CN114656270A - Carbon-ceramic fiber heat-insulation composite material and preparation method thereof - Google Patents
Carbon-ceramic fiber heat-insulation composite material and preparation method thereof Download PDFInfo
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- CN114656270A CN114656270A CN202210237232.3A CN202210237232A CN114656270A CN 114656270 A CN114656270 A CN 114656270A CN 202210237232 A CN202210237232 A CN 202210237232A CN 114656270 A CN114656270 A CN 114656270A
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- 239000000835 fiber Substances 0.000 title claims abstract description 234
- 239000000919 ceramic Substances 0.000 title claims abstract description 129
- 238000009413 insulation Methods 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 183
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 119
- 239000004917 carbon fiber Substances 0.000 claims abstract description 119
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 109
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 91
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 76
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 49
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000005011 phenolic resin Substances 0.000 claims abstract description 36
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 36
- 239000012774 insulation material Substances 0.000 claims abstract description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005096 rolling process Methods 0.000 claims description 24
- 238000003763 carbonization Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 17
- 238000005507 spraying Methods 0.000 claims description 11
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 8
- 238000009960 carding Methods 0.000 claims description 7
- 238000005087 graphitization Methods 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000003754 machining Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000011224 oxide ceramic Substances 0.000 claims description 2
- 229910052574 oxide ceramic Inorganic materials 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 20
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000005336 cracking Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000032798 delamination Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 169
- 239000007787 solid Substances 0.000 description 12
- 238000012546 transfer Methods 0.000 description 11
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 9
- 229910010271 silicon carbide Inorganic materials 0.000 description 9
- 230000005855 radiation Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
- 230000000903 blocking effect Effects 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 5
- 239000011810 insulating material Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000003085 diluting agent Substances 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007770 graphite material Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
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Abstract
The invention belongs to the technical field of carbon fiber ceramic composite materials, and particularly relates to a novel carbon ceramic fiber heat insulation material and a preparation method thereof. Comprising, at least one non-woven felt layer of carbon fibers; at least one layer of ceramic fiber mat; the ceramic fiber felt layer is arranged outside the carbon fiber non-woven felt layer, and phenolic resin is sprayed between the ceramic fiber felt layer and the carbon fiber non-woven felt layer; the ceramic fiber felt layer is composed of one or more of alumina and/or silicon dioxide fibers. The carbon fiber ceramic composite material provided by the invention has better electromagnetic wave scattering property, better oxidation resistance, better heat insulation effect and lower thermal conductivity, and effectively solves the technical problems of high manufacturing cost, poor heat insulation effect, easy delamination, cracking and the like of the existing heat insulation and heat insulation materials.
Description
Technical Field
The invention belongs to the technical field of carbon fiber ceramic composite materials, and particularly relates to a novel carbon ceramic fiber heat insulation material and a preparation method thereof.
Background
In the production process of an industrial vacuum furnace and a single crystal growth furnace, the carbon emission is reduced, the effective utilization rate of heat energy is increased, so that the energy consumption of an enterprise is reduced, the production cost is saved, and the technical problem to be solved is always needed. Then the heat insulating material in the prior art has high cost, high heat conductivity and long product manufacturing period, thereby causing a vacuum furnace or a crystal growth furnace to have low effective utilization rate of heat energy, high energy consumption and overhigh production cost. The existing heat insulation material has high manufacturing cost and poor heat insulation effect and can not meet the technical problem of the existing process requirement.
Disclosure of Invention
The invention provides a novel carbon-ceramic fiber heat insulation composite material, which solves the technical problem that a carbon fiber heat insulation material in the existing ultrahigh-temperature vacuum environment is high in cost and poor in heat insulation effect.
In order to achieve the above objects, according to one aspect of the present invention, there is provided a carbon ceramic fiber thermal insulation composite material including,
at least one non-woven felt layer of carbon fibers;
at least one layer of ceramic fiber mat;
the ceramic fiber felt layer is arranged outside the carbon fiber non-woven felt layer, and phenolic resin is sprayed between the ceramic fiber felt layer and the carbon fiber non-woven felt layer; the phenolic resin is liquid and/or powder;
the ceramic fiber felt layer is composed of one or more of alumina and/or silicon dioxide fibers.
Further, a carbon fiber non-woven felt layer filled with alumina fiber or alumina ceramic fiber felt is arranged outside the ceramic fiber felt layer of the carbon-ceramic fiber heat-insulation composite material.
