CN117945711A - Low-cost non-ablative sandwich heat-resistant structural material and preparation method thereof - Google Patents

Low-cost non-ablative sandwich heat-resistant structural material and preparation method thereof Download PDF

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CN117945711A
CN117945711A CN202410352905.9A CN202410352905A CN117945711A CN 117945711 A CN117945711 A CN 117945711A CN 202410352905 A CN202410352905 A CN 202410352905A CN 117945711 A CN117945711 A CN 117945711A
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heat
sandwich
powder
insulating
ablative
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姜勇刚
冯坚
冯军宗
李良军
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National University of Defense Technology
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National University of Defense Technology
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Abstract

The invention relates to the technical field of heat-proof structural materials, and provides a low-cost non-ablative sandwich heat-proof structural material and a preparation method thereof, wherein the low-cost non-ablative sandwich heat-proof structural material comprises a sandwich structure framework formed by spacer fabrics and a heat-insulating medium filled in a middle core layer of the sandwich structure framework; the weight percentage is as follows: 25% -60% of sandwich structure skeleton, and 40% -75% of heat insulation medium; the sandwich structure skeleton is obtained by shaping the spacer fabric after sol impregnation; the heat insulating medium comprises heat insulating powder, fiber powder, cement powder and surfactant, and the preparation method comprises 4 steps of preparing a framework of a sandwich structure, preparing heat insulating slurry, preparing a sandwich structure/heat insulating slurry composite body and drying at normal pressure. The material has the advantages of low cost, high temperature resistance, non-ablation, low thermal conductivity, high strength and the like. The preparation method has the advantages of mild preparation process conditions, safe preparation process, environment friendliness, short preparation period and easiness in realization of large-scale production.

Description

Low-cost non-ablative sandwich heat-resistant structural material and preparation method thereof
Technical Field
The invention relates to the technical field of heat-resistant structural materials, in particular to a low-cost non-ablative sandwich heat-resistant structural material and a preparation method thereof.
Background
When the novel high-speed aircraft flies in the atmosphere, the surface of the aircraft body can face high-speed airflow scouring and aerodynamic heat load, and in order to protect equipment inside the aircraft body from overtemperature and burnout and work normally, a high-efficiency heat-proof structure is required to be arranged on the surface of the aircraft body, and the heat-proof structure has heat-proof and heat-insulating functions.
The prior non-ablative heat-proof structural materials mainly comprise four types of flexible ceramic fiber felts, ceramic fiber heat-insulating tiles, cover plate heat-proof structures and sandwich heat-proof structures. Wherein the sandwich heat-proof structural material is one of the hot spots studied in recent years. The existing non-ablative sandwich heat-proof structure material generally consists of a ceramic matrix composite surface layer (serving as a heat-proof panel) and an aerogel heat-insulating material (serving as a core layer), wherein the panels are positioned on the upper surface and the lower surface of the core layer and are integrally formed by needling, puncturing or sewing.
The non-ablative sandwich heat-proof structural material has heat-proof and heat-insulating functions, and the published patent literature is CN 102642350B, CN 109824372A, CN 110128158A, CN 112094130B and the like. For example, CN 102642350B discloses a high-temperature-resistant heat-insulating sandwich ceramic matrix composite and a preparation method thereof, wherein the upper and lower panels are inorganic fiber reinforced oxide ceramic matrix composite, the middle core layer is aerogel composite, and the prepared sandwich material has the functions of heat prevention, heat insulation, bearing, wave transmission and the like through stitching and panel densification processes. The CN 111703142A adds the infrared reflection film material in the aerogel composite material core layer of the sandwich heat-proof structure, and further improves the heat transfer capacity of inhibiting high-temperature radiation.
However, the aerogel composite core layer in the sandwich heat-proof structure is generally prepared by a supercritical ethanol drying process (the temperature is more than or equal to 243 ℃ and the pressure is more than or equal to 6.7 MPa) under severe conditions and high temperature and high pressure, or by repeated replacement of organic solvents (ethanol, n-hexane and the like) with lengthy procedures and normal-pressure drying of surface modification (trimethylchlorosilane, hexamethyldisilazane and the like); the ceramic heat-proof panels on the upper and lower surfaces can be obtained through repeated sol dipping-high-temperature sintering processes; the preparation process for connecting the panel and the heat insulation core layer still adopts the traditional manual sewing process, which has low efficiency and insufficient stability of sewing quality batch. Therefore, the process conditions for preparing the panel, the core layer and the stitching of the panel and the core layer are harsh and the process flow is long, so that the manufacturing and using cost of the sandwich heat-proof structure is high.
