CN105967717A - Preparation method of carbon fiber thermal-insulation board - Google Patents
Preparation method of carbon fiber thermal-insulation board Download PDFInfo
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- CN105967717A CN105967717A CN201610344321.2A CN201610344321A CN105967717A CN 105967717 A CN105967717 A CN 105967717A CN 201610344321 A CN201610344321 A CN 201610344321A CN 105967717 A CN105967717 A CN 105967717A
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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
- C04B35/71—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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
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Abstract
The invention discloses a preparation method of a carbon fiber thermal-insulation board. By adopting the carbon fiber material, the high temperature resistance of the thermal-insulation board is enhanced; and the technique adopts vacuum filtration one-step formation, so the thermal-insulation board has favorable overall performance. The product surface is treated, thereby enhancing the product quality and prolonging the service life of the product.
Description
Technical field
The present invention relates to the preparation method of a kind of Carbon fiber thermal insulation plate.
Background technology
Along with the development of science and technology, the demand of insulation material is increased severely by all fields of national economy such as military affairs, national defence, metallurgy, chemical industry day by day, and more and more higher to the performance requirement of insulation material.China has the multiple high temperature furnaces such as sintering cemented carbide stove, monocrystaline silicon stove, polycrystalline ingot furnace, vacuum smelting furnace, vacuum heat treatment furnace, gaseous phase deposition stove more than at least 10 ten thousand, these high temperature furnaces the most commonly used traditional heat-insulating heat-preserving material.
Insulation material used in current domestic high-temperature vacuum furnace exists that intensity is low, yielding, easy-weathering, effect of heat insulation are poor, remove and install shortcomings such as wasting time and energy, and carbon fiber hardening insulation material can overcome disadvantages mentioned above, can be used widely as the heat-insulating heat-preserving material in the high temperature furnaces such as crystalline silicon high temperature furnace, gaseous phase deposition stove, ceramic sintering furnace.
Carbon fiber reinforced carbon matrix composite material, it is called for short carbon/carbon (carbon fiber) composite, carbon fibre composite is the carbon fiber of high intensity to be embedded matrix carbon be composited, and reinforcement and matrix are all the feature of a kind of element so that the two respective performance is maintained.Carbon fibre composite light specific gravity, density is only the 1/2 of ceramic material, the 1/4 of nickel-base alloy；Mechanical property has specific strength height, specific modulus is big, fracture toughness good, and particularly when high temperature, its intensity does not the most decline and rises along with temperature on the contrary and raise, and this is the exclusive feature that other materials is incomparable；It is low that carbon fibre composite thermophysical property then has thermal coefficient of expansion, the feature such as resistance to ablation, good thermal shock stability.
Summary of the invention
The present invention provides the preparation method of a kind of Carbon fiber thermal insulation plate, uses warming plate prepared by the method, and resistance to elevated temperatures is strong, high insulating effect.
To achieve these goals, the present invention provides the preparation method of a kind of Carbon fiber thermal insulation plate, 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, grinding, the carbon fiber wire accounting obtaining a length of 10-30mm is 50%-90%, the composite carbon fibrous material that carbon fiber wire accounting is 10%-50% of a length of 1-5mm；
(2) base substrate vacuum filtration molding
Vacuum filtration composite carbon fibrous material serosity, form base substrate: weigh composite carbon fibrous material 1-3 part, dispersant 1-2 part and 100 parts of water by weight, it is uniformly mixing to obtain composite carbon fibrous material serosity, composite carbon fibrous material serosity is cast in vacuum filtration mould, sucking filtration forms base substrate, casting resin solution in vacuum filtration mould, until solution submergence base substrate, starts vacuum filtration, takes unnecessary resin solution away；
(3) base substrate curing molding
Base substrate after taking unnecessary resin solution away with the heating rate of 5-10 DEG C/min is heated to 200-300 DEG C；Then, by base substrate in vacuum or the environment of noble gas, it is heated to 600-1200 DEG C and carries out carbonization process；
(4) billet surface processes
Base substrate after carbonization carries out surface polishing, dust suction processes, and carries out surface oxidation-resistant process and/or reinforcing and processing surface after handling well again；
(5) base substrate high-temperature process
Base substrate after being processed on surface is transferred to, in vacuum or the environment of noble gas, be heated to 2000-2800 DEG C and carry out high-temperature process, be prepared as Carbon fiber thermal insulation plate.
Preferably, in composite catalyst, the mol ratio of Ni, La, Al is: Ni:La:Al=10:1:4.
Preferably, the one during described resin solution is phenol resin solution, epoxy resin solution, furane resins solution, urea-formaldehyde resin solution, vinyl ester resins solution.
Carbon fiber thermal insulation plate prepared by the present invention, uses composite carbon fibrous material, improves the resistance to elevated temperatures of warming plate, and technique uses vacuum filtration one-shot forming, and overall performance is good；Product surface processes, and improves product quality, extends the service life of product.
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 depositing the high temperature graphitization at a temperature of 2200 DEG C of the sample after density and processes 2h, after natural cooling, grind, the carbon fiber wire accounting obtaining a length of 10-30mm is 50%, the composite carbon fibrous material that carbon fiber wire accounting is 10% of a length of 1-5mm.
Vacuum filtration composite carbon fibrous material serosity, form base substrate: weigh composite carbon fibrous material 1 part, dispersant 1 part and 100 parts of water by weight, it is uniformly mixing to obtain composite carbon fibrous material serosity, composite carbon fibrous material serosity is cast in vacuum filtration mould, sucking filtration forms base substrate, casting resin solution in vacuum filtration mould, until solution submergence base substrate, starts vacuum filtration, takes unnecessary resin solution away.Described resin solution is the one in phenol resin solution, epoxy resin solution, furane resins solution, urea-formaldehyde resin solution, vinyl ester resins solution.