Further, the ceramic fiber felt layer is a silicon dioxide fiber felt layer, a connecting layer is further arranged between the carbon fiber non-woven felt layer and the silicon dioxide fiber felt layer, and the connecting layer is a carbon fiber and silicon dioxide fiber mixed felt layer; phenolic resin is sprayed among the carbon fiber non-woven felt layer, the connecting layer and the silicon dioxide fiber felt layer.
Furthermore, a carbon fiber non-woven felt body is further arranged outside the silicon dioxide fiber felt body layer, and phenolic resin is sprayed between the silicon dioxide fiber felt body layer and the carbon fiber non-woven felt body layer.
Further, the carbon-ceramic fiber heat insulation composite material is subjected to carbon/graphitization treatment.
Further, one or more of alumina and/or silicon dioxide fibers are added into the carbon fiber non-woven felt layer.
Further, the carbon fiber non-woven felt layer on the inner layer of the carbon-ceramic fiber heat insulation composite material is a high-temperature area of a heat insulation material, the carbon fiber and ceramic fiber mixed felt layer is a connecting area, the silicon dioxide fiber felt layer is a low-temperature area of the heat insulation material, and the carbon fiber non-woven felt layer on the outer layer is a material protection area.
Furthermore, more than 90% of carbon fibers and silicon dioxide fibers in the connecting layer are arranged along the circumferential direction or parallel to the cylindrical axis direction of the carbon ceramic fibers.
In another aspect of the invention, a preparation method of a carbon-ceramic fiber heat insulation composite material is provided, which comprises the following steps of (1) respectively cutting a carbon fiber tow and a ceramic fiber tow; (2) respectively putting the cut carbon fiber tows and the ceramic fiber tows into an opening and carding machine for opening treatment; (3) laying the loosened carbon fiber tows and the loosened ceramic fiber tows into a carbon fiber net tire felt, a ceramic fiber net tire and a carbon-ceramic mixed fiber net tire through a carding machine; (4) rolling the laid carbon fiber mesh felt into a carbon fiber non-woven felt layer with the thickness of 60mm by an automatic rounding forming machine, then rolling a carbon ceramic mixed fiber mesh felt outside the carbon fiber non-woven felt layer, spraying phenolic resin while rolling to form a carbon ceramic fiber mixed felt layer with the thickness of 20mm, rolling a ceramic fiber mesh felt after finishing the carbon ceramic fiber mixed felt layer, spraying phenolic resin while rolling to form a ceramic fiber mesh felt with the thickness of 50mm, rolling a carbon fiber non-woven felt layer with the thickness of 10mm after finishing the ceramic fiber mesh felt; (5) putting the formed carbon-ceramic fiber heat-insulation composite material with the four-layer structure into a mold, putting the carbon-ceramic fiber heat-insulation composite material and the mold into an oven with the temperature of more than 200 ℃, and curing and molding for 2 hours to form a 125mm carbon-ceramic fiber heat-insulation composite material; (6) putting the cured carbon-ceramic fiber heat-insulating composite material into a carbonization furnace at the temperature of 2000 ℃ for high-temperature treatment for 5 hours; (7) machining the appearance according to the requirement; (8) and coating a graphite coating on the outer layer to obtain a finished product.
Further, the preparation method of the carbon-ceramic fiber heat insulation composite material is characterized by comprising the following steps: in the step (6), the carbonization furnace at 2000 ℃ is used for internal heating, and the carbon ceramic heat-insulating barrel is arranged outside the heater, so that the processing temperature of the ceramic fiber felt layer is below 1000 ℃ when the processing temperature of the inner-layer carbon fiber non-woven felt layer structure is 2000 ℃, the critical use temperature of the silicon dioxide fiber is ensured, and meanwhile, the heat utilization efficiency is effectively improved.
Compared with the prior art, the invention has the beneficial effects that: according to the carbon-ceramic fiber heat-insulation composite material, the carbon fiber non-woven felt layer is arranged as the inner layer, and the carbon-ceramic fiber heat-insulation composite material is arranged as the ceramic fiber felt layer, so that the heat-insulation effect of the heat-insulation material is better, and the cost is lower.
Drawings
Fig. 1 is a schematic structural view of the present invention.
