CN112743932B - Heat-proof integrated material and preparation method thereof - Google Patents
Heat-proof integrated material and preparation method thereof Download PDFInfo
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- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B9/047—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material made of fibres or filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/10—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a discontinuous layer, i.e. formed of separate pieces of material
- B32B3/18—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a discontinuous layer, i.e. formed of separate pieces of material characterised by an internal layer formed of separate pieces of material which are juxtaposed side-by-side
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- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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Abstract
The invention provides an integrated material for heat insulation and a preparation method thereof, which comprises a heat insulation layer, an enhancement layer and a heat protection layer, wherein the heat insulation layer comprises a silicon-based nano heat insulation material positioned on a cold surface layer and a gradient aluminum-silicon-based nano heat insulation material positioned on a hot surface layer, and the two heat insulation materials form cross splicing in the form of blocks; the heat insulation layer comprises a heat insulation layer and a reinforcing layer, wherein the reinforcing layer comprises a first reinforcing layer and a second reinforcing layer, the first reinforcing layer is an alumina composite material formed by coating six surfaces of 1-3 silicon-based nano heat insulation material blocks and aluminum-silicon-based nano heat insulation material blocks, and the second reinforcing layer is an alumina composite material formed by coating 3-20 layers of alumina composite material and is bonded with a hot surface layer of the heat insulation layer; the heat-proof layer is 1-3 layers of alumina composite material integrally coated with the heat-insulating layer and the enhancement layer. The invention adopts the integrated treatment of heat insulation and prevention, effectively combines the heat-proof layer with excellent oxidation resistance and ablation resistance with the heat-insulating layer with excellent heat-insulating property, improves the impact resistance of the surface and ensures the safety of a heat protection system.
Description
Technical Field
The invention belongs to the technical field of thermal protection materials, and particularly relates to an integrated material for preventing and insulating heat and a preparation method thereof.
Background
The thermal protection system is a key technology for restricting the final service capacity of the aerospace vehicle. Research and development in the aerospace field of various countries find that the thermal protection system of the aerospace vehicle gradually changes from ablation to non-ablation, and from heat protection and heat insulation separation to heat protection and heat insulation integration development. The successful launching of the X-37B aerospace vehicle draws wide attention, and particularly, a novel thermal protection system makes a great breakthrough. The novel integral toughening type fiber reinforced anti-oxidation composite material (TUFROC) thermal protection system is adopted, a design method of heat prevention and heat insulation integration is innovatively used, and the integrated connection of an anti-oxidation ablation outer layer and a high-toughness heat insulation base body is realized. The heat-proof layer and the heat-insulating layer are effectively combined in a mechanical connection mode, and coating treatment is uniformly carried out. The outer layer is a completely compact carbon-containing ceramic composite material, the inner layer is a porous low-density heat-insulating layer containing fibers, the surface coating is antioxidant and contains TaSi 2 、MoSi 2 、B 2 O 3 And so on. The novel composite material can bear the high temperature of 1700 ℃. T Pichon and Marlana N.Behnke et al developed a cover plate type heat-proof and heat-insulating integrated combined structure, and structural units of the combined structure are cover plate materials and heat-insulating materials for bearing mechanical load and are connected according to a specific mode. The cover plate material can be divided into a metal cover plate thermal protection system and a nonmetal composite cover plate thermal protection system. The high-temperature area of the metal thermal protection system adopts high-temperature alloy (cobalt-based alloy, nickel-based alloy and the like), the low-temperature area is titanium alloy, and the outer wall of the thin-wall box mainly adopts a multi-wall type and honeycomb sandwich structure. The nonmetal composite cover plate thermal protection structure mainly comprises a ceramic matrix composite material as a cover plate material, and a composite material and a mechanical support structure are adopted inside the cover plate thermal protection structure. Currently, the cover plate shell material is SiC f /SiC、C f /SiC、C f a/C material or a composite material improved on the basis of the/C material.
In the above examples, the connection mode of the heat-proof layer and the heat-insulating layer is mechanical connection, and the process is complex. Meanwhile, the insulating layer in the existing thermal protection system generally has the problem of poor impact resistance.
Disclosure of Invention
In order to overcome the defects in the prior art, the inventor of the invention carries out intensive research and provides an integrated heat-insulation-preventing material and a preparation method thereof 2 O 3 The reinforced layer is made of an alumina composite material, and the heat-proof and heat-insulating properties and the mechanical properties of the material are coordinated through the gradient layer design of the heat-insulating layer and the gradient layer design of the whole material; and the heat-proof layer with excellent oxidation resistance and ablation resistance and the heat-insulating layer with good heat-insulating property are effectively combined by adopting heat-proof integration treatment. The invention is different from the traditional design method of separating heat prevention and heat insulation and forming integration by mechanical connection, and the integrated material of heat prevention and heat insulation innovatively uses the design method of integrating heat prevention and heat insulation, overcomes the defect of low surface mechanical strength of a pure heat insulation material, improves the impact resistance of the surface, ensures the safety of a heat protection system, and realizes the design idea of integrating functions, heat prevention and heat insulation, thereby completing the invention.
