CN113831130B - Light high-strength heat preservation felt and preparation method and application thereof - Google Patents
Light high-strength heat preservation felt and preparation method and application thereof Download PDFInfo
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- CN113831130B CN113831130B CN202111141399.1A CN202111141399A CN113831130B CN 113831130 B CN113831130 B CN 113831130B CN 202111141399 A CN202111141399 A CN 202111141399A CN 113831130 B CN113831130 B CN 113831130B
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- 238000004321 preservation Methods 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 103
- 229910021384 soft carbon Inorganic materials 0.000 claims abstract description 79
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 53
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 53
- 238000010438 heat treatment Methods 0.000 claims description 86
- 239000007789 gas Substances 0.000 claims description 56
- 229910052799 carbon Inorganic materials 0.000 claims description 41
- 229920000877 Melamine resin Polymers 0.000 claims description 29
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 239000012495 reaction gas Substances 0.000 claims description 23
- 238000003763 carbonization Methods 0.000 claims description 21
- 238000005229 chemical vapour deposition Methods 0.000 claims description 20
- 238000009413 insulation Methods 0.000 claims description 20
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000011065 in-situ storage Methods 0.000 claims description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 11
- 239000001294 propane Substances 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 5
- 238000002309 gasification Methods 0.000 claims description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 4
- 239000005977 Ethylene Substances 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 239000012774 insulation material Substances 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 20
- 229910052786 argon Inorganic materials 0.000 description 10
- 229910002804 graphite Inorganic materials 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 238000005452 bending Methods 0.000 description 8
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 6
- 238000010000 carbonizing Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 6
- 239000012300 argon atmosphere Substances 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 5
- 229920000049 Carbon (fiber) Polymers 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
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- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 239000002923 metal particle Substances 0.000 description 4
- 229920006267 polyester film Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000006262 metallic foam Substances 0.000 description 2
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- 150000003384 small molecules Chemical class 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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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
- C04B35/515—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
- C04B35/52—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 carbon, e.g. graphite
- C04B35/524—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 carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
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Abstract
The invention discloses a light high-strength heat preservation felt, which relates to the technical field of heat preservation and insulation materials. The invention also provides a preparation method and application of the light high-strength heat preservation felt. The invention has the beneficial effects that: the surface of the prefabricated soft carbon felt is covered with the carbon nanotube layer, and the carbon nanotubes have excellent mechanical properties due to the special nanostructure. Therefore, when external force acts on the light high-strength heat preservation felt, the force can be transmitted to the carbon nanotube layer through the interface, the carbon nanotubes bear the load applied to the prefabricated soft carbon felt, and the mechanical property of the carbon nanotubes is effectively applied, so that the prefabricated soft carbon felt has higher toughness, and the mechanical strength of the prefabricated soft carbon felt is integrally improved.
Description
Technical Field
The invention relates to the technical field of heat preservation and insulation materials, in particular to a light high-strength heat preservation felt and a preparation method and application thereof.
Background
The heat preservation furnace comprises a degreasing furnace, a high-temperature carbonization furnace, a low-temperature carbonization furnace, a CVD furnace, a CVI furnace and the like, and is widely applied to the fields of chemical industry, energy, aerospace and the like, and the heat insulation layer plays a vital role in the heat preservation furnace. Therefore, the heat insulation felt with the excellent high-temperature heat insulation effect can effectively reduce the diffusion of heat in the furnace, reduce the loss of heat, save energy, simultaneously improve the mechanical strength of the heat insulation felt and prolong the service life of the heat insulation felt. At present, various heat preservation furnaces in China still adopt traditional felt heat insulation materials which have the defects of low use temperature, poor heat insulation performance, unstable thermal field, lower mechanical strength, short service life and the like.