FIG. 2 shows the results of the thermal insulation effect test of the present invention and a pure carbon fiber thermal insulation material under the same conditions.
Description of reference numerals: 1. an inner layer; 2. a connection layer; 3. an intermediate layer; 4. and (4) an outer layer.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The terms "first" and "second," and the like, in the description and in the claims of embodiments of the present invention are used for distinguishing between different objects and not for describing a particular order of the objects. For example, the first parameter set and the second parameter set, etc. are used to distinguish different parameter sets, rather than to describe a particular order of parameter sets.
In the description of the embodiments of the present invention, the meaning of "a plurality" means two or more unless otherwise specified. For example, a plurality of elements refers to two elements or more.
The term "and/or" herein is an association relationship describing an associated object, and means that there may be three relationships, for example, a display panel and/or a backlight, which may mean: there are three cases of a display panel alone, a display panel and a backlight together, and a backlight alone. The symbol "/" herein denotes a relationship in which the associated object is or, for example, input/output denotes input or output.
In the present embodiments, words such as "exemplary" or "for example" are used to indicate examples, illustrations or descriptions. Any embodiment or design described as "exemplary" or "e.g.," an embodiment of the present invention is not necessarily to be construed as preferred or advantageous over other embodiments or designs. Rather, use of the word "exemplary" or "such as" is intended to present concepts related in a concrete fashion.
In order to solve the technical problem that the existing heat insulation material is high in cost and poor in heat insulation effect, the embodiment of the invention provides a carbon-ceramic fiber heat insulation composite material, which comprises at least one carbon fiber non-woven felt layer; at least one layer of ceramic fiber mat; the ceramic fiber felt layer is arranged outside the carbon fiber non-woven felt layer, and phenolic resin is sprayed between the ceramic fiber felt layer and the carbon fiber non-woven felt layer; the ceramic fiber felt layer is composed of one or more of alumina and/or silicon dioxide fibers. Therefore, the ceramic fiber and the carbon fiber are combined, and the silicon dioxide fiber and the aluminum oxide are combined, so that the manufacturing cost is lower while the heat insulation effect is improved.
Example 1, the carbon-ceramic fiber thermal insulation composite comprises, a layer of carbon fiber nonwoven felt; a silica fiber felt layer; the silica fiber felt layer is arranged outside the carbon fiber non-woven felt layer. The carbon-ceramic fiber heat-insulation composite material is characterized in that a connecting layer is further arranged between the carbon fiber non-woven felt layer and the silicon dioxide fiber felt layer, and the connecting layer is a carbon fiber and silicon dioxide fiber mixed felt layer; phenolic resin is sprayed among the carbon fiber non-woven felt layer, the connecting layer and the silicon dioxide fiber felt layer; the phenolic resin is a liquid. The carbon fiber and silicon dioxide fiber mixed felt layer is manufactured by mixing the carbon fiber and the silicon dioxide fiber, so that the technical problems of easy cracking and fracture of interface connection of two different materials and high connection strength and difficulty in layered cracking are solved through the felt body prepared after mixing the two fibers.
Example 2, as shown in fig. 1, the carbon-ceramic fiber thermal insulation composite material comprises an inner layer 1, wherein the inner layer 1 is a carbon fiber non-woven felt layer; the connecting layer 2 is a carbon fiber and silicon dioxide fiber mixed felt layer, is arranged between the inner layer and the silicon dioxide fiber felt layer, and is prepared by mixing carbon fibers and silicon dioxide fibers in a ratio of 1: 1; and the middle layer 3 is silica fiber. The silicon dioxide fiber felt layer is connected with the inner layer 1 through the connecting layer 2; an outer layer 4, wherein the outer layer 4 is a carbon fiber non-woven felt body; phenolic resin is also sprayed among the inner layer 1, the connecting layer 2, the middle layer 3 and the outer layer 4; the phenolic resin is powder. The carbon-ceramic fiber heat insulation composite material is subjected to carbon/graphitization treatment. Thereby make whole carbon ceramic fiber thermal-insulated combined material, manufacturing cost is lower, and thermal-insulated effect is better, through the use of the mixed felt layer of tie layer 2 carbon fiber and silica fiber to through the felt body of two kinds of fibre preparation after mixing, the interface connection easy fracture of having solved two kinds of different materials, cracked technical problem makes joint strength higher, is difficult for the layering fracture.