The technical scheme provided by the invention is as follows:
in a first aspect, the heat-proof and heat-insulating integrated material comprises a heat-insulating layer, a reinforcing layer and a heat-proof layer, wherein the heat-insulating layer comprises a silicon-based nano heat-insulating material positioned on a cold surface layer and a gradient aluminum silicon-based nano heat-insulating material positioned on a hot surface layer, and the two layers of heat-insulating materials are spliced in a cross shape in a block form; the reinforcing layer comprises a first reinforcing layer and a second reinforcing layer, the first reinforcing layer is an alumina composite material formed by coating six surfaces of 1-3 layers of silicon-based nano heat insulation material blocks and aluminum-silicon-based nano heat insulation material blocks, and the second reinforcing layer is an alumina composite material formed by coating 3-20 layers of alumina composite materials and is bonded with the hot surface layer of the heat insulation layer; the heat-proof layer is 1-3 layers of alumina composite material integrally coated with the heat-insulating layer and the enhancement layer.
In a second aspect, a preparation method of an integrated heat-proof and heat-insulation material comprises the following steps:
stirring and dispersing the nano silicon dioxide powder, the inorganic fiber and the opacifier in a high-speed mixer according to the proportion, and fully dispersing and mixing to obtain composite powder A; calculating the mass of the required composite powder A according to the density requirement of the heat-insulating material; placing the composite powder A with the required mass into a forming die, placing the forming die into a pressure forming machine, applying pressure of 0.5-10 MPa, maintaining the pressure for 1-24 hours, and demolding to obtain the silicon-based nano heat insulation material;
stirring and dispersing the nano alumina, the inorganic fiber and the opacifier in a high-speed mixer according to a certain proportion, and fully dispersing and mixing to obtain composite powder B; calculating the mass of the required composite powder A and B according to the thickness and density of the designed composite powder B and the designed composite powder A; putting the composite powder A with the required mass into a forming die, putting the forming die into a pressure forming machine, applying pressure of 0.25-2 MPa, maintaining the pressure for 0.5-4 h, adding the composite powder B with the required mass, applying pressure of 0.5-10 MPa, maintaining the pressure for 1-24 h, and demoulding to obtain the gradient aluminum-silicon-based nano heat-insulating material;
respectively carrying out blocking treatment on the obtained silicon-based nano heat insulation material and the gradient aluminum-silicon-based nano heat insulation material; brushing the adhesive on alumina fiber cloth, and coating six surfaces of the partitioned silicon-based nano heat-insulating material and the gradient aluminum-silicon-based nano heat-insulating material with the number of coating layers being 1-3 to form a first enhancement layer;
brushing adhesive between two adjacent layers of 3-20 layers of alumina fiber cloth, and applying no less than 50kg/m on the surface 2 The cover plate is placed in an oven at the temperature of 80-110 ℃ and dried for 3-24 hours to form a second enhancement layer;
placing the partitioned gradient aluminum-silicon-based nano heat-insulating material on a hot surface layer, placing the silicon-based nano heat-insulating material on a cold surface layer, and enabling the silicon-based nano heat-insulating material to be close to the silicon-containing surface of the gradient aluminum-silicon-based nano heat-insulating material, so that the two layers form cross splicing; brushing an adhesive on the hot surface layer, adding a second enhancement layer obtained in the fourth step, and finally, integrally coating the hot surface layer with the aluminum oxide fiber cloth coated with the adhesive, wherein the number of coating layers is 1-3; and putting the coated material into a die for integral pressure forming, applying pressure of 0.5-10 MPa, and maintaining the pressure for 1-24 h to obtain the heat-insulation integrated material.
According to the heat-proof integrated material and the preparation method thereof provided by the invention, the following beneficial effects are achieved:
(1) in the invention, the hot surface of the heat insulation layer is designed by adopting an integrated gradient aluminum-silicon-based nano heat insulation material, and the application of alumina can ensure that the use temperature of the material reaches over 1200 ℃; through aluminum-silicon integrated molding, interlayer slippage of the aluminum oxide and silicon oxide nanometer heat insulation materials can be reduced, and later-stage blocking reinforcement is facilitated; the cold surface is designed by adopting a silicon dioxide nanometer heat insulation material, so that the material has a good heat insulation effect. By adopting a method of two-layer block reinforcement and cross superposition, the stress release path can be increased, and the overall strength of the material is improved.
(2) In the invention, the reinforced layer and the heat-proof layer are made of relatively compact alumina composite materials, and the structure of the composite materials is designed to be integrally reinforced after a plurality of layers of alumina fiber cloth are superposed and nano powder is compounded to form a relatively compact structure, so that the material can have higher impact resistance. The aluminum oxide fiber cloth woven fibers are almost completely distributed along the horizontal direction, so that the low heat conductivity in the vertical direction is ensured. In addition, in the integrated pressure forming process, the nano alumina powder flows along with the adhesive slurry under pressure, and can fill the defects of large pores, fiber defects and the like in a fabric structure, so that the surface strength of the material can be further improved.