In order to simplify the preparation conditions and the process and reduce the material manufacturing and using cost, CN 113246563B provides a novel non-ablative sandwich heat-proof and heat-insulating integrated material and a preparation method thereof, nano porous ceramic is filled in situ in the variable-density inorganic ceramic fiber reinforced skeleton to serve as a matrix through the sol dipping and high-temperature drying process, and the prepared sandwich heat-proof structure material has the performances of high temperature resistance, non-ablative property, low heat conduction, high strength, low cost and the like. However, the variable-density ceramic fiber reinforced skeleton used by the material still needs needling and manual sewing to obtain, and the preparation process conditions (high-pressure container is needed, the high-temperature drying temperature is 140-350 ℃ and the pressure is 4-20 MPa) are still harsh, so that the manufacturing and use cost of the material is further reduced.
Therefore, the existing non-ablative sandwich heat-resistant structure forming process is still complex, the preparation process conditions are severe, the manufacturing and using costs are still high, and the use requirements of the novel high-speed aircraft on low-cost non-ablative heat-resistant structure materials are difficult to meet.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a low-cost non-ablative sandwich heat-proof structure material and a preparation method thereof, wherein the non-ablative sandwich heat-proof structure uses a sandwich structure skeleton obtained after a spacer fabric dipping sol shaping treatment as a support body of a product, and a gap of a middle core layer of the support body is filled with a heat-insulating medium prepared from raw materials in a preset proportion.
The technical scheme of the invention is that the low-cost non-ablative sandwich heat-proof structure material is provided firstly, and comprises a sandwich structure framework formed by a spacer fabric and a heat-insulating medium filled in a middle core layer of the sandwich structure framework; the total mass of the non-ablative sandwich heat-proof structural material is calculated as 100%, and the mass percentage of each component is as follows: 25% -60% of sandwich structure skeleton, and 40% -75% of heat insulation medium; the sandwich structure framework is obtained by shaping a spacer fabric after sol impregnation; the heat insulation medium comprises heat insulation powder, fiber powder, cement powder and surfactant.
Furthermore, the spacer fabric is integrally woven by ceramic fiber tows with the linear density of 75-390 tex; the ceramic fiber bundle filaments are one or more of high silica fibers, quartz fibers, aluminum silicate fibers and aluminum oxide fibers; the spacer fabric comprises an upper layer, a lower layer and a spacer space layer, wherein fiber core posts in the spacer space layer connect the upper layer and the lower layer: the thickness of the upper layer and the lower layer is 1-2 mm, and the thickness of the interval space layer is 10-40 mm; the fiber core column in the interval space layer forms an angle of 45 degrees plus or minus 5 degrees with the upper layer and the lower layer.
Furthermore, the sol for impregnating the spacer fabric is silica sol and/or alumina sol which takes water as a solvent, wherein the particle size of the sol is 10-20 nm, and the solid content of the sol is 35-50 wt%; the shaping treatment after sol impregnation comprises the following steps: and taking out the spacer fabric from the sol pool after sol impregnation, and airing at room temperature and carrying out high-temperature heat treatment to obtain the shaped sandwich structure framework, wherein the high-temperature heat treatment temperature is 600-1200 ℃, and the high-temperature treatment time is 0.5-2 h.
Further, the fiber powder is formed by crushing heat-insulating ceramic fibers with the diameter of 2-3 mu m, and the heat-insulating ceramic fibers are any one or more of titanium oxide, zirconium oxide and silicon carbide fibers; the length of the fiber powder is 50-100 μm.
Further, the heat insulation powder is aerogel powder formed by crushing hydrophobic aerogel blocks, wherein the hydrophobic aerogel blocks are hydrophobic silica aerogel and/or alumina aerogel blocks; the particle size of the heat insulation powder is 20-50 mu m.
Further, the cement powder is silicate cement and/or aluminate cement; the surfactant is one or two of sodium dodecyl benzene sulfonate, alkyl glucoside, fatty glyceride, sucrose ester and fatty alcohol ester.