Illustratively, the intermediate layer 3 is alumina fiber.
Illustratively, the intermediate layer 3 is composed of fibers (silicate fibers) synthesized from alumina and silica in a ratio of 1: 5. In addition, the phenolic resin is used as the adhesive, so that the aluminum oxide and the silicon dioxide fibers are effectively connected after carbonization treatment, and the technical problem that the aluminum oxide and the silicon dioxide fibers cannot be combined into the solid fibrofelt in the prior art is solved. Meanwhile, the good infrared radiation blocking effect of the aluminum oxide further improves the heat blocking effect of the middle layer. Further spraying phenolic resin on the surface of the silicon dioxide fiber, and performing high-temperature treatment to obtain a skin-core structure, wherein the core is tridymite, and the skin layer forms a residual carbon layer/silicon carbide layer (SiO)2+3C＝SiO2+2CO) is converted from the original infrared penetration to reflection, absorbing the infrared radiation effect, and further improving the heat insulation effect.
Illustratively, the outside of the body layer of the ceramic fiber felt of the carbon ceramic fiber heat insulation composite material,and a carbon fiber non-woven felt layer with an outer layer filled with alumina fiber or alumina ceramic fiber felt is also arranged. The phenolic resin is sprayed in alumina or silicon dioxide fiber and carbonized at 1000 ℃ after being cured at 200 ℃. A carbon layer/silicon carbide layer is deposited on the surface of the silicon dioxide fiber (the carbon layer and the surface of the silicon dioxide fiber are subjected to gas-solid reaction at high temperature to form the silicon carbide layer (SiO)2+3C＝SiO2+2CO) and a residual carbon layer). The thermal insulation material has a higher infrared blocking effect, and a silicon carbide layer formed after phenolic resin carbonization further plays roles in reflection and absorption, so that the thermal conductivity of the thermal insulation material is obviously reduced.
Illustratively, the carbon-ceramic fiber thermal insulation composite material is subjected to a carbon/graphitization treatment.
Illustratively, one or more of alumina and/or silica fibers are added to the carbon fiber nonwoven felt layer.
Illustratively, the carbon fiber non-woven felt layer of the inner layer 1 of the carbon-ceramic fiber heat-insulation composite material is a heat-insulation material high-temperature layer, the carbon fiber and ceramic fiber mixed felt layer is a connecting layer 2, and the silicon dioxide fiber felt layer is an intermediate layer 3, so that a heat-insulation material low-temperature region is formed; the outer layer 4 is a carbon fiber non-woven felt layer as a material protection zone. The thermal conductivity of the carbon graphite material is gradually reduced along with the temperature rise, the thermal conductivity of the silicon dioxide material is rapidly increased along with the temperature rise, and the thermal conductivity of the silicon dioxide is lower than that of the carbon graphite material. The carbon material in the high-temperature area has better infrared absorption and reflection effects, the heat transfer mainly based on heat radiation conduction is reduced by utilizing the property of the carbon material, and the heat transfer of the fiber solid is reduced by utilizing the low thermal conductivity of the silicon dioxide solid in the low-temperature area. The carbon-ceramic heat insulation composite material prepared by utilizing the physical properties of the two materials has lower heat conductivity, so that the composite material has higher absorption, scattering and reflection effects on infrared radiation, and the high-temperature radiation heat transfer and the low-temperature solid heat transfer of the thermal field material are obviously reduced. The cost of the carbon fiber is 3-4 times of that of the silicon dioxide fiber, and the cost of the thermal field is saved by more than one time in material use.
Illustratively, more than 90% of the carbon fibers and the silica fibers in the connecting layer are arranged along the circumferential direction or parallel to the axial direction of the carbon ceramic fiber cylindrical heat-insulating composite material. Therefore, through the physical properties of the crystal structure in the fiber and the difference between the radial thermal conductivity and the axial thermal conductivity of the fiber, the fiber is arranged along the circumferential direction after the arrangement mode is selected, so that the thermal conductivity can be extremely reduced, and the heat insulation effect is improved.
Illustratively, more than 90% of the carbon fibers and the silica fibers in the connecting layer are arranged along the circumferential direction or parallel to the axial direction of the carbon ceramic fiber cylindrical heat insulation material.