The domestic patent with the application number of CN201410235108.9 discloses a preparation method of a hard heat-preservation carbon felt, which comprises the following steps: (1) preparing glue solution; (2) Flatly paving a polyester film on a working platform, and then paving graphite paper on the polyester film; (3) paving a plurality of soft carbon felts above the graphite paper layer by layer; (4) Laying graphite paper and a polyester film on the soft carbon felt on the uppermost layer to obtain an assembly; (5) putting the assembly into a hot press for hot-pressing solidification; (6) And removing the polyester film of the assembly, then placing the assembly in a carbonization furnace, and carbonizing the assembly under the protection of nitrogen to obtain the hard heat-preservation carbon felt. The invention introduces resin into the common soft carbon felt, bonds a plurality of soft carbon felts together by laying layer by layer, and then adopts hot pressing solidification and carbonization, so that the prepared hard heat preservation carbon felt has excellent performances of small density, small heat conductivity coefficient, high carbon content, low thermal capacity, small linear expansion coefficient, high temperature resistance, strong thermal shock resistance, strong chemical corrosion resistance, energy saving and the like, and can replace the heat insulation material of the traditional heat preservation furnace.
However, the preparation process of the hard heat-preservation carbon felt is complex, and although graphite paper is laid on two sides of the carbon felt assembly, the heat conduction and heat convection of the carbon felt can be enhanced, and the radiation heat transfer can be prevented to a certain extent, so that the prepared hard heat-preservation carbon felt can better play a role in heat insulation. However, the mechanical properties of the graphite paper are poor, the mechanical properties, especially the toughness, of the soft carbon felt are not improved, and meanwhile, the bonding strength of the graphite paper and the soft carbon felt is limited, and the graphite paper and the soft carbon felt are easy to crack and delaminate after being used for a long time, so that in order to overcome the technical defects, a heat-preservation carbon felt with more excellent performances still needs to be developed to meet the requirements of various fields.
Disclosure of Invention
The invention aims to solve the technical problems that the heat preservation carbon felt in the prior art is complex in preparation process and poor in mechanical property, so that the heat preservation carbon felt is easy to crack and delaminate after being used, and the light high-strength heat preservation felt is simple to prepare and capable of improving the mechanical property of the carbon felt.
The invention solves the technical problems through the following technical means:
a light high-strength heat preservation felt comprises a prefabricated soft carbon felt, wherein a carbon nanotube layer is covered on the surface of the prefabricated soft carbon felt.
Has the advantages that: the surface of the prefabricated soft carbon felt is covered with the carbon nanotube layer, and the carbon nanotubes have excellent mechanical properties due to the special nanostructure. Therefore, when external force acts on the light high-strength heat preservation felt, the force can be transmitted to the carbon nanotube layer through the interface, the carbon nanotubes bear the load applied to the prefabricated soft carbon felt, and the mechanical property of the carbon nanotubes is effectively applied, so that the prefabricated soft carbon felt has higher toughness, and the mechanical strength of the prefabricated soft carbon felt is integrally improved.
Preferably, the prefabricated soft carbon felt is prepared by carbonizing melamine nano sponge (nano sponge prepared by foaming melamine) in vacuum or inert gas atmosphere.
Has the advantages that: the melamine nano sponge has light porous quality, is convenient to use, has certain flexibility and deformability compared with metal foam, and can change the thickness and the density of pores according to the external pressure condition even after carbonization treatment, so that the melamine nano sponge has good foldability and thermal insulation performance, and the application range is wider. According to the invention, the surface of the microstructure of the prefabricated soft carbon felt prepared by carbonizing the melamine nano sponge has certain roughness, so that catalyst particles can be better supported when the carbon nano tube grows in situ subsequently, and small molecules generated by hydrocarbon decomposition are better combined on the surface of the prefabricated soft carbon felt, thereby generating the carbon nano tube which is more uniform, has good crystallinity and high purity.
When the prefabricated soft carbon felt is prepared, the melamine nano sponge is directly used for carbonization, the carbon fiber preform forming process is not needed, the cost is relatively low, and the prefabricated soft carbon felt is soft, low in density, low in heat conductivity coefficient, uniform in thermal field and high in porosity.
Preferably, the density of the melamine nano sponge is 0.008-0.01g/cm 3 。
Has the advantages that: the melamine nano sponge with the density effectively ensures the porosity of the prepared soft carbon felt. The thickness of the melamine nano sponge can be determined according to actual needs.