(3) According to the invention, the integrated molding method of heat prevention and insulation can realize integrated molding of the whole inorganic material without mechanical connection, thereby reducing the risk of heat bridge at high temperature. The yttrium sol, the zirconium sol or the aluminum sol composite nano alumina powder is used as the adhesive to coat, reinforce and integrally form the material, the material components are stable at high temperature, and the use temperature and the heat insulation performance of the reinforcing layer are not influenced. After the integrated pressure forming, the material can keep higher integrity, the internal structure is not damaged, the good heat insulation effect of the nano heat insulation material is kept, and in addition, the safety and reliability in the using process, assembly and transportation are also improved.
Drawings
FIG. 1 is a gradient Al-Si based nano thermal insulation material;
FIG. 2 is a cross-shaped split joint formed by two layers of nano heat insulation layers after being enhanced in blocks;
FIG. 3 is a side view of an integrated thermal barrier material;
fig. 4 is a front image of the integrated heat-proof and heat-insulation integrated material.
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
According to the first aspect of the invention, an integrated heat insulation and protection material is provided, which comprises a heat insulation layer, a reinforcing layer and a heat protection layer, wherein the heat insulation layer comprises a silicon-based nano heat insulation material positioned on a cold surface layer and a gradient aluminum silicon-based nano heat insulation material positioned on a hot surface layer, and the two heat insulation materials are spliced in a cross shape in a block form; the reinforcing layer comprises a first reinforcing layer and a second reinforcing layer, the first reinforcing layer is 1-3 layers of aluminum oxide fiber cloth with six surfaces coated with silicon-based nano heat insulation material blocks and aluminum-silicon-based nano heat insulation material blocks, an adhesive is coated between two adjacent layers of aluminum oxide fiber cloth, the second reinforcing layer is 3-20 layers of aluminum oxide fiber cloth, an adhesive is coated between two adjacent layers of aluminum oxide fiber cloth, and the second reinforcing layer is bonded with the hot surface layer of the heat insulation layer through the adhesive; the heat-proof layer is 1-3 layers of alumina fiber cloth integrally coated with the heat-insulating layer and the reinforcing layer, and an adhesive is coated between every two adjacent layers of alumina fiber cloth.
In a preferred embodiment, the silicon-based nano heat-insulating material is obtained by compression molding of a composite powder A, wherein the composite powder A comprises nano silica powder, inorganic fibers and an opacifier, and the mass ratio of the nano silica powder to the inorganic fibers to the opacifier is (14-20): (1-5): 1. preferably, the nano silicon dioxide is one or more of flame silica fume, white carbon black or fumed silica; the inorganic fiber is chopped fiber and is one or more of glass fiber, quartz fiber, alumina silicate fiber, basalt fiber or mullite fiber; the opacifier is one or more of titanium dioxide, zirconia, silicon carbide and ferric oxide.
Further, the silicon-based nano heat-insulating material is molded by the following steps: and (3) putting the composite powder A with the required mass into a forming die, putting the die into a pressure forming machine, applying pressure of 0.5-10 MPa, maintaining the pressure for 1-24 hours, and demoulding to obtain the silicon-based nano heat-insulating material.
In a preferred embodiment, the gradient aluminum-silicon-based nano heat-insulating material is obtained by compression molding of a composite powder A and a composite powder B, wherein the composite powder A is identical to the composite powder A used in the silicon-based nano heat-insulating material, the composite powder B comprises nano alumina, inorganic fibers and an opacifier, and the mass ratio of the nano alumina to the inorganic fibers to the opacifier is (15-20): (1-5): 1. preferably, the inorganic fiber is chopped fiber and is one or more of quartz fiber, alumina silicate fiber or mullite fiber; the opacifier is one or more of titanium dioxide, zirconia and silicon carbide.
Further, the step of compression molding of the gradient aluminum-silicon-based nano heat-insulating material is as follows: and (2) placing the composite powder A with the required mass into a forming die, placing the forming die into a pressure forming machine, applying pressure of 0.25-2 MPa, maintaining the pressure for 0.5-4 h, adding the composite powder B with the required mass, applying pressure of 0.5-10 MPa, maintaining the pressure for 1-24 h, and demolding to obtain the gradient aluminum-silicon-based nano heat insulation material.
In a preferred embodiment, the silicon-based nano heat insulation material in the heat insulation layer is close to the silicon-containing surface of the gradient aluminum-silicon-based nano heat insulation material.
In the invention, the hot surface of the heat insulation layer is designed by adopting an integrated gradient aluminum-silicon-based nano heat insulation material, and the application of alumina can ensure that the use temperature of the material reaches over 1200 ℃; through aluminum-silicon integrated molding, the interlayer slippage of the aluminum oxide and silicon oxide nanometer heat-insulating materials can be reduced, and the later-stage blocking reinforcement can be realized; the cold surface is designed by adopting a silicon dioxide nanometer heat insulation material, so that the material has a good heat insulation effect. By adopting a method of two-layer block reinforcement and cross superposition, the stress release path can be increased, and the overall strength of the material is improved.
In a preferred embodiment, the binder is one or more of yttrium sol, aluminum sol and zirconium sol mixed with alumina nano powder. The selected adhesive sol can generate certain adhesive strength at 80-110 ℃, and the reinforcing layer is adhered to form a whole. Can generate stable ceramic powder at high temperature and has low heat conductivity. The sols can be used singly or in combination, because they do not react with one another when used in combination, and are highly stable. The content of the powder is controlled to be 2-15 wt% of the total mass of the adhesive, and if the content of the powder is too high, the flowability of the powder and the adhesive property of the sol are influenced.