In a preferred embodiment, as shown in fig. 1, the carbon-ceramic fiber heat insulation composite material comprises an inner layer 1, wherein the inner layer 1 is a carbon fiber non-woven felt layer; the connecting layer 2 is a carbon fiber and silicon dioxide fiber mixed felt layer and is arranged between the inner layer and the silicon dioxide fiber felt layer; the middle layer 3 is a silica fiber felt layer, and the silica fiber felt layer is connected with the inner layer 1 through a connecting layer 2; an outer layer 4, wherein the outer layer 4 is a carbon fiber non-woven felt body; phenolic resin is also sprayed among the inner layer 1, the connecting layer 2, the middle layer 3 and the outer layer 4; the carbon-ceramic fiber heat insulation composite material is subjected to carbon/graphitization treatment. The outer side 4 of the carbon-ceramic fiber heat-insulation composite material is a carbon fiber non-woven felt layer filled with aluminum oxide fibers or aluminum oxide ceramic fiber felts. Meanwhile, phenolic resin is sprayed in aluminum oxide and/or silicon dioxide fibers and subjected to 2000 ℃ carbon/graphitization through 200 ℃ curing, and a carbon layer/silicon carbide layer is deposited on the surfaces of the silicon dioxide fibers (the carbon layer and the surfaces of the silicon dioxide fibers are subjected to gas-solid reaction at high temperature to form a silicon carbide layer and a residual carbon layer). More than 60% of the carbon fibers and the silica fibers in the connecting layer are arranged along the circumferential direction (the arrangement mode is mainly to solve the connecting strength after the two fibers are mixed). The thermal insulation material has higher connection strength and better infrared blocking effect, thereby reducing the thermal conductivity of the thermal insulation material and the connection strength of the two fibers.
Embodiment 3, another aspect of the embodiments of the present invention, provides a method for preparing a carbon ceramic fiber heat insulation composite material, comprising the steps of, (1) cutting a carbon fiber tow and a silica fiber tow respectively; (2) respectively putting the cut carbon fiber tows and the cut silicon dioxide fiber tows into an opening carding machine for opening treatment; (3) laying the loosened carbon fiber tows and the loosened silicon dioxide fiber tows into a carbon fiber net tire felt, a silicon dioxide fiber net tire and a carbon fiber and silicon dioxide fiber mixed net tire through a carding machine; (4) rolling the laid carbon fiber mesh felt into a carbon fiber non-woven felt layer with the thickness of 60mm by an automatic rolling forming machine, then rolling a carbon fiber and silicon dioxide fiber mixed mesh on the carbon fiber non-woven felt layer in a ratio of 1:1, spraying phenolic resin while rolling to form a carbon fiber and silicon dioxide fiber mixed felt layer with the thickness of 20mm, rolling a silicon dioxide fiber mesh after finishing the carbon fiber and silicon dioxide fiber mixed felt layer, spraying phenolic resin while rolling to form a silicon dioxide fiber felt layer with the thickness of 50mm, and rolling a carbon fiber non-woven felt layer with the thickness of 10mm on the outer layer after finishing the ceramic fiber mesh; (5) putting the formed carbon ceramic fiber heat insulation composite material with the four-layer structure into a mold, putting the mold and the carbon ceramic fiber heat insulation composite material into an oven with the temperature of more than 200 ℃, and curing and molding for 2 hours to form a 125mm carbon ceramic fiber heat insulation material; (6) putting the cured carbon-ceramic fiber heat-insulating composite material into a carbonization furnace at the temperature of 2000 ℃ for high-temperature treatment for 5 hours; (7) machining the appearance according to the requirement; (8) and (4) coating a graphite coating on the surface of the product to obtain a finished product. Thus, a carbon layer/silicon carbide layer is deposited on the surface of a silicon dioxide fiber layer formed after phenolic resin carbonization, and the heat insulation effect is further improved.
Illustratively, in the step (6), the carbonization furnace at 2000 ℃ is used for internal heating, and the carbon ceramic heat-insulating barrel is arranged outside the heater, so that the processing temperature of the ceramic fiber felt layer is below 1000 ℃ when the processing temperature of the inner-layer carbon fiber non-woven felt layer structure is 2000 ℃, the critical use temperature of the silicon dioxide fiber is ensured, and meanwhile, the heat utilization efficiency is effectively improved.
