, confficient of static friction is high and the outstanding advantages such as life-span length, substantially increase the safety of brake.
Summary of the invention
The present invention provides the preparation method of a kind of composite carbon ceramic material, uses the method technique controlled, and density is little, mechanical property good, wear extent is few, curve is steady, it is little to vibrate.
To achieve these goals, the present invention provides the preparation method of a kind of composite carbon ceramic material, and the method comprises the steps:
(1) carbon fibre composite is prepared
Under vacuum, carbon fiber is put into calcination 2-3h in 2150 DEG C of-2225 DEG C of environment, the mixed solution of the carbon fiber substrate nitric acid after calcination and sulphuric acid is soaked 50-80min at 50-70 DEG C, then with deionized water rinsing to neutral, finally dries stand-by；
Taking 10-12mL composite catalyst, add the ammonia 90-120mL that concentration is 2mol/L, add 30-50mL dehydrated alcohol, stirring makes its mix homogeneously；
By mixed solution transfer in autoclave, the prefabricated carbon fiber body of gained is put in still dipping 8-10h；
Reactor is immersed reaction 2-3h in the oil bath of 120-140 DEG C；
With cold water to reactor chilling so that it is temperature is down to room temperature, take out prefabricated carbon fiber body, dry in the shade in the case of constantly stirring；
Proceed to the sample of gained vacuum carbon tube furnace be calcined, reduces, the prefabricated carbon fiber body of metallic catalyst Ni granule must be loaded with；
Gained prefabricated carbon fiber body is loaded in vacuum carbon tube furnace, carries out depositing density.Wherein, main technologic parameters is: temperature 1200-1300 DEG C, and pipe natural gas gas flow scope is 5-7L, and atmosphere pressures controls to be 1.5-2KPa, and sedimentation time is 50-60h；
Gained is deposited the high temperature graphitization at a temperature of 2200-2250 DEG C of the sample after density and processes 2h-3h, after natural cooling, obtain composite carbon fibrous material；
(2) described composite carbon fibrous material being placed in impregnation liquid one dipping, after dipping, carry out Pintsch process under protective atmosphere, repeated impregnations-Pintsch process operation, until obtaining density is 1.85-1.9g/cm3Carbon ceramic composite material；Described impregnation liquid one is by polymethyl silicane, and styrene composition；The temperature of described Pintsch process is 1000-1300 DEG C；
(3) under protective atmosphere, gained carbon ceramic composite material is carried out high-temperature process, until the density of carbon ceramic composite material is down to 1.85-1.89g/cm3, obtain preform；The temperature of described high-temperature process is 1450-1650 DEG C；
(4) being placed in by preform in impregnation liquid two, after having impregnated, crack under protective atmosphere, polish after cracking, repetitive cycling dipping impregnation liquid two-cracking-sanding operation is until obtaining density is 1.95-2.03g/cm3Carbon ceramic composite material finished product；Described impregnation liquid two is by silica flour and polymethyl silicane 10-24:100 in mass ratio, and the temperature of described cracking is 1200-1300 DEG C.
Carbon-carbon composite prepared by the present invention, uses composite carbon fibrous material, improves the mechanical performance of material, uses special process and parameter so that density is little, mechanical property good, anti-yaw damper is functional.
Detailed description of the invention
Embodiment one
Under vacuum, carbon fiber is put into calcination 2h in 2150 DEG C of environment, the mixed solution of the carbon fiber substrate nitric acid after calcination and sulphuric acid is soaked 50min at 50 DEG C, then with deionized water rinsing to neutral, finally dries stand-by.
Taking 10mL composite catalyst, add the ammonia 90mL that concentration is 2mol/L, add 30mL dehydrated alcohol, stirring makes its mix homogeneously.By mixed solution transfer in autoclave, the prefabricated carbon fiber body of gained is put in still dipping 8h.Reactor is immersed in the oil bath of 120 DEG C and react 2h.With cold water to reactor chilling so that it is temperature is down to room temperature, take out prefabricated carbon fiber body, dry in the shade in the case of constantly stirring.Proceed to the sample of gained vacuum carbon tube furnace be calcined, reduces, the prefabricated carbon fiber body of metallic catalyst Ni granule must be loaded with.In composite catalyst, the mol ratio of Ni, La, Al is: Ni:La:Al=10:1:4.