In a preferred embodiment, the second reinforcing layer is prepared by: brushing adhesive between two adjacent layers of 3-20 layers of alumina fiber cloth, and applying no less than 50kg/m on the surface 2 The cover plate is placed in an oven at 80-110 ℃ and dried for 3-24 h.
In the invention, the first reinforcing layer mainly has the function of ensuring that the bearing unit keeps stable structure, does not crack and is not loose in the material compression process. The first reinforcing layer can improve the material strength of each structural unit (block material unit), and can also improve the overall strength of the material in a reinforcing rib form after the cross-shaped splicing. If the reinforcing layer is too thick, a thermal bridge effect can be caused, and the heat insulation of the material is not good, so that 1-3 layers are selected as the first reinforcing layer; the second enhancement layer not only assists in increasing mechanical strength, but also assists in heat protection, improves the impact resistance of the material, reduces the heat insulation effect of the material due to too many layers, greatly increases the density of the material, and is not beneficial to popularization and application, so that the optimal thickness of the second enhancement layer is 3-20 layers. The heat-proof layer has the main function of realizing the integral molding of the material, so that the material can keep higher integrity, and the internal structure is not damaged; the density and the heat insulation requirements of the whole material are combined, the heat-proof layer is not easy to be designed to be too thick, and 1-3 layers are preferred.
In the invention, the enhancement layer and the heat-proof layer are made of relatively compact alumina composite materials, and the structure of the composite materials is designed to be that a plurality of layers of alumina fiber cloth are superposed and compounded with nano powder to form a relatively compact structure, thereby providing higher impact resistance of the materials. The aluminum oxide fiber cloth woven fibers are almost completely distributed along the horizontal direction, so that the low heat conductivity in the vertical direction is ensured. In addition, in the integrated pressure forming process, the nano alumina powder flows along with the adhesive slurry under pressure, and can fill the defects of large pores, fiber defects and the like in a fabric structure, so that the surface strength of the material can be further improved.
In the invention, the heat-proof and heat-insulating integrated material comprises 12-40 wt% of alumina fiber cloth, 40-60 wt% of nano silicon dioxide, 10-30 wt% of nano alumina, 5-20 wt% of inorganic fiber and 1-15 wt% of an opacifier, wherein the mass of an adhesive is 60-190 wt% of the total mass of the components; the overall density of the material is less than or equal to 0.60g/cm 3 The heat conductivity at room temperature is less than or equal to 0.039W/(m.K), the bending strength is more than or equal to 3.00MPa, and the back surface temperature is less than or equal to 130 ℃ after the material is heated at 1200 ℃ for 30 min.
According to a second aspect of the invention, a preparation method of an integrated heat-proof and heat-insulation material is provided, which comprises the following steps:
step 1, preparing a silicon-based nano heat-insulating material:
stirring and dispersing the nano silicon dioxide powder, the inorganic fiber and the opacifier in a high-speed mixer according to the proportion, and fully dispersing and mixing to obtain composite powder A; calculating the mass of the required composite powder A according to the density requirement of the heat-insulating material; placing the composite powder A with the required mass into a forming die, placing the forming die into a pressure forming machine, applying pressure of 0.5-10 MPa, maintaining the pressure for 1-24 hours, and demolding to obtain the silicon-based nano heat insulation material;
stirring and dispersing the nano-alumina, the inorganic fiber and the opacifier in a high-speed mixer according to a certain proportion, and fully dispersing and mixing to obtain composite powder B; calculating the mass of the required composite powder A and B according to the thickness and density of the designed composite powder B and the designed composite powder A; putting the composite powder A with the required mass into a forming die, placing the die into a pressure forming machine, applying pressure of 0.25-2 MPa, maintaining the pressure for 0.5-4 h, adding the composite powder B with the required mass, applying pressure of 0.5-10 MPa, maintaining the pressure for 1-24 h, and demoulding to obtain the gradient aluminum-silicon-based nano heat-insulating material;
step 3, partitioning and surface enhancing treatment of the nano heat insulation material;
respectively carrying out blocking treatment on the silicon-based nano heat insulation material obtained in the step 1 and the step 2 and the gradient aluminum-silicon-based nano heat insulation material; brushing the adhesive on alumina fiber cloth, and coating six surfaces of the partitioned silicon-based nano heat-insulating material and the gradient aluminum-silicon-based nano heat-insulating material with the number of coating layers being 1-3 to form a first enhancement layer;
step 4, preparing a second enhancement layer;
brushing adhesive between two adjacent layers of 3-20 layers of alumina fiber cloth, and applying no less than 50kg/m on the surface 2 The cover plate is placed in an oven at the temperature of 80-110 ℃ and dried for 3-24 hours to form a second enhancement layer;
step 5, integrating and molding the materials to obtain an anti-heat-insulation integrated material;
placing the partitioned gradient aluminum-silicon-based nano heat-insulating material on a hot surface layer, placing the silicon-based nano heat-insulating material on a cold surface layer, and enabling the silicon-based nano heat-insulating material to be close to the silicon-containing surface of the gradient aluminum-silicon-based nano heat-insulating material, so that the two layers form cross splicing; brushing an adhesive on the hot surface layer, adding a second enhancement layer obtained in the fourth step, and finally, integrally coating the hot surface layer with the aluminum oxide fiber cloth coated with the adhesive, wherein the number of coating layers is 1-3; and putting the coated material into a die for integral pressure forming, applying pressure of 0.5-10 MPa, and maintaining the pressure for 1-24 h to obtain the heat-insulation integrated material.