Embodiment 4, a method for preparing a carbon-ceramic fiber heat insulation composite material, comprising the following steps, wherein in the preparation method, in the embodiment (1), carbon and ceramic fiber tows are respectively cut, the fiber diameter is 7um, and the fiber length is 2-3 mm; (2) separately putting the cut carbon fiber and ceramic fiber into an opener for opening treatment; (3) laying the loosened carbon and ceramic fiber yarns into a carbon fiber net tire felt and a ceramic fiber net tire through carding; (4) the method comprises the steps of sequentially rolling the opened and carded carbon fiber net tire, the carbon fiber and ceramic fiber mixed net tire, the silicon dioxide fiber net tire and the carbon fiber net tire according to the thickness requirement by using an automatic rolling forming machine, and uniformly spraying phenolic resin diluent in each layer of fiber net tire by using an automatic glue spraying device during rolling. Carbon-ceramic fiber: phenolic resin diluent 1: 0.5, the thickness of the first layer of carbon fiber net tire felt structure is 60mm, and the inner side 1 is formed; the thickness of the second layer structure carbon fiber and silicon dioxide fiber mixed net tire felt is 20mm, and a connecting layer 2 is formed; the thickness of the third layer structure silicon dioxide fiber net tire felt is 50mm, and a middle layer 3 is formed; the thickness of the carbon fiber net tire felt of the fourth layer structure is 10mm, and an outer layer is formed; (5) putting the formed carbon and ceramic fiber heat insulation material with the four-layer structure into a mold, compressing the heat insulation material, controlling the thickness to be 125mm, putting the heat insulation material and the mold into an oven with the temperature of more than 200 ℃, and curing and molding for 2 hours; (6) and then placing the cured carbon-ceramic fiber heat-insulating material into a special carbonization furnace at the temperature of 2000 ℃ for high-temperature treatment for 5 hours, and mechanically processing (8) the outer layer of the carbon-ceramic fiber heat-insulating material to be coated with a graphite coating layer through high-temperature shrinkage with the thickness of 120mm (7) to obtain a finished product.
In one embodiment of the invention, the carbon fiber filaments in the carbon fiber nonwoven felt body have a length of 2-3mm and a diameter of 7 um; the length of the silicon dioxide fiber is 2-3mm, and the diameter is 7 um.
Illustratively, the phenolic resin diluent is a phenolic resin: alcohol 1: 2 in a weight ratio.
Illustratively, the preparation method of the carbon-ceramic fiber heat insulation material is prepared by preparing carbon fibers with the diameter of 7um and the weight of 15kg, liquid phenolic resin with the weight of 10kg, alcohol with the weight of 20kg and silica fibers with the diameter of 7um and the weight of 20 kg.
The device comprises required equipment, carbon fiber weaving felt equipment, phenolic resin spraying equipment, a circular mould, a 200 ℃ oven, a 2000 ℃ vacuum carbonization/graphitization furnace, processing equipment and a vacuum thermal conductivity test furnace.
Testing of furnaces by vacuum thermal conductivity(steady state flat plate method thermal conductivity test), sampling 100 x 120mm thickness of the heat preservation cylinder, performing main performance test, sampling 100 x 120mm sample of the carbon ceramic fiber heat insulation material of the embodiment 2 of the invention at the ambient temperature of 10 ℃ and the RH ambient humidity of 80%, and taking the pure carbon fiber heat insulation material in the prior art as reference, wherein the sizes of the selected materials and the test parameters of the two tests are consistent. The main performance test was performed by using a vacuum thermal conductivity test furnace (steady state flat plate thermal conductivity test), sampling a pure carbon fiber composite product 100 x 120mm (thickness) from an insulation cylinder at an ambient temperature of 10 ℃ and an RH ambient humidity of 80%, and comparing the data of the experiment with the carbon fiber thermal insulation material shown in table 1, wherein the density was 0.2g/cm3, and the external temperature of the carbon fiber thermal insulation material was 115 ℃ according to the 30-minute steady state data of 1200 ℃ sampling in table 1. The thermal expansion coefficient of the carbon fiber in the parallel direction is 1.8x10-6K, and a compressive strength of 0.8 MPa. According to the embodiment of the application, the external temperature of the carbon-ceramic fiber heat-insulating material is 55 ℃, and the thermal expansion coefficient of the fiber in the parallel direction is lower than 1.9x10-6K, compressive strength 1.5MPa, density 0.11g/cm 3. Comparing the two, it can be seen that the density of the examples of the present application is reduced by 0.09g/cm compared with the prior art3The temperature difference is 60 ℃ at 1200 ℃, and the higher the temperature is, the more obvious the heat preservation effect is. The compressive strength is improved by 0.7Mpa, compared with the prior art, the performance is obviously improved in all aspects, and unexpected technical effects and obvious progress are achieved.