Further, in the above heat insulating medium: the heat-insulating powder comprises (by weight) 5-20 parts of a surfactant, (40-70 parts of) 10-25 parts of (0.3-1 parts of) and (the heat-insulating powder comprises (by weight) cement powder.
The invention also provides a preparation method of the low-cost non-ablative sandwich heat-resistant structural material, which comprises the following steps:
S1, performing sol dipping and shaping treatment on the spacer fabric to obtain a sandwich structure framework;
S2, preparing heat insulation slurry: the method comprises the steps of adopting a stirring device to fully mix heat-insulating powder, fiber powder and cement powder, and then adding a mixed solution of a surfactant and deionized water into the stirring device to continuously stir for 10-30 min to form heat-insulating slurry with low viscosity and good fluidity;
S3, vertically placing the sandwich structure skeleton obtained in the S1 into an impregnating tank, pouring the heat-insulating slurry obtained in the S2 into the impregnating tank, fixing the impregnating tank on a vibrating table, continuously vibrating at a preset vibration frequency, standing after the heat-insulating slurry is completely filled into a middle sandwich layer of the sandwich structure skeleton, and obtaining a sandwich structure/heat-insulating slurry complex after the heat-insulating slurry is solidified;
S4, drying at normal pressure: and (3) placing the sandwich structure/heat-insulating slurry composite obtained in the step (S3) into a blast drying box, drying at normal pressure at a preset temperature, and taking out after the moisture in the sandwich structure/heat-insulating slurry composite slurry is completely removed, thereby obtaining the low-cost non-ablative sandwich heat-insulating structure material.
Further, in the step S2: the proportion of the surfactant and the deionized water is calculated according to mass fraction: (0.3-1 parts of (180-300 parts); the time for fully mixing the heat-insulating powder with the fiber powder and the cement powder is 0.5-4 h; in the step S3: the vibration frequency of the vibration table is 60-120 Hz, the amplitude is 0.5-2 mm, and the vibration time is 10-30 min; standing for 0.5-2 h; in the step S4: the drying temperature is 70-120 ℃, and the drying time is 2-24 hours.
Compared with the prior art, the invention has the following advantages:
(1) The invention provides a low-cost non-ablative sandwich heat-proof structural material, which takes a spacer fabric as a framework through sol dipping and shaping treatment, wherein the spacer fabric is a fabric knitting structure and form commonly used in the prior art, especially in the textile field, and comprises two parallel fabric planes and vertical yarns or vertical tissues (namely fiber core columns) for connecting the two fabric planes, and a layer where the fiber core columns are positioned is a spacer space layer of the invention; the structure can enable structural materials to be integrated automatically, sewing or needling connection technology between the surface layers does not exist, the framework forms the whole of the layer structure, and the risks of connection looseness and falling between the surface layers are avoided; the sandwich heat-proof structural material suitable for being used in the temperature range of 400-1200 ℃ can be prepared by selecting different inorganic material for spacer fabrics and an antioxidant ceramic fiber and nanometer heat-proof material system;
(2) The commercial common spacer fabric has certain flexibility on the macroscopic scale, is not stiff and smooth, and is difficult to control the product profile precision when being directly used, so that the spacer fabric is firstly subjected to sol dipping and shaping treatment to obtain a supporting framework structure consisting of a compact upper layer, a compact lower layer and a fiber core column structure, namely: after the spacer fabric is subjected to sol impregnation, air drying and high-temperature heat treatment, the upper layer and the lower layer of the spacer fabric respectively form a compact ceramic fiber reinforced oxide ceramic matrix composite surface layer with corresponding thickness, which is equivalent to a sandwich heat-resistant structural material, and the upper and lower surfaces of the spacer fabric are ceramic panels, so that the spacer fabric has the high-temperature-resistant and ablation-resistant functions.
(3) The low-cost non-ablative sandwich heat-resistant structural material provided by the invention has the advantages that the heat-insulating medium is filled in the middle core layer of the framework, and the obtained sandwich heat-resistant structural material has good high temperature resistance and ablation resistance: from the material system, the sandwich heat-proof structure is composed of a sandwich structure skeleton and a heat-proof medium, wherein the heat-proof medium comprises fiber powder, heat-proof powder and cement powder, the fiber powder plays the roles of inhibiting high-temperature radiation heat transfer and reducing radiation heat conductivity coefficient in the heat-proof medium, the heat-proof powder can reduce the heat conductivity coefficient of a heat-proof structure material core layer, and the heat-proof powder and the heat-proof material core layer are mixed in a certain proportion to form the skeleton inner core layer, and an upper surface layer and a lower surface layer are added to ensure that the sandwich heat-proof structure material has good ablation resistance in the use process, no ablation on the surface and excellent high-temperature resistance and non-ablation performance.