In a preferred embodiment, in the step 1, the nano-silica powder, the inorganic fiber and the light-shading agent are stirred and dispersed in a high-speed mixer for 2-10 minutes at a rotating speed of 500-1200 r/min, the high-speed stirring aims to uniformly disperse the fiber and the light-shading agent and break up nano-particle aggregates in the powder, the stirring time and the rotating speed are related to the mass of the put raw materials, and the higher the mass is, the longer the high-speed stirring time is, the higher the speed is;
in the step 2, the nano aluminum oxide, the inorganic fibers and the opacifier are stirred and dispersed in a high-speed mixer for 2-10 minutes at the rotating speed of 800-1800 rpm.
In a preferred embodiment, after the blocking treatment in step 3, the width of the single silicon-based nano heat insulation material and the gradient aluminum silicon-based nano heat insulation material is 10-50 mm. The overall external dimension of the thermal insulation material applied in engineering is designed to be integral multiples of the strip dimension by combining the universal dimension (100-400 mm) x (10-40 mm) of the thermal insulation material applied in engineering, and the width of a single block is preferably 10-50 mm by combining the processing difficulty of the nanometer thermal insulation material.
According to the heat-insulation integrated forming method, the integrated forming of the whole inorganic material can be realized, the mechanical connection is not adopted, and the risk of a heat bridge at high temperature is reduced. The yttrium sol, the zirconium sol or the aluminum sol composite nano alumina powder is used as the adhesive to coat, reinforce and integrally form the material, the material components are stable at high temperature, and the use temperature and the heat insulation performance of the reinforcing layer are not influenced. After the integrated pressure forming, the material can keep higher integrity, the internal structure is not damaged, the good heat insulation effect of the nano heat insulation material is kept, and in addition, the safety and reliability in the using process, assembly and transportation are also improved.
Examples
Example 1
Weighing 3060g of nano silicon dioxide powder, 360g of quartz fiber and 180g of zirconia powder (17:2:1), stirring for 8 minutes in a high-speed mixer at the rotating speed of 1200 rpm, and fully dispersing and mixing to obtain composite powder A; weighing 360g of composite powder A, placing the composite powder A into a 200 x 200mm forming die, placing the composite powder A into a pressure forming machine, raising the column by 20mm, applying 2MPa pressure, maintaining the pressure for 3 hours, and demolding to obtain the silicon-based nano heat insulation material;
weighing 1380g of nano alumina, 160g of mullite fiber and 80g (17.25:2:1) of zirconia powder, stirring for 7 minutes in a high-speed mixer at the rotating speed of 1200 revolutions per minute, and fully dispersing and mixing to obtain composite powder B; respectively weighing 180g of composite powder A and 162g of composite powder B, putting the composite powder A into a 200 x 200mm forming die, putting the die into a pressure forming machine, raising the column by 10mm, applying 1MPa pressure, keeping the pressure for 0.5h, then adding the composite powder B, raising the column by 19mm, applying 10MPa pressure, keeping the pressure for 5h, and demoulding to obtain the gradient aluminum-silicon-based nano heat-insulating material, wherein the formula is shown in figure 1;
the silicon-based nano heat-insulating material and the gradient aluminum-silicon-based nano heat-insulating material are evenly divided into 10 blocks. 50g of nano alumina powder and 730g of alumina sol are mixed according to the proportion and mechanically stirred to prepare the adhesive. Coating the adhesive on the alumina fiber cloth in a brush way, and respectively coating six surfaces of the two partitioned nanometer heat-insulating materials, wherein the number of the coating layers is 2;
brushing 6 layers of alumina fiber cloth with an adhesive, applying 1 block of cover plate of 5kg on the surface, and drying in an oven at 95 ℃ for 6h to form a compact reinforcing layer;
splicing the partitioned heat insulation materials to form an upper layer and a lower layer, keeping the gradient aluminum-silicon-based nano heat insulation material placed on the hot surface layer, and keeping the silicon-based nano heat insulation material placed on the cold surface layer, wherein the two layers form a cross splice, as shown in figure 2; and brushing an adhesive on the hot surface layer, adding a compact reinforcing layer, and finally, integrally coating the hot surface layer with an alumina fiber cloth coated with the adhesive, wherein the number of coating layers is 2. And putting the coated material into a 200 x 200mm mould for integral pressure molding, applying 10MPa of pressure, and maintaining the pressure for 10h to obtain the heat-insulation integrated material, as shown in figures 3 and 4.
The integral density of the integrated material for preventing and insulating heat is 0.58g/cm 3 The thermal conductivity at room temperature is 0.037W/(m.K), the bending strength is 3.23MPa, and the temperature of the back surface is 103 ℃ after heating at 1200 ℃ for 30 min.