Preferably, the prefabricated soft carbon felt is prepared by the following method: placing melamine nano sponge into a carbonization furnace, rapidly heating to 200-250 ℃ in a vacuum state or in an inert gas atmosphere, keeping the temperature for 15-60min, then heating to 350-400 ℃ at a heating rate of 0.2-1 ℃/min, keeping the temperature for 30-120min, then heating to 700-750 ℃ at a heating rate of 1-5 ℃/min, keeping the temperature for 30-120min, then heating to 900-950 ℃ at a heating rate of 0.2-1 ℃/min, keeping the temperature for 15-60min, then heating to 1000-1200 ℃ at a heating rate of 1-5 ℃/min, keeping the temperature for 60-120min, and cooling to room temperature with the furnace to obtain the prefabricated soft carbon felt.
In the invention, the melamine nano sponge has stronger temperature resistance, so that the temperature can be quickly raised to 200-250 ℃ in the low-temperature stage for early preheating, and the heat preservation time is not too long, so that the temperature is set to be 15-60min; heating to 350-400 ℃ at a slow speed of 0.2-1 ℃/min, preserving heat for 30-120min, wherein the melamine nano sponge starts to shrink in the temperature range, and in order to ensure the stability and uniformity of the organization structure of the melamine nano sponge, heating is carried out for a long heat preservation time at a low speed so that the melamine nano sponge uniformly and slowly shrinks and achieves certain stability; after the structure reaches a certain stability, the temperature is raised to 700-750 ℃ at a rapid rate of 1-5 ℃/min, and the temperature is preserved for 30-120min to achieve the effects of rapid carbonization and shaping; then heating to 900-950 ℃ at a slow speed of 0.2-1 ℃/min, preserving the heat for 15-60min, and further shrinking and carbonizing to reach the required density and thickness; finally, heating at a fast speed of 1-5 ℃/min, preserving heat for 60-120min, and finally carbonizing and shaping; the five-step heating method can gradually and gradually shrink and carbonize the melamine nano sponge, so that the melamine nano sponge is prevented from shrinking too fast to cause nonuniform and unstable structure, and the excellent performance of the finally obtained soft carbon felt is ensured.
As a general inventive concept, the present invention also provides a method for preparing a lightweight high-strength insulation blanket, comprising the steps of: and growing a carbon nano tube on the surface of the prefabricated soft carbon felt in situ by adopting a chemical vapor deposition method to prepare the light high-strength heat preservation felt.
Has the advantages that: compared with the traditional method (carbon fiber, carbon cloth, graphite paper and the like are adopted to carry out bonding, hot pressing, curing and other ways to prepare the carbon felt), the heat preservation felt prepared by the invention has the advantages that the weight is light, the density is small, the heat preservation performance is good, the carbon nanotube grows on the foam prefabricated soft carbon felt with a continuous porous structure in situ to form the carbon felt with an integral structure, the bonding force between the carbon nanotube layer and the surface of the prefabricated soft carbon felt is strong, the mechanical property of the carbon nanotube can be effectively applied, the obtained light high-strength heat preservation felt cannot crack and delaminate, the bending strength is high, the service life is effectively prolonged, the process is simple, the energy is saved, the manufacturing cost is reduced, a series of problems of the existing heat preservation felt are fundamentally solved, and the heat preservation and insulation effect of the heat preservation furnace is good.
Preferably, the preparation method of the light-weight high-strength heat-insulating felt specifically comprises the following steps: placing the prefabricated soft carbon felt into a reaction cavity of a chemical vapor deposition furnace, sealing the reaction cavity, heating the chemical vapor deposition furnace to 300-500 ℃ in a vacuum state, keeping the temperature for 30-60min, then heating to 650-850 ℃, heating and gasifying a metal element compound, continuously entering the reaction cavity along with reaction gas, preserving the temperature for 10-45min, and growing a carbon nano tube on the surface of the prefabricated soft carbon felt in situ, wherein the reaction gas is mixed gas of carbon source gas and reducing gas; and stopping introducing gas after the reaction is finished, vacuumizing, freely cooling to room temperature, and discharging.
Has the beneficial effects that: in the preparation method, the metal element compound is reduced into metal particles in the atmosphere of reducing gas, the metal particles are deposited on the surface of a substrate to be used as a catalyst for growing the carbon nano tube, carbon source gas (hydrocarbon) is decomposed at high temperature to generate small molecular chains, and then the carbon nano tube is generated under the action of the catalyst. Wherein the temperature of 300-500 ℃ is the temperature of the furnace body, the preparation is made for the subsequent deposition, and then the temperature is increased to 650-850 ℃ selectively, because the decomposition rate of reactants in the temperature range is stable, the activity is moderate, and finally the carbon nano tube with uniform deposition and better quality is obtained.