The invention has the advantages that the connection layer is formed by the felt body prepared by mixing two fibers, thereby solving the problems that the interface connection of two different materials is easy to crack and fracture; the fibers are uniformly arranged along the circumferential direction in an arrangement mode, so that the thermal conductivity efficiency is reduced to the maximum extent, the difference between the radial thermal conductivity and the axial thermal conductivity of the fibers is determined by more than several times through the physical properties of the internal crystal structures of the fibers, and the thermal conductivity can be reduced extremely when the fibers are arranged along the circumferential direction. Wherein, phenolic resin diluent is sprayed in the continuous felt preparation and is cured and molded at 200 ℃ by using a mold. The inner-layer carbon fiber non-woven felt body is used in a high-temperature area, and one or more of aluminum oxide and/or silicon dioxide fibers are filled in a low-temperature area of the outer layer of the carbon fiber non-woven felt body. The phenolic resin is sprayed in alumina and/or silicon dioxide fiber and carbonized at 2000 ℃ after being cured at 200 ℃. A silicon carbide layer and/or a carbon residue layer are formed on the surface of the silicon dioxide fiber (the carbon layer and the surface of the silicon dioxide fiber are subjected to gas-solid reaction at high temperature to form the silicon carbide layer). So that the thermal insulation material has higher infrared absorption and reflection effects, thereby reducing the thermal conductivity of the thermal insulation material. Carbon materials have a gradually decreasing thermal conductivity with increasing temperature. The thermal conductivity of the silicon dioxide material is rapidly increased when the temperature is higher than 800 ℃, and the thermal conductivity of the silicon dioxide material is lower than that of the carbon graphite material. The carbon material in the high-temperature area has better infrared absorption and reflection effects, the heat transfer mainly based on thermal radiation conduction is reduced by utilizing the property of the carbon material, the heat transfer of the fiber solid is reduced by utilizing the low thermal conductivity of the silicon dioxide solid in the low-temperature area, the heat transfer of the fiber solid is reduced, the low thermal conductivity is realized, so that the high-temperature absorption, scattering and reflection effects on infrared radiation are realized, and the high-temperature radiation heat transfer and the low-temperature solid heat transfer of the thermal field material are obviously reduced. The cost of the carbon fiber is 3-4 times of that of the silicon dioxide fiber, and the cost of the thermal field is saved by more than one time in material use.
The carbon ceramic fiber heat-insulating material provided by the embodiment of the invention has better high-temperature heat blocking effect, better oxidation resistance, better heat-insulating effect, lower heat conductivity, lower density and stronger pressure resistance.
By adding the alumina fiber and the silicon dioxide fiber into the carbon fiber matrix, the cost is lower, and the thermal conductivity is lower. The silicon dioxide material has low heat conductivity and high oxidation resistance, and has higher heat transfer resistance to infrared radiation and solid heat transfer in a low-temperature area by adding the silicon dioxide fiber surface spraying phenolic resin.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A carbon-ceramic fiber heat insulation composite material is characterized in that: the carbon-ceramic fiber heat insulation composite material comprises,
at least one non-woven felt layer of carbon fibers;
at least one layer of ceramic fiber mat;
the ceramic fiber felt layer is arranged outside the carbon fiber non-woven felt layer, and phenolic resin is sprayed between the ceramic fiber felt layer and the carbon fiber non-woven felt layer; the phenolic resin is liquid and/or powder.
The ceramic fiber felt layer is composed of one or more of alumina and/or silicon dioxide fibers.
2. The carbon-ceramic fiber thermal insulation composite material as claimed in claim 1, wherein: and a carbon fiber non-woven felt layer filled with aluminum oxide fibers or aluminum oxide ceramic fiber felts is arranged outside the ceramic fiber felt layer of the carbon-ceramic fiber heat-insulation composite material.