Example 2
Weighing 2880g of nano silicon dioxide powder, 540g of quartz fiber and 180g (16:3:1) of zirconia powder, stirring for 7 minutes in a high-speed mixer at the rotating speed of 1100 r/min, and fully dispersing and mixing to obtain composite powder A; weighing 360g of composite powder A, placing the composite powder A into a 200 x 200mm forming die, placing the composite powder A into a pressure forming machine, raising the column by 20mm, applying 2MPa pressure, maintaining the pressure for 3 hours, and demolding to obtain the silicon-based nano heat insulation material;
weighing 1300g of nano alumina, 240g of mullite fiber and 80g (16.25:3:1) of zirconia powder, stirring for 7 minutes in a high-speed mixer at the rotating speed of 1200 rpm, and fully dispersing and mixing to obtain composite powder B; respectively weighing 180g of composite powder A and 162g of composite powder B, putting the composite powder A into a 200 x 200mm forming die, putting the die into a pressure forming machine, raising the column by 10mm, applying 1MPa pressure, keeping the pressure for 0.5h, then adding the composite powder B, raising the column by 19mm, applying 10MPa pressure, keeping the pressure for 5h, and demoulding to obtain the gradient aluminum-silicon-based nano heat-insulating material;
respectively carrying out average 10-block treatment on the silicon-based nano heat-insulating material and the gradient aluminum-silicon-based nano heat-insulating material; 50g of nano alumina powder and 750g of zirconium sol are mixed according to a proportion and mechanically stirred to prepare the adhesive. Coating the adhesive on the alumina fiber cloth in a brush way, and respectively coating six surfaces of the two partitioned nanometer heat-insulating materials, wherein the number of the coating layers is 2;
brushing an adhesive on 8 layers of aluminum oxide fiber cloth, applying 1 cover plate of 5kg on the surface, and drying in an oven at 95 ℃ for 6h to form a compact reinforcing layer;
splicing the partitioned heat insulation materials to form an upper layer and a lower layer, keeping the gradient aluminum-silicon-based nano heat insulation material placed on the hot surface layer, and keeping the silicon-based nano heat insulation material placed on the cold surface layer, wherein the two layers form a cross splice; and brushing an adhesive on the hot surface layer, adding a compact reinforcing layer, and finally, integrally coating the hot surface layer with the adhesive-brushed alumina fiber cloth, wherein the number of coating layers is 2. And putting the coated material into a 200 x 200mm mould for integral pressure forming, applying 10MPa of pressure, and maintaining the pressure for 10h to obtain the heat-insulation integrated material.
Integral density of the integrated material for preventing and insulating heat is 0.6g/cm 3 The thermal conductivity at room temperature is 0.039W/(m.K), the bending strength is 3.45MPa, and after heating at 1200 ℃ for 30min, the back surface temperature is 127 ℃.
Example 3
2720g of nano silicon dioxide powder, 320g of quartz fiber and 160g (17:2:1) of titanium dioxide powder are weighed, stirred in a high-speed mixer for 7 minutes at the rotating speed of 1100 r/min, and fully dispersed and mixed to obtain composite powder A; weighing 320g of composite powder A, putting the composite powder A into a 200 x 200mm forming die, putting the composite powder A into a pressure forming machine, raising the column by 20mm, applying 2MPa pressure, maintaining the pressure for 3 hours, and demoulding to obtain the silicon-based nano heat-insulating material;
weighing 1380g of nano alumina, 160g of alumina fiber and 80g (17.25:2:1) of titanium dioxide powder, stirring for 7 minutes in a high-speed mixer at the rotating speed of 1200 revolutions per minute, and fully dispersing and mixing to obtain composite powder B; respectively weighing 160g of composite powder A and 162g of composite powder B, placing the composite powder A into a 200 x 200mm forming die, placing the die into a pressure forming machine, raising the height of a column by 10mm, applying 1MPa pressure, maintaining the pressure for 0.5h, then adding the composite powder B, raising the height of the column by 19mm, applying 10MPa pressure, maintaining the pressure for 5h, and demoulding to obtain the gradient aluminum-silicon-based nano heat-insulating material;
respectively carrying out average 8-block treatment on the silicon-based nano heat-insulating material and the gradient aluminum-silicon-based nano heat-insulating material; 35g of nano alumina powder and 690g of alumina sol are mixed according to a proportion and mechanically stirred to prepare the adhesive. Coating the adhesive on the alumina fiber cloth in a brush way, and respectively coating six surfaces of the two partitioned nanometer heat-insulating materials, wherein the number of the coating layers is 2;
brushing 7 layers of aluminum oxide fiber cloth with an adhesive, applying 1 block of cover plate of 5kg on the surface, and drying in an oven at 95 ℃ for 6h to form a compact reinforcing layer;
splicing the partitioned heat insulation materials to form an upper layer and a lower layer, keeping the gradient aluminum-silicon-based nano heat insulation material placed on the hot surface layer, and keeping the silicon-based nano heat insulation material placed on the cold surface layer, wherein the two layers form a cross splice; and brushing an adhesive on the hot surface layer, adding a compact reinforcing layer, and finally, integrally coating the hot surface layer with the adhesive-brushed alumina fiber cloth, wherein the number of coating layers is 2. And putting the coated material into a 200 x 200mm mould for integral pressure forming, applying 10MPa of pressure, and maintaining the pressure for 10h to obtain the heat-insulation integrated material.