(4) The sandwich heat-resistant structural material provided by the invention has low heat conductivity and high strength: firstly, after sol impregnation, air drying and high-temperature heat treatment, spacer yarns in the middle of the spacer fabric form a ceramic fiber reinforced oxide ceramic matrix composite material 'support column' structure, so that the prepared sandwich structure skeleton has good compressive strength (not lower than 0.15MPa and 3% deformation); secondly, the heat insulation medium comprises hydrophobic aerogel powder, and after the prepared heat insulation slurry is completely filled into the middle core layer of the sandwich skeleton by controlling the mass fractions of the hydrophobic aerogel, the surfactant and the cement, the thickness of the heat insulation slurry slightly expands (the thickness expansion rate is 2.3-8.2%) in the drying process of the baking oven, so that the heat insulation slurry in the core layer of the sandwich skeleton structure can be ensured to be still completely filled into the middle core layer after being dried, and micron-sized pores and cracks which are not beneficial to efficient heat insulation cannot occur; in addition, the nanometer heat insulation medium containing titanium oxide, zirconium oxide and silicon carbide fiber powder is filled in the middle of the sandwich structure spacing fabric (wherein the fiber powder can effectively inhibit the low radiation heat conductivity coefficient of the high-temperature radiation heat transfer endowing material, the aerogel heat insulation powder has low solid and gas heat conductivity coefficient), so that the sandwich heat insulation structure material has low high temperature heat conductivity at high temperature, and the lowest heat conductivity at 1000 ℃ is onlyAnd the compressive strength (not lower than 0.2MPa and 3% deformation) of the sandwich heat-resistant structural material is further improved.
(5) The sandwich heat-resistant structural material provided by the invention has the advantages of mild preparation process conditions and low cost: in the raw materials, the sandwich structure skeleton is derived from the spacer fabric woven by mature mechanical process, the sol used is produced in a commercial scale, water is used as the solvent, and the cost of the raw materials is low. In addition, the preparation process of the sandwich structure/heat insulation slurry composite is simple, and the slurry can be uniformly filled into the sandwich structure by adopting a simple vibrating table; the material has mild drying conditions, the drying process is carried out under normal pressure, the drying temperature is low (70-120 ℃), the drying time is short (2-24 h), and the energy consumption is low; the whole material flow does not adopt any organic solvent replacement and surface modification process, and does not use flammable and explosive organic solvents such as ethanol and the like, so that the explosion hazard is avoided; the gas released in the drying process is water gas, and is nontoxic and harmless to the environment. Therefore, the invention adopts the commercial low-cost raw materials, has simple equipment operation, safe and environment-friendly whole process, and low cost and the preparation process has warm conditions.
The sandwich heat-proof structure material with the performances of low cost, high temperature resistance, non-ablation, low thermal conductivity, high strength and the like is prepared by adopting the sol taking water as a solvent, sandwich structure spacer fabric, hydrophobic aerogel, cement powder, surfactant, deionized water and the like which are sold in the market as materials through 4 steps of preparing a sandwich structure skeleton, preparing heat-proof slurry, preparing a sandwich structure/heat-proof slurry composite body and drying at normal pressure. The preparation method has the advantages of mild preparation process conditions, safe, environment-friendly and short preparation period, low cost and easy realization of large-scale production.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings, wherein:
FIG. 1 is a schematic diagram of a sandwich heat-resistant material of the present invention;
FIG. 2 is a general flow chart of a method of preparing a sandwich heat resistant structural material of the present invention.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and detailed description for the purpose of enabling those skilled in the art to understand the invention better.
Example 1
Referring to fig. 1, an embodiment provides a low-cost non-ablative sandwich heat-proof structure material, which comprises a sandwich structure skeleton formed by a spacer fabric and a heat-insulating medium filled in a middle core layer of the sandwich structure skeleton; the total mass of the non-ablative sandwich heat-proof structural material is calculated as 100%, and the mass percentage of each component is as follows: 25% -60% of sandwich structure skeleton, and 40% -75% of heat insulation medium;
the sandwich structure framework is obtained by shaping a spacer fabric after sol impregnation;
The heat insulation medium comprises heat insulation powder, fiber powder, cement powder and surfactant.