Preferably, in the preparation method, the temperature is increased to 300-500 ℃ at the temperature-increasing rate of 5-10 ℃/min; heating to 650-850 ℃ at a heating rate of 5-10 ℃/min.
Preferably, the flow rate of the reaction gas is 90-350sccm, and the volume ratio of the carbon source gas to the reducing gas in the reaction gas is 1: (3-8), the carbon source gas is a mixed gas of any one or more of methane, ethylene, propane and propylene, the reducing gas is a mixed gas of hydrogen and an inert gas, and the volume ratio of the hydrogen to the inert gas is 1: (2-8).
Preferably, the metal element compound is a chloride of at least one metal of iron, molybdenum, cobalt, nickel, copper and chromium, and the gasification flow rate of the metal element compound is 150-400sccm.
The invention reasonably selects carbon source gas, metal element compounds and the like, and can enable the carbon nano tubes to uniformly grow on the prefabricated soft carbon felt by adjusting parameters such as heating rate, flow and the like.
As a general inventive concept, the invention also provides an application of the light-weight high-strength heat preservation felt or the light-weight high-strength heat preservation felt prepared by the preparation method in heat preservation and insulation of a heat preservation furnace.
The invention has the advantages that: the surface of the prefabricated soft carbon felt is covered with the carbon nano tube layer, and the carbon nano tube has excellent mechanical property due to the special nano structure. Therefore, when external force acts on the light high-strength heat-insulating felt, the force can be transmitted to the carbon nano tube layer through the interface, the carbon nano tubes bear the load applied to the prefabricated soft carbon felt, and the mechanical property of the carbon nano tubes is effectively applied, so that the prefabricated soft carbon felt has high toughness, and the mechanical strength of the prefabricated soft carbon felt is integrally improved.
Compared with the traditional method (carbon fiber, carbon cloth, graphite paper and the like are adopted to carry out bonding, hot pressing, curing and other ways to prepare the carbon felt), the heat preservation felt prepared by the invention has the advantages that the weight is light, the density is small, the heat preservation performance is good, the carbon nanotube grows on the foam prefabricated soft carbon felt with a continuous porous structure in situ to form the carbon felt with an integral structure, the bonding force between the carbon nanotube layer and the surface of the prefabricated soft carbon felt is strong, the mechanical property of the carbon nanotube can be effectively applied, the obtained light high-strength heat preservation felt cannot crack and delaminate, the bending strength is high, the service life is effectively prolonged, the process is simple, the energy is saved, the manufacturing cost is reduced, a series of problems of the existing heat preservation felt are fundamentally solved, and the heat preservation and insulation effect of the heat preservation furnace is good.
The melamine nano sponge has light porous quality, is convenient to use, has certain flexibility and deformability compared with metal foam, and can change the thickness and the density of pores according to the external pressure condition even after carbonization treatment, so that the melamine nano sponge has good foldability and thermal insulation performance, and the application range is wider. The surface of the microstructure of the prefabricated soft carbon felt prepared by carbonizing the melamine nano sponge has certain roughness, and when the carbon nano tubes grow in situ subsequently, catalyst particles can be better supported, so that small molecules generated by hydrocarbon decomposition are better combined on the surface of the prefabricated soft carbon felt, and the carbon nano tubes which are more uniform, have good crystallinity and high purity are generated.
When the prefabricated soft carbon felt is prepared, the melamine nano sponge is directly used for carbonization, the carbon fiber preform forming process is not needed, the cost is relatively low, and the prefabricated soft carbon felt is soft, low in density, low in heat conductivity coefficient, uniform in thermal field and high in porosity.
The melamine nano sponge with certain density is adopted, so that the porosity of the prefabricated soft carbon felt is effectively ensured. The thickness of the melamine nano sponge can be determined according to actual needs.
In the vapor deposition step, the metal element compound is reduced into metal particles in the atmosphere of reducing gas, the metal particles are deposited on the surface of the substrate to be used as a catalyst for growing the carbon nano tube, carbon source gas (hydrocarbon) is decomposed at high temperature to generate small molecular chains, and then the carbon nano tube is generated under the action of the catalyst. Wherein the temperature of 300-500 ℃ is the temperature of the furnace body, the preparation is made for the subsequent deposition, and then the temperature is increased to 650-850 ℃ selectively, because the decomposition rate of reactants in the temperature range is stable, the activity is moderate, and finally the carbon nano tube with uniform deposition and better quality is obtained.