Gained prefabricated carbon fiber body is loaded in vacuum carbon tube furnace, carries out depositing density.Wherein, main technologic parameters is: temperature 1200 DEG C, and pipe natural gas gas flow scope is 5L, and atmosphere pressures controls to be 1.5KPa, and sedimentation time is 50h.
Gained is deposited the high temperature graphitization at a temperature of 2200 DEG C of the sample after density and processes 2h, after natural cooling, obtain composite carbon fibrous material.
Described composite carbon fibrous material being placed in impregnation liquid one dipping, after dipping, carries out Pintsch process under protective atmosphere, repeated impregnations-Pintsch process operation, until obtaining density is 1.85g/cm3Carbon ceramic composite material；Described impregnation liquid one is by polymethyl silicane, and styrene composition；The temperature of described Pintsch process is 1000-1300 DEG C.
Under protective atmosphere, gained carbon ceramic composite material is carried out high-temperature process, until the density of carbon ceramic composite material is down to 1.85g/cm3, obtain preform；The temperature of described high-temperature process is 1450 DEG C.
Being placed in by preform in impregnation liquid two, after having impregnated, crack under protective atmosphere, polish after cracking, repetitive cycling dipping impregnation liquid two-cracking-sanding operation is until obtaining density is 1.95g/cm3Carbon ceramic composite material finished product；Described impregnation liquid two is 1200 DEG C by silica flour and polymethyl silicane 10:100 in mass ratio, the temperature of described cracking.
Embodiment two
Under vacuum, carbon fiber is put into calcination 3h in 2225 DEG C of environment, the mixed solution of the carbon fiber substrate nitric acid after calcination and sulphuric acid is soaked 80min at 70 DEG C, then with deionized water rinsing to neutral, finally dries stand-by.
Taking 12mL composite catalyst, add the ammonia 120mL that concentration is 2mol/L, add 50mL dehydrated alcohol, stirring makes its mix homogeneously.By mixed solution transfer in autoclave, the prefabricated carbon fiber body of gained is put in still dipping 10h.Reactor is immersed in the oil bath of 140 DEG C and react 3h.With cold water to reactor chilling so that it is temperature is down to room temperature, take out prefabricated carbon fiber body, dry in the shade in the case of constantly stirring.Proceed to the sample of gained vacuum carbon tube furnace be calcined, reduces, the prefabricated carbon fiber body of metallic catalyst Ni granule must be loaded with.In composite catalyst, the mol ratio of Ni, La, Al is: Ni:La:Al=10:1:4.
Gained prefabricated carbon fiber body is loaded in vacuum carbon tube furnace, carries out depositing density.Wherein, main technologic parameters is: temperature 1300 DEG C, and pipe natural gas gas flow scope is 7L, and atmosphere pressures controls to be 2KPa, and sedimentation time is 60h.
Gained is deposited the high temperature graphitization at a temperature of 2250 DEG C of the sample after density and processes 3h, after natural cooling, obtain composite carbon fibrous material.
Described composite carbon fibrous material being placed in impregnation liquid one dipping, after dipping, carries out Pintsch process under protective atmosphere, repeated impregnations-Pintsch process operation, until obtaining density is 1.9g/cm3Carbon ceramic composite material；Described impregnation liquid one is by polymethyl silicane, and styrene composition；The temperature of described Pintsch process is 1300 DEG C.
Under protective atmosphere, gained carbon ceramic composite material is carried out high-temperature process, until the density of carbon ceramic composite material is down to 1.89g/cm3, obtain preform；The temperature of described high-temperature process is 1650 DEG C.
Being placed in by preform in impregnation liquid two, after having impregnated, crack under protective atmosphere, polish after cracking, repetitive cycling dipping impregnation liquid two-cracking-sanding operation is until obtaining density is 2.03g/cm3Carbon ceramic composite material finished product；Described impregnation liquid two is 1300 DEG C by silica flour and polymethyl silicane 24:100 in mass ratio, the temperature of described cracking.