The spacer fabric is integrally woven by ceramic fiber bundles and filaments with the linear density of 75-390 tex; the ceramic fiber bundle filaments are one or more of high silica fibers, quartz fibers, aluminum silicate fibers and aluminum oxide fibers;
The spacer fabric comprises an upper layer 1, a lower layer 4 and a spacer space layer 3, wherein fiber core posts 2 in the spacer space layer 3 are connected with the upper layer 1 and the lower layer 4; the thickness of the upper surface layer 1 and the lower surface layer 4 is 1-2 mm, and the thickness of the interval space layer 3 is 10-40 mm;
The fiber core column 2 in the interval space layer 3 forms an angle of 45 DEG + -5 DEG with the upper layer 1 and the lower layer 4.
Example 2
Referring to fig. 2, a method for preparing a low-cost non-ablative sandwich heat-resistant structural material is provided, comprising the following steps:
(1) Preparation of Sandwich Structure skeleton
Firstly, immersing a spacing fabric of a commercially available sandwich structure into a sol pool, taking the spacing fabric out of the sol pool, airing at room temperature, and performing high-temperature heat treatment to obtain a shaped sandwich structure framework, wherein the compression strength of the framework is 0.15MPa (3% deformation), and the bending strength of the framework is 19MPa.
Wherein, the upper layer of the spacer fabric is 1mm, the lower layer is 1mm, the thickness of the middle hollow interlayer is 17mm, and the spacer fabric is woven by adopting ceramic fiber bundles with the linear density of 195 tex. The spacing yarn of the spacing fabric is ceramic fiber bundle yarn with 75tex, and the inclination angle of the spacing yarn is equal to the upper plane and the lower planeThe ceramic fiber bundle filaments are quartz fibers; the sol is silica sol taking water as a solvent, the average particle diameter of the sol is 10nm, and the solid content of the sol is 35wt%; the high-temperature heat treatment temperature is 800 ℃, and the heat treatment time is 1h.
(2) Preparing heat insulation slurry
Firstly, crushing titanium oxide fiber with an average diameter of 2.3 mu m (which plays the roles of inhibiting high-temperature radiation heat transfer and reducing radiation heat conductivity coefficient in a heat insulation medium, wherein the highest using temperature can reach 1100 ℃) into fiber powder with an average length of 50 mu m, crushing silica aerogel blocks into aerogel powder which is used as heat insulation powder (with an average particle diameter of 30 mu m and very low solid and gas heat conductivity coefficient), fully mixing the heat insulation powder, the fiber powder and cement powder for 0.5h by adopting a stirring device, and then adding deionized water solution containing sodium dodecyl benzene sulfonate serving as a surfactant into the stirring device to continuously stir for 25min to form heat insulation slurry with low viscosity and good fluidity. The heat insulation cement comprises 15 parts of fiber powder, 20 parts of heat insulation powder, 0.5 part of cement powder, 220 parts of surfactant and deionized water in parts by mass.
(3) Preparation of Sandwich Structure/Heat insulation slurry composite
Firstly, vertically placing the sandwich structure skeleton obtained in the first step into an impregnating tank, pouring the heat-insulating slurry obtained in the second step into the impregnating tank, then fixing the impregnating tank on a vibrating table, continuously vibrating for 20min at a vibration frequency of 100Hz, wherein the amplitude is 0.5mm, and the heat-insulating slurry can completely fill the middle core layer of the sandwich structure skeleton under the continuous vibration condition due to low viscosity and good fluidity of the heat-insulating slurry, and standing for 0.5h, so that the sandwich structure/heat-insulating slurry composite is obtained after the heat-insulating slurry is solidified.
(4) Drying under normal pressure
And (3) placing the sandwich structure/heat-insulating slurry composite obtained in the third step into a forced air drying box, and drying for a period of time at normal pressure and a certain temperature, wherein the drying temperature is 80 ℃ and the drying time is 20 hours. In the drying process, the thickness of the solidified heat-insulating slurry in the step 3 after being dried is slightly expanded, the thickness expansion rate is 4.3%, and the fact that the middle core layer of the sandwich skeleton structure can be completely filled with heat-insulating medium is ensured, so that the low-cost non-ablative sandwich heat-insulating structure material is obtained.