The invention reasonably selects carbon source gas, metal element compounds and the like, and can ensure that the carbon nano tubes uniformly grow on the prefabricated soft carbon felt by adjusting parameters such as heating rate, flow and the like.
The light high-strength heat preservation felt prepared by the invention has small density which is between 0.03 and 0.18g/cm 3 And the density of the carbon felt is lower than that of the common carbon felt, the heat conductivity coefficient is 0.05-0.3W/(m.K), and the bending strength can reach 15-20MPa.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Those skilled in the art who do not specify any particular technique or condition in the examples can follow the techniques or conditions described in the literature in this field or follow the product specification.
Example 1
A light high-strength heat preservation felt comprises a prefabricated soft carbon felt, wherein a carbon nanotube layer is covered on the surface of the prefabricated soft carbon felt.
The preparation method of the light high-strength heat preservation felt specifically comprises the following steps:
1) The density is 0.01g/cm 3 And melamine nano sponge with the thickness of 2cm is laid on a tool and then placed in a carbonization furnace, under the argon atmosphere, the carbonization furnace is quickly heated to 200 ℃ at the heating rate of 10 ℃/min and is kept at the constant temperature for 60min, then the temperature is heated to 350 ℃ at the heating rate of 0.2 ℃/min and is kept at the constant temperature for 120min, and then the temperature is kept at 5 ℃/mAnd raising the temperature to 750 ℃ at the in heating rate, keeping the temperature for 30min, raising the temperature to 950 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 15min, raising the temperature to 1000 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 120min, and cooling the temperature to room temperature along with the furnace to obtain the prefabricated soft carbon felt.
2) Placing the prefabricated soft carbon felt on a growth carrying platform of a chemical vapor deposition furnace (CVD system furnace), then placing the prefabricated soft carbon felt into a CVD reaction cavity of the chemical vapor deposition furnace, sealing the CVD reaction cavity, heating the chemical vapor deposition furnace to 300 ℃ at a heating rate of 10 ℃/min under a vacuum state, keeping the temperature for 60min, then heating to 650 ℃ at a heating rate of 5 ℃/min, heating and gasifying ferric chloride, then continuously entering the CVD reaction cavity along with reaction gas, controlling the heat preservation time to be 10min, and growing a carbon nano tube on the surface of the prefabricated soft carbon felt in situ; and stopping introducing the gas after the reaction is finished, vacuumizing, freely cooling to room temperature, and discharging.
The reaction gas is a mixed gas of methane and reducing gas, the flow of the reaction gas is adjusted to 90sccm, and the volume ratio of the methane to the reducing gas is 1:3; the reducing gas is a mixed gas of hydrogen and argon, and the volume ratio of the hydrogen to the argon is 1:2. the gasification flow rate of ferric chloride was 150sccm.
The overall bulk density of the lightweight high-strength insulation felt carbon prepared in the example is 0.03g/cm 3 The thermal conductivity coefficient is 0.05W/(m.K), the bending strength is 15MPa, and the mass of the carbon nano tube is 0.5wt% of the total mass of the heat preservation felt carbon.
Example 2
A light high-strength heat preservation felt comprises a prefabricated soft carbon felt, wherein a carbon nanotube layer is covered on the surface of the prefabricated soft carbon felt.
The preparation method of the light high-strength heat preservation felt specifically comprises the following steps:
1) The density is 0.01g/cm 3 And melamine nano sponge with the thickness of 2cm is laid on a tool and then placed in a carbonization furnace, under the argon atmosphere, the carbonization furnace is quickly heated to 250 ℃ at the heating rate of 10 ℃/min firstly and is kept at the constant temperature for 15min, then the temperature is heated to 400 ℃ at the heating rate of 1 ℃/min and is kept at the constant temperature for 30min, then the temperature is heated to 700 ℃ at the heating rate of 1 ℃/min and is kept at the constant temperature for 120min, and then the temperature is heated at the heating rate of 0.2 ℃/minRaising the temperature to 900 ℃ at a speed rate, keeping the temperature for 60min, then raising the temperature to 1200 ℃ at a temperature rise rate of 5 ℃/min, keeping the temperature for 60min, and then cooling to room temperature along with the furnace to obtain the prefabricated soft carbon felt.