3. The carbon-ceramic fiber thermal insulation composite material as claimed in claim 1, wherein: the ceramic fiber felt layer is a silicon dioxide fiber felt layer, a connecting layer is further arranged between the carbon fiber non-woven felt layer and the silicon dioxide fiber felt layer, and the connecting layer is a carbon fiber and silicon dioxide fiber mixed felt layer; phenolic resin is sprayed among the carbon fiber non-woven felt layer, the connecting layer and the silicon dioxide fiber felt layer.
4. The carbon-ceramic fiber thermal insulation composite material as claimed in claim 3, wherein: and a carbon fiber non-woven felt body is further arranged outside the silicon dioxide fiber felt body layer, and phenolic resin is sprayed between the silicon dioxide fiber felt body layer and the carbon fiber non-woven felt body layer.
5. The carbon-ceramic fiber thermal insulation composite material as claimed in any one of claims 1 to 4, wherein: the carbon-ceramic fiber heat insulation composite material is subjected to carbon/graphitization treatment.
6. The carbon-ceramic fiber thermal insulation composite material as claimed in claim 5, wherein: one or more of alumina and/or silicon dioxide fibers are added into the carbon fiber non-woven felt layer.
7. The carbon-ceramic fiber thermal insulation composite material as claimed in claim 5, wherein: the carbon fiber non-woven felt layer on the inner layer of the carbon-ceramic fiber heat insulation composite material is a high-temperature area of a heat insulation material, the carbon fiber and ceramic fiber mixed felt layer is a connecting area, the silicon dioxide fiber felt layer is a low-temperature area of the heat insulation material, and the carbon fiber non-woven felt layer on the outer layer is a material protection area.
8. The carbon-ceramic fiber thermal insulation composite material as claimed in claim 3, wherein: more than 90% of carbon fibers and silicon dioxide fibers in the connecting layer are arranged along the circumferential direction or the direction parallel to the cylindrical axis of the carbon ceramic fibers.
9. A preparation method of a carbon-ceramic fiber heat insulation composite material is characterized by comprising the following steps: the method comprises the following steps of (1) respectively cutting carbon fiber tows and ceramic fiber tows; (2) respectively putting the cut carbon fiber tows and the ceramic fiber tows into an opening and carding machine for opening treatment; (3) laying the loosened carbon fiber tows and the loosened ceramic fiber tows into a carbon fiber net tire felt, a ceramic fiber net tire and a carbon-ceramic mixed fiber net tire through a carding machine; (4) rolling the laid carbon fiber mesh felt into a carbon fiber non-woven felt layer with required thickness by an automatic rolling forming machine, then rolling a carbon ceramic mixed fiber mesh layer outside the carbon fiber non-woven felt layer, spraying phenolic resin while rolling to form the carbon ceramic fiber mixed felt layer with required thickness, rolling a ceramic fiber mesh layer after finishing the carbon ceramic fiber mixed felt layer, spraying phenolic resin while rolling to form a ceramic fiber mesh layer with required thickness, rolling the carbon fiber non-woven felt layer with required thickness after finishing the ceramic fiber mesh layer, and rolling a carbon fiber non-woven felt layer with required thickness on the outer layer; (5) putting the formed carbon ceramic fiber heat insulation composite material with the four-layer structure into a mold, putting the mold and the carbon ceramic fiber heat insulation composite material into an oven with the temperature of more than 200 ℃, and curing and molding for more than 2 hours to form a 125mm carbon ceramic fiber heat insulation composite material; (6) putting the cured carbon-ceramic fiber heat-insulating composite material into a carbonization furnace at the temperature of 2000 ℃ for high-temperature treatment for 5 hours; (7) machining the appearance according to the requirement; (8) and coating a graphite coating on the surface of the finished product to obtain the finished product.
10. The preparation method of the carbon-ceramic fiber heat insulation composite material as claimed in claim 9, characterized in that: in the step (6), the carbonization furnace at 2000 ℃ is used for internal heating, and the carbon ceramic heat-insulating barrel is arranged outside the heater, so that the processing temperature of the ceramic fiber felt layer is below 1000 ℃ when the processing temperature of the inner-layer carbon fiber non-woven felt layer structure is 2000 ℃, the critical use temperature of the silicon dioxide fiber is ensured, and meanwhile, the heat utilization efficiency is effectively improved.
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