The integral density of the integrated material for preventing and insulating heat is 0.55g/cm 3 The thermal conductivity at room temperature is 0.034W/(m.K), the bending strength is 3.02MPa, and after heating at 1200 ℃ for 30min, the back surface temperature is 88 ℃.
Example 4
Weighing 2560g of nano silicon dioxide powder, 480g of quartz fiber and 160g of silicon carbide powder (16:3:1), stirring for 7 minutes in a high-speed mixer at the rotating speed of 1000 revolutions per minute, and fully dispersing and mixing to obtain composite powder A; weighing 320g of composite powder A, putting the composite powder A into a 200 x 200mm forming die, putting the composite powder A into a pressure forming machine, raising the column by 20mm, applying 2MPa pressure, maintaining the pressure for 3 hours, and demoulding to obtain the silicon-based nano heat-insulating material;
weighing 1300g of nano alumina, 240g of alumina fiber and 80g (16.25:3:1) of titanium dioxide, stirring for 7 minutes in a high-speed mixer at the rotating speed of 1200 rpm, and fully dispersing and mixing to obtain composite powder B; respectively weighing 160g of composite powder A and 162g of composite powder B, putting the composite powder A into a 200 x 200mm forming die, putting the die into a pressure forming machine, raising the column by 10mm, applying 1MPa pressure, keeping the pressure for 0.5h, then adding the composite powder B, raising the column by 19mm, applying 10MPa pressure, keeping the pressure for 5h, and demoulding to obtain the gradient aluminum-silicon-based nano heat-insulating material;
respectively carrying out average 8-block treatment on the silicon-based nano heat-insulating material and the gradient aluminum-silicon-based nano heat-insulating material; 32g of nano alumina powder and 693g of yttrium sol are mixed according to a proportion and mechanically stirred to prepare the adhesive. Brushing the adhesive on the alumina fiber cloth, and respectively coating six surfaces of the partitioned nanometer heat-insulating material with 2 coating layers;
brushing 7 layers of aluminum oxide fiber cloth with an adhesive, applying 1 block of cover plate of 5kg on the surface, and drying in an oven at 95 ℃ for 6h to form a compact reinforcing layer;
splicing the partitioned heat insulation materials to form an upper layer and a lower layer, keeping the gradient aluminum-silicon-based nano heat insulation material placed on the hot surface layer, and keeping the silicon-based nano heat insulation material placed on the cold surface layer to form a cross splice; and brushing an adhesive on the hot surface layer, adding a compact reinforcing layer, and finally, integrally coating the hot surface layer with the adhesive-brushed alumina fiber cloth, wherein the number of coating layers is 2. And putting the coated material into a 200 x 200mm mould for integral pressure forming, applying 10MPa of pressure, and maintaining the pressure for 10h to obtain the heat-insulation integrated material.
The integral density of the integrated material for preventing and insulating heat is 0.55g/cm 3 The thermal conductivity at room temperature is 0.035W/(m.K), the bending strength is 3.11MPa, the temperature of the back surface is 95 ℃ after heating for 30min at 1200 ℃.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.
Claims (8)
1. The heat-proof and heat-insulating integrated material is characterized by comprising a heat-insulating layer, a reinforcing layer and a heat-proof layer, wherein the heat-insulating layer comprises a silicon-based nano heat-insulating material positioned on a cold surface layer and a gradient aluminum-silicon-based nano heat-insulating material positioned on a hot surface layer, the two layers of heat-insulating materials are spliced in a cross shape in a block form, and the silicon-based nano heat-insulating material in the heat-insulating layer is close to a silicon-containing surface of the gradient aluminum-silicon-based nano heat-insulating material; the silicon-based nano heat-insulating material is obtained by compression molding of a composite powder A, wherein the composite powder A comprises nano silicon dioxide powder, inorganic fibers and an opacifier, and the mass ratio of the nano silicon dioxide powder to the inorganic fibers to the opacifier is (14-20): (1-5): 1; the gradient aluminum-silicon-based nano heat-insulating material is obtained by compression molding of a composite powder A and a composite powder B, the composite powder A is consistent with the composite powder A used in the silicon-based nano heat-insulating material, the composite powder B comprises nano alumina, inorganic fibers and an opacifier, and the mass ratio of the nano alumina to the inorganic fibers to the opacifier is (15-20): (1-5): 1; the step of compression molding of the gradient aluminum-silicon-based nano heat-insulating material is as follows: putting the composite powder A with the required mass into a forming die, putting the forming die into a pressure forming machine, applying pressure of 0.25-2 MPa, maintaining the pressure for 0.5-4 h, adding the composite powder B with the required mass, applying pressure of 0.5-10 MPa, maintaining the pressure for 1-24 h, and demoulding to obtain the gradient aluminum-silicon-based nano heat-insulating material;
the heat insulation layer comprises a heat insulation layer and a reinforcing layer, wherein the reinforcing layer comprises a first reinforcing layer and a second reinforcing layer, the first reinforcing layer is an alumina composite material formed by coating six surfaces of 1-3 silicon-based nano heat insulation material blocks and aluminum-silicon-based nano heat insulation material blocks, and the second reinforcing layer is an alumina composite material formed by coating 3-20 layers of alumina composite material and is bonded with a hot surface layer of the heat insulation layer; the heat-proof layer is 1-3 layers of alumina composite material integrally coated with the heat-insulating layer and the enhancement layer.