2) Placing the prefabricated soft carbon felt on a growth carrying platform of a chemical vapor deposition furnace (CVD system furnace), then placing the prefabricated soft carbon felt into a CVD reaction cavity of the chemical vapor deposition furnace, sealing the CVD reaction cavity, heating the chemical vapor deposition furnace to 500 ℃ at a heating rate of 10 ℃/min under a vacuum state, keeping the temperature for 30min, then heating to 850 ℃ at a heating rate of 10 ℃/min, heating and gasifying cobalt chloride, then continuously entering the CVD reaction cavity along with reaction gas, controlling the heat preservation time to be 10min, and growing a carbon nano tube on the surface of the prefabricated soft carbon felt in situ; and stopping introducing gas after the reaction is finished, vacuumizing, freely cooling to room temperature, and discharging.
The reaction gas is a mixed gas of ethylene and reducing gas, the flow rate of the reaction gas is regulated to 350sccm, and the volume ratio of the ethylene to the reducing gas is 1:5, the reducing gas is a mixed gas of hydrogen and argon, and the volume ratio of the hydrogen to the argon is 1:5. the gasification flow rate of cobalt chloride was 250sccm.
The overall bulk density of the lightweight high-strength insulation felt carbon prepared in the example is 0.08g/cm 3 The thermal conductivity coefficient is 0.25W/(m.K), the bending strength reaches 15.8MPa, and the mass of the carbon nano tube is 0.65wt% of the total mass of the heat preservation felt carbon.
Example 3
A light high-strength heat preservation felt comprises a prefabricated soft carbon felt, wherein a carbon nanotube layer is covered on the surface of the prefabricated soft carbon felt.
The preparation method of the light high-strength heat preservation felt specifically comprises the following steps:
1) The density is 0.01g/cm 3 The melamine nano sponge with the thickness of 2cm is laid on a tool and then placed in a carbonization furnace, the carbonization furnace is quickly heated to 250 ℃ at the heating rate of 10 ℃/min under the argon atmosphere, the temperature is kept for 30min, then the temperature is increased to 400 ℃ at the heating rate of 0.5 ℃/min, the temperature is kept for 60min, then the temperature is increased to 700 ℃ at the heating rate of 3 ℃/min, the temperature is kept for 80min, then the temperature is increased to 930 ℃ at the heating rate of 0.6 ℃/min, the temperature is kept for 40min, and then the temperature is increased at the heating rate of 3 ℃/minHeating to 1200 ℃, keeping the temperature for 90min, and cooling to room temperature along with the furnace to obtain the prefabricated soft carbon felt.
2) Placing the prefabricated soft carbon felt on a growth carrying platform of a chemical vapor deposition furnace (CVD system furnace), then placing the prefabricated soft carbon felt into a CVD reaction cavity of the chemical vapor deposition furnace, sealing the CVD reaction cavity, heating the chemical vapor deposition furnace to 400 ℃ at a heating rate of 10 ℃/min under a vacuum state, keeping the temperature for 40min, then heating to 800 ℃ at a heating rate of 10 ℃/min, heating and gasifying nickel chloride, then continuously entering the CVD reaction cavity along with reaction gas, controlling the heat preservation time to be 30min, and growing a carbon nano tube on the surface of the prefabricated soft carbon felt in situ; and stopping introducing the gas after the reaction is finished, vacuumizing, freely cooling to room temperature, and discharging.
The reaction gas is a mixed gas of propane and a reducing gas, the flow rate of the reaction gas is regulated to be 220sccm, and the volume ratio of the propane to the reducing gas is 1:6, the reducing gas is a mixed gas of hydrogen and argon, and the volume ratio of the hydrogen to the argon is 1:5. the gasification flow rate of nickel chloride was 300sccm.
The overall bulk density of the lightweight high-strength insulation felt carbon prepared in the example is 0.15/cm 3 The thermal conductivity coefficient is 0.23W/(m.K), the bending strength reaches 16MPa, and the mass of the carbon nano tube is 0.85wt% of the total mass of the heat preservation felt carbon.