Claims (1)

1. a preparation method for composite carbon ceramic material, the method comprises the steps:
(1) carbon fibre composite is prepared
Under vacuum, carbon fiber is put into calcination 2-3h in 2150 DEG C of-2225 DEG C of environment, the mixed solution of the carbon fiber substrate nitric acid after calcination and sulphuric acid is soaked 50-80min at 50-70 DEG C, then with deionized water rinsing to neutral, finally dries stand-by；
Taking 10-12mL composite catalyst, add the ammonia 90-120mL that concentration is 2mol/L, add 30-50mL dehydrated alcohol, stirring makes its mix homogeneously；
By mixed solution transfer in autoclave, the prefabricated carbon fiber body of gained is put in still dipping 8-10h；
Reactor is immersed reaction 2-3h in the oil bath of 120-140 DEG C；
With cold water to reactor chilling so that it is temperature is down to room temperature, take out prefabricated carbon fiber body, dry in the shade in the case of constantly stirring；
Proceed to the sample of gained vacuum carbon tube furnace be calcined, reduces, the prefabricated carbon fiber body of metallic catalyst Ni granule must be loaded with；
Being loaded in vacuum carbon tube furnace by gained prefabricated carbon fiber body, carry out depositing density, wherein, main technologic parameters is: temperature 1200-1300 DEG C, and pipe natural gas gas flow scope is 5-7L, and atmosphere pressures controls to be 1.5-2KPa, and sedimentation time is 50-60h；
Gained is deposited the high temperature graphitization at a temperature of 2200-2250 DEG C of the sample after density and processes 2h-3h, after natural cooling, obtain composite carbon fibrous material；
(2) described composite carbon fibrous material being placed in impregnation liquid one dipping, after dipping, carry out Pintsch process under protective atmosphere, repeated impregnations-Pintsch process operation, until obtaining density is 1.85-1.9g/cm3Carbon ceramic composite material；Described impregnation liquid one is by polymethyl silicane, and styrene composition；The temperature of described Pintsch process is 1000-1300 DEG C；
(3) under protective atmosphere, gained carbon ceramic composite material is carried out high-temperature process, until the density of carbon ceramic composite material is down to 1.85-1.89g/cm3, obtain preform；The temperature of described high-temperature process is 1450-1650 DEG C；
(4) being placed in by preform in impregnation liquid two, after having impregnated, crack under protective atmosphere, polish after cracking, repetitive cycling dipping impregnation liquid two-cracking-sanding operation is until obtaining density is 1.95-2.03g/cm3Carbon ceramic composite material finished product；Described impregnation liquid two is by silica flour and polymethyl silicane 10-24:100 in mass ratio, and the temperature of described cracking is 1200-1300 DEG C.
CN201610344300.0A 2016-05-23 2016-05-23 Preparation method of composite carbon pottery material Pending CN105967714A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107141006A (en) * 2017-07-05 2017-09-08 孟庆桓 A kind of method that utilization electrostatic self-assembled technology improves carbon pottery brake disc oxygen-proof property

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103568385A (en) * 2013-10-18 2014-02-12 四川创越炭材料有限公司 Heat-preservation hard composite carbon fiber felt and preparation method thereof
CN105565837A (en) * 2015-12-17 2016-05-11 湖南博望碳陶有限公司 Preparation method and application of carbon/ceramic composite material
CN105565836A (en) * 2014-10-11 2016-05-11 西安艾菲尔德复合材料科技有限公司 Method for preparing carbon fiber composite material through catalytic CVD

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103568385A (en) * 2013-10-18 2014-02-12 四川创越炭材料有限公司 Heat-preservation hard composite carbon fiber felt and preparation method thereof
CN105565836A (en) * 2014-10-11 2016-05-11 西安艾菲尔德复合材料科技有限公司 Method for preparing carbon fiber composite material through catalytic CVD
CN105565837A (en) * 2015-12-17 2016-05-11 湖南博望碳陶有限公司 Preparation method and application of carbon/ceramic composite material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107141006A (en) * 2017-07-05 2017-09-08 孟庆桓 A kind of method that utilization electrostatic self-assembled technology improves carbon pottery brake disc oxygen-proof property
CN107141006B (en) * 2017-07-05 2020-07-28 浙江蓝天知识产权运营管理有限公司 Method for improving oxidation resistance of carbon-ceramic brake disc by using electrostatic self-assembly technology

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Application publication date: 20160928