The non-ablative sandwich heat-resistant structural material prepared in example 2 has a density of 0.45 g/cm 3 and a low thermal conductivity at 1000 DEG CThe thermal conductivity coefficient test method (water flow plate method) of YB/T4130-2005 refractory material is adopted (the same applies below), after heat treatment is carried out on 3600 s in muffle furnace air at 1000 ℃, the thickness shrinkage rate of the material is 0.48%, and the 3% deformation compression strength is 0.22 MPa.
Example 3
(1) Preparation of Sandwich Structure skeleton
Firstly, immersing a spacing fabric of a commercially available sandwich structure into a sol pool, taking the spacing fabric out of the sol pool, airing at room temperature, and performing high-temperature heat treatment to obtain a shaped sandwich structure framework, wherein the compression strength of the framework is 0.26MPa (3% deformation), and the bending strength of the framework is 15MPa.
Wherein, the upper surface layer of the spacer fabric has a thickness of 2mm, the lower surface layer has a thickness of 1mm, the middle hollow interlayer has a thickness of 25mm, and the spacer fabric is woven by adopting ceramic fiber bundles with a linear density of 225 tex. The spacer yarn of the spacer fabric is ceramic fiber bundle yarn with the thickness of 100tex, and the inclination angle of the spacer yarn is equal to the upper plane and the lower planeThe ceramic fiber bundle filaments are alumina fibers; the sol is a mixed sol (volume ratio is 1:3) of silica sol and alumina sol which take water as a solvent, the particle size of the two sols is 10-20 nm, and the solid content of the sol is 45wt%; the high-temperature heat treatment temperature is 1200 ℃, and the heat treatment time is 1h.
(2) Preparing heat insulation slurry
Firstly, crushing heat-insulating ceramic fibers into fiber powder, crushing aerogel blocks into aerogel powder to serve as heat-insulating powder, then adopting a stirring device to fully mix the heat-insulating powder with the fiber powder and the cement powder for 1h, and then adding deionized water solution containing a surfactant into the stirring device to continuously stir for 30min to form heat-insulating slurry with low viscosity and good fluidity.
The heat-insulating ceramic fibers are zirconium oxide and silicon carbide fibers (the mass ratio is 1:5, the two fibers play the roles of inhibiting high-temperature radiation heat transfer and reducing radiation heat conductivity coefficient in a heat-insulating medium, the fibers have higher temperature resistance than the titanium oxide fibers in the embodiment 2, the highest use temperature can reach more than 1200 ℃), the diameters are 3 mu m, and the average length of fiber powder is 100 mu m; the heat insulation powder is alumina aerogel, and the average grain diameter after crushing is 50 mu m; the cement powder is aluminate cement; the surfactant is fatty glyceride. The heat insulation type cement mortar comprises 20 parts by mass of fiber powder, 70 parts by mass of heat insulation powder, 1 part by mass of cement powder, 300 parts by mass of surfactant and deionized water.
(3) Preparation of Sandwich Structure/Heat insulation slurry composite
Firstly, vertically placing the sandwich structure skeleton obtained in the first step into an impregnating tank, pouring the heat-insulating slurry obtained in the second step into the impregnating tank, then fixing the impregnating tank on a vibrating table, continuously vibrating for a period of time at a certain vibration frequency of 120Hz with an amplitude of 0.5mm, completely filling the middle core layer of the sandwich structure skeleton with the heat-insulating slurry with low viscosity and good fluidity after the vibration time is 15min, standing for 1h, and obtaining the sandwich structure/heat-insulating slurry composite after the heat-insulating slurry is solidified.
(4) Drying under normal pressure
And (3) placing the sandwich structure/heat-insulating slurry composite obtained in the third step into a blast drying box, and drying for 2 hours at the normal pressure at 120 ℃, wherein the thickness of the heat-insulating slurry solidified in the step (3) after drying slightly expands, the thickness expansion rate is 7.1%, and the sandwich structure middle core layer can be completely filled with heat-insulating medium, so that the low-cost non-ablative sandwich heat-insulating structure material is obtained.