Base substrate after taking unnecessary resin solution away with the heating rate of 5 DEG C/min is heated to 200 DEG C；Then, by base substrate in vacuum or the environment of noble gas, it is heated to 600 DEG C and carries out carbonization process.
Base substrate after carbonization carries out surface polishing, dust suction processes, and carries out surface oxidation-resistant process and/or reinforcing and processing surface after handling well again.Base substrate after being processed on surface is transferred to, in vacuum or the environment of noble gas, be heated to 2000 DEG C and carry out high-temperature process, be prepared as Carbon fiber thermal insulation plate.
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 depositing the high temperature graphitization at a temperature of 2250 DEG C of the sample after density and processes 3h, after natural cooling, grind, the carbon fiber wire accounting obtaining a length of 10-30mm is 50%, the composite carbon fibrous material that carbon fiber wire accounting is 50% of a length of 1-5mm.
Vacuum filtration composite carbon fibrous material serosity, form base substrate: weigh composite carbon fibrous material 3 parts, dispersant 2 parts and 100 parts of water by weight, it is uniformly mixing to obtain composite carbon fibrous material serosity, composite carbon fibrous material serosity is cast in vacuum filtration mould, sucking filtration forms base substrate, casting resin solution in vacuum filtration mould, until solution submergence base substrate, starts vacuum filtration, takes unnecessary resin solution away.Described resin solution is the one in phenol resin solution, epoxy resin solution, furane resins solution, urea-formaldehyde resin solution, vinyl ester resins solution.
Base substrate after taking unnecessary resin solution away with the heating rate of 10 DEG C/min is heated to 300 DEG C；Then, by base substrate in vacuum or the environment of noble gas, it is heated to 600-1200 DEG C and carries out carbonization process.
Base substrate after carbonization carries out surface polishing, dust suction processes, and carries out surface oxidation-resistant process and/or reinforcing and processing surface after handling well again.Base substrate after being processed on surface is transferred to, in vacuum or the environment of noble gas, be heated to 2800 DEG C and carry out high-temperature process, be prepared as Carbon fiber thermal insulation plate.
Claims (3)
1. a preparation method for Carbon fiber thermal insulation plate, 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, grinding, the carbon fiber wire accounting obtaining a length of 10-30mm is 50%-90%, the composite carbon fibrous material that carbon fiber wire accounting is 10%-50% of a length of 1-5mm；
(2) base substrate vacuum filtration molding
Vacuum filtration composite carbon fibrous material serosity, form base substrate: weigh composite carbon fibrous material 1-3 part, dispersant 1-2 part and 100 parts of water by weight, it is uniformly mixing to obtain composite carbon fibrous material serosity, composite carbon fibrous material serosity is cast in vacuum filtration mould, sucking filtration forms base substrate, casting resin solution in vacuum filtration mould, until solution submergence base substrate, starts vacuum filtration, takes unnecessary resin solution away；
(3) base substrate curing molding
Base substrate after taking unnecessary resin solution away with the heating rate of 5-10 DEG C/min is heated to 200-300 DEG C；Then, by base substrate in vacuum or the environment of noble gas, it is heated to 600-1200 DEG C and carries out carbonization process；
(4) billet surface processes
Base substrate after carbonization carries out surface polishing, dust suction processes, and carries out surface oxidation-resistant process and/or reinforcing and processing surface after handling well again；
(5) base substrate high-temperature process
Base substrate after being processed on surface is transferred to, in vacuum or the environment of noble gas, be heated to 2000-2800 DEG C and carry out high-temperature process, be prepared as Carbon fiber thermal insulation plate.
2. the method for claim 1, it is characterised in that in composite catalyst, the mol ratio of Ni, La, Al is: Ni:La:Al=10:1:4.
3. the method for claim 1, it is characterised in that described resin solution is the one in phenol resin solution, epoxy resin solution, furane resins solution, urea-formaldehyde resin solution, vinyl ester resins solution.
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| CN201610344321.2A CN105967717A (en) | 2016-05-23 | 2016-05-23 | Preparation method of carbon fiber thermal-insulation board |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109734461A (en) * | 2019-02-27 | 2019-05-10 | 盐城飞潮环保技术有限公司 | A kind of preparation method of pyroceram fibre screen pipe |
| CN115157516A (en) * | 2022-09-06 | 2022-10-11 | 湖南搏盛天弘新材料技术有限公司 | Preparation method of novel carbon fiber insulation board |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN104891950A (en) * | 2015-05-12 | 2015-09-09 | 湖南搏盛天弘新材料技术有限公司 | Hard carbon fiber heat insulation board 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 |
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2016
- 2016-05-23 CN CN201610344321.2A patent/CN105967717A/en active Pending
Patent Citations (3)
| 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 |
| CN104891950A (en) * | 2015-05-12 | 2015-09-09 | 湖南搏盛天弘新材料技术有限公司 | Hard carbon fiber heat insulation board and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109734461A (en) * | 2019-02-27 | 2019-05-10 | 盐城飞潮环保技术有限公司 | A kind of preparation method of pyroceram fibre screen pipe |
| CN109734461B (en) * | 2019-02-27 | 2022-06-07 | 江苏赛图新材料科技有限公司 | Preparation method of high-temperature-resistant ceramic fiber filter tube |
| CN115157516A (en) * | 2022-09-06 | 2022-10-11 | 湖南搏盛天弘新材料技术有限公司 | Preparation method of novel carbon fiber insulation board |
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