Example 4
A light high-strength heat preservation felt comprises a prefabricated soft carbon felt, wherein a carbon nanotube layer is covered on the surface of the prefabricated soft carbon felt.
The preparation method of the light high-strength heat preservation felt comprises the following steps:
1) The density is 0.01g/cm 3 And melamine nano sponge with the thickness of 2cm is laid on a tool and then placed in a carbonization furnace, the carbonization furnace is quickly heated to 250 ℃ at the heating rate of 10 ℃/min under the argon atmosphere, the temperature is kept for 30min, then the temperature is heated to 400 ℃ at the heating rate of 0.5 ℃/min, the temperature is kept for 60min, then the temperature is heated to 700 ℃ at the heating rate of 3 ℃/min, the temperature is kept for 80min, then the temperature is heated to 930 ℃ at the heating rate of 0.6 ℃/min, the temperature is kept for 40min, then the temperature is heated to 1200 ℃ at the heating rate of 3 ℃/min, the temperature is kept for 90min, and then the furnace is cooled to the room temperature to obtain the prefabricated partA soft carbon felt.
2) Placing the prefabricated soft carbon felt on a growth carrying platform of a chemical vapor deposition furnace (CVD system furnace), then placing the prefabricated soft carbon felt into a CVD reaction cavity of the chemical vapor deposition furnace, sealing the CVD reaction cavity, heating the chemical vapor deposition furnace to 450 ℃ at a heating rate of 10 ℃/min under a vacuum state, keeping the temperature for 40min, then heating to 800 ℃ at a heating rate of 10 ℃/min, heating and gasifying nickel chloride, then continuously entering the CVD reaction cavity along with reaction gas, controlling the heat preservation time to be 35min, and growing a carbon nano tube on the surface of the carbon felt in situ; and stopping introducing gas after the reaction is finished, vacuumizing, freely cooling to room temperature, and discharging.
The reaction gas is a mixed gas of propane and a reducing gas, the flow rate of the reaction gas is regulated to be 220sccm, and the volume ratio of the propane to the reducing gas is 1: and 8, the reducing gas is a mixed gas of hydrogen and argon, and the volume ratio of the hydrogen to the argon is 1:6. the vaporization flow rate of nickel chloride was 350sccm.
The overall bulk density of the lightweight high-strength insulation felt carbon prepared in the example is 0.16/cm 3 The thermal conductivity coefficient is 0.22W/(m.K), the bending strength reaches 16.5MPa, and the mass of the carbon nano tube is 0.85wt% of the total mass of the heat preservation felt carbon.
Example 5
A light high-strength heat preservation felt comprises a prefabricated soft carbon felt, wherein a carbon nanotube layer is covered on the surface of the prefabricated soft carbon felt.
The preparation method of the light high-strength heat preservation felt comprises the following steps:
1) The density is 0.01g/cm 3 And the melamine nano sponge with the thickness of 2cm is laid on a tool and then placed in a carbonization furnace, under the argon atmosphere, the carbonization furnace is quickly heated to 250 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 45min, then the temperature is heated to 400 ℃ at the heating rate of 0.5 ℃/min, the temperature is kept for 50min, then the temperature is heated to 700 ℃ at the heating rate of 3 ℃/min, the temperature is kept for 100min, then the temperature is heated to 930 ℃ at the heating rate of 0.6 ℃/min, the temperature is kept for 40min, then the temperature is heated to 1200 ℃ at the heating rate of 3 ℃/min, the temperature is kept for 90min, and then the furnace is cooled to the room temperature to obtain the prefabricated soft carbon felt.
2) Placing the prefabricated soft carbon felt on a growth carrying platform of a chemical vapor deposition furnace (CVD system furnace), then placing the prefabricated soft carbon felt into a CVD reaction cavity of the chemical vapor deposition furnace, sealing the CVD reaction cavity, heating the chemical vapor deposition furnace to 400 ℃ at a heating rate of 10 ℃/min under a vacuum state, keeping the temperature for 40min, then heating to 800 ℃ at a heating rate of 10 ℃/min, heating and gasifying nickel chloride, then continuously entering the CVD reaction cavity along with reaction gas, controlling the heat preservation time to be 30min, and growing a carbon nano tube on the surface of the prefabricated soft carbon felt in situ; and stopping introducing gas after the reaction is finished, vacuumizing, freely cooling to room temperature, and discharging.