2. The integrated material of claim 1, wherein in the composite powder A, the nano-silica is one or more of flame silica fume, white carbon black or fumed silica; the inorganic fiber is chopped fiber and is one or more of glass fiber, quartz fiber, alumina silicate fiber, basalt fiber or mullite fiber; the opacifier is one or more of titanium dioxide, zirconia, silicon carbide and ferric oxide.
3. The integrated material of claim 2, wherein the silicon-based nano heat-insulating material is molded by the following steps: and (3) putting the composite powder A with the required mass into a forming die, putting the die into a pressure forming machine, applying pressure of 0.5-10 MPa, maintaining the pressure for 1-24 hours, and demoulding to obtain the silicon-based nano heat-insulating material.
4. The integrated material of claim 1, wherein in the composite powder B, the inorganic fiber is chopped fiber, and is one or more of quartz fiber, alumina silicate fiber or mullite fiber; the opacifier is one or more of titanium dioxide, zirconia and silicon carbide.
5. The integrated heat and heat prevention and insulation integrated material as claimed in claim 1, wherein the main component of the alumina composite material in the first reinforcing layer, the second reinforcing layer and the heat protection layer is alumina fiber cloth, and an adhesive is coated between two adjacent layers of alumina fiber cloth.
6. The integrated material of claim 5, wherein the second reinforcement layer is prepared by the following method: brushing an adhesive between two adjacent layers of 3-20 layers of aluminum oxide fiber cloth, applying a cover plate with the surface not less than 50kg/m < 2 >, and drying in an oven at the temperature of 80-110 ℃ for 3-24 h.
7. The integrated heat-insulation and heat-prevention integrated material as claimed in claim 1, wherein the integrated heat-insulation and heat-prevention material comprises 12-40 wt% of alumina fiber cloth, 40-60 wt% of nano silica, 10-30 wt% of nano alumina, 5-20 wt% of inorganic fiber, 1-15 wt% of light-screening agent, and 60-190 wt% of adhesive; the integrated material has an integral density of less than or equal to 0.60g/cm < 3 >, a room-temperature thermal conductivity of less than or equal to 0.039W/(m.K), a bending strength of greater than or equal to 3.00MPa, and a back temperature of less than or equal to 130 ℃ after heating at 1200 ℃ for 30 min.
8. A preparation method of the heat-proof and insulation integrated material as claimed in one of claims 1 to 7, characterized by comprising the following steps:
stirring and dispersing the nano silicon dioxide powder, the inorganic fiber and the opacifier in a high-speed mixer according to the proportion, and fully dispersing and mixing to obtain composite powder A; calculating the mass of the required composite powder A according to the density requirement of the heat-insulating material; placing the composite powder A with the required mass into a forming die, placing the forming die into a pressure forming machine, applying pressure of 0.5-10 MPa, maintaining the pressure for 1-24 hours, and demolding to obtain the silicon-based nano heat insulation material;
stirring and dispersing the nano alumina, the inorganic fiber and the opacifier in a high-speed mixer according to a certain proportion, and fully dispersing and mixing to obtain composite powder B; calculating the mass of the required composite powder A and B according to the thickness and density of the designed composite powder B and the designed composite powder A; putting the composite powder A with the required mass into a forming die, putting the forming die into a pressure forming machine, applying pressure of 0.25-2 MPa, maintaining the pressure for 0.5-4 h, adding the composite powder B with the required mass, applying pressure of 0.5-10 MPa, maintaining the pressure for 1-24 h, and demoulding to obtain the gradient aluminum-silicon-based nano heat-insulating material;
respectively carrying out blocking treatment on the obtained silicon-based nano heat insulation material and the gradient aluminum-silicon-based nano heat insulation material; brushing the adhesive on alumina fiber cloth, and coating six surfaces of the partitioned silicon-based nano heat-insulating material and the gradient aluminum-silicon-based nano heat-insulating material with the number of coating layers being 1-3 to form a first enhancement layer;
brushing an adhesive between two adjacent layers of 3-20 layers of aluminum oxide fiber cloth, applying a cover plate with the surface not less than 50kg/m & lt 2 & gt, and drying in an oven at 80-110 ℃ for 3-24 hours to form a second enhancement layer;
placing the partitioned gradient aluminum-silicon-based nano heat-insulating material on a hot surface layer, placing the silicon-based nano heat-insulating material on a cold surface layer, and enabling the silicon-based nano heat-insulating material to be close to the silicon-containing surface of the gradient aluminum-silicon-based nano heat-insulating material, so that the two layers form cross splicing; brushing an adhesive on the hot surface layer, adding a second enhancement layer obtained in the fourth step, and finally, integrally coating the hot surface layer with the aluminum oxide fiber cloth coated with the adhesive, wherein the number of coating layers is 1-3; and putting the coated material into a die for integral pressure forming, applying pressure of 0.5-10 MPa, and maintaining the pressure for 1-24 h to obtain the heat-insulation integrated material.
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