The reaction gas is a mixed gas of propane and a reducing gas, the flow rate of the reaction gas is regulated to 220sccm, and the volume ratio of the propane to the reducing gas is 1: and 8, the reducing gas is a mixed gas of hydrogen and argon, and the volume ratio of the hydrogen to the argon is 1:8. the vaporization flow rate of nickel chloride was 400sccm.
The overall bulk density of the lightweight high-strength insulation felt carbon prepared in the example is 0.18g/cm 3 The thermal conductivity coefficient is 0.3W/(m.K), the bending strength reaches 20MPa, and the mass of the carbon nano tube is 0.85wt% of the total mass of the heat preservation felt carbon.
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. A preparation method of a light high-strength heat preservation felt is characterized by comprising the following steps: the light high-strength heat preservation felt comprises a prefabricated soft carbon felt, wherein a carbon nanotube layer is covered on the surface of the prefabricated soft carbon felt;
the preparation method of the prefabricated soft carbon felt comprises the following steps: placing melamine nano sponge into a carbonization furnace, rapidly heating to 200-250 ℃ in a vacuum state or in an inert gas atmosphere, keeping the temperature for 15-60min, then heating to 350-400 ℃ at a heating rate of 0.2-1 ℃/min, keeping the temperature for 30-120min, then heating to 700-750 ℃ at a heating rate of 1-5 ℃/min, keeping the temperature for 30-120min, then heating to 900-950 ℃ at a heating rate of 0.2-1 ℃/min, keeping the temperature for 15-60min, then heating to 1000-1200 ℃ at a heating rate of 1-5 ℃/min, keeping the temperature for 60-120min, and cooling to room temperature with the furnace to obtain a prefabricated soft carbon felt;
the preparation method of the light high-strength heat preservation felt comprises the following steps: placing the prefabricated soft carbon felt into a reaction cavity of a chemical vapor deposition furnace, sealing the reaction cavity, heating the chemical vapor deposition furnace to 300-500 ℃ in a vacuum state, keeping the temperature for 30-60min, then heating to 650-850 ℃, heating and gasifying a metal element compound, continuously feeding the metal element compound into the reaction cavity along with reaction gas, preserving the temperature for 10-45min, and growing a carbon nano tube on the surface of the prefabricated soft carbon felt in situ, wherein the reaction gas is mixed gas of carbon source gas and reducing gas; and stopping introducing the gas after the reaction is finished, vacuumizing, freely cooling to room temperature, and discharging to obtain the light high-strength heat-insulating felt.
2. The method for preparing the light-weight high-strength heat preservation felt according to claim 1, characterized in that: the density of the melamine nano sponge is 0.008-0.01g/cm 3 。
3. The method for preparing the light-weight high-strength heat preservation felt according to claim 1, characterized in that: heating to 300-500 ℃ at a heating rate of 5-10 ℃/min; heating to 650-850 ℃ at a heating rate of 5-10 ℃/min.
4. The method for preparing the light-weight high-strength heat preservation felt according to claim 1, characterized in that: the flow rate of the reaction gas is 90-350sccm, and the volume ratio of the carbon source gas to the reducing gas in the reaction gas is 1: (3-8), the carbon source gas is a mixed gas of any one or more of methane, ethylene, propane and propylene, the reducing gas is a mixed gas of hydrogen and an inert gas, and the volume ratio of the hydrogen to the inert gas is 1: (2-8).
5. The method for preparing the light-weight high-strength heat-insulating felt according to claim 1, characterized in that: the metal element compound is chloride of at least one of metal iron, molybdenum, cobalt, nickel, copper and chromium, and the gasification flow rate of the metal element compound is 150-400sccm.
6. Use of the lightweight high-strength insulation mat prepared by the preparation method according to any one of claims 1 to 5 in heat preservation and insulation of a heat preservation furnace.
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Denomination of invention: A lightweight and high-strength insulation felt and its preparation method and application Effective date of registration: 20230628 Granted publication date: 20221216 Pledgee: Suixi Jinmao financing Company limited by guarantee Pledgor: Anhui Hongchang New Materials Co.,Ltd. Registration number: Y2023980046214 |
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