The non-ablative sandwich heat-resistant structural material prepared in example 3 had a density of 0.55g/cm 3 and a thermal conductivity of only 1000℃After heat treatment for 3600s in muffle furnace air at 1200 ℃, the thickness shrinkage rate of the material is 0.46%, and the 3% deformation compression strength is 0.32MPa.
Example 4
(1) Preparation of Sandwich Structure skeleton
Firstly, immersing a spacing fabric of a commercially available sandwich structure into a sol pool, taking the spacing fabric out of the sol pool, airing at room temperature, and performing high-temperature heat treatment to obtain a shaped sandwich structure framework, wherein the compression strength of the framework is 0.18MPa (3% deformation), and the bending strength of the framework is 13MPa.
Wherein, the thickness of the upper layer and the lower layer of the spacer fabric is 2mm and 1mm respectively, the thickness of the middle hollow interlayer is 40mm, and the spacer fabric is woven by ceramic fiber bundles with the linear density of 390 tex. The spacer yarn of the spacer fabric is ceramic fiber bundle yarn with the thickness of 100tex, and the inclination angle of the spacer yarn is equal to the upper plane and the lower planeThe ceramic fiber bundles can be high silica fibers; the sol is silica sol taking water as a solvent, the average particle diameter of the sol is 15nm, and the solid content of the sol is 40wt%; the high-temperature heat treatment temperature is 750 ℃, and the heat treatment time is 2h.
(2) Preparing heat insulation slurry
Firstly, crushing heat-insulating ceramic fibers into fiber powder, crushing aerogel blocks into aerogel powder to serve as heat-insulating powder, then adopting a stirring device to fully mix the heat-insulating powder with the fiber powder and the cement powder for 0.5h, and then adding deionized water solution containing a surfactant into the stirring device to continuously stir for 10min to form heat-insulating slurry with low viscosity and good fluidity.
Wherein the heat-insulating ceramic fiber is zirconia fiber, the average diameter of the fiber is 3 mu m, and the length of the fiber powder is 75 mu m; the heat insulation powder is a silicon oxide aerogel block, and the average grain diameter of the crushed aerogel is 45 mu m; the cement powder is silicate cement; the surfactant is sucrose ester. The heat insulation type cement mortar comprises, by mass, 5 parts of fiber powder, 45 parts of heat insulation powder, 15 parts of cement powder, 0.5 part of surfactant and 180 parts of deionized water.
(3) Preparation of Sandwich Structure/Heat insulation slurry composite
Firstly, vertically placing the sandwich structure skeleton obtained in the first step into an impregnating tank, pouring the heat-insulating slurry obtained in the second step into the impregnating tank, then fixing the impregnating tank on a vibrating table, wherein the vibration frequency of the vibrating table is 90Hz, the vibration amplitude is 0.5mm, after the vibration time is 20min, the heat-insulating slurry with low viscosity and good fluidity completely fills the middle core layer of the sandwich structure skeleton, standing for 2h, and obtaining the sandwich structure/heat-insulating slurry composite after the heat-insulating slurry is solidified.
(4) Drying under normal pressure
And (3) placing the sandwich structure/heat-insulating slurry composite obtained in the third step into a blast drying box, wherein the drying temperature is 95 ℃, the drying time is 18h, and in the drying process, the thickness of the heat-insulating slurry solidified in the step (3) after drying is slightly expanded, and the thickness expansion rate is 2.3%, so that the middle core layer of the sandwich skeleton structure can be completely filled with heat-insulating medium, and the low-cost non-ablative sandwich heat-insulating structure material is obtained.
The non-ablative sandwich heat resistant structural material prepared in example 4 had a density of 0.45g/cm 3 and a thermal conductivity of only 1000℃After heat treatment in muffle furnace air at 1000 ℃ for 3600s, the thickness shrinkage rate of the material is 0.74%, and the 3% deformation compression strength is 0.26MPa.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims (9)

1. The low-cost non-ablative sandwich heat-resistant structural material is characterized by comprising a sandwich structure framework formed by spacer fabrics and a heat-insulating medium filled in a middle core layer of the sandwich structure framework; the total mass of the non-ablative sandwich heat-proof structural material is calculated as 100%, and the mass percentage of each component is as follows: 25% -60% of sandwich structure skeleton, and 40% -75% of heat insulation medium;
the sandwich structure framework is obtained by shaping a spacer fabric after sol impregnation;
The heat insulation medium comprises heat insulation powder, fiber powder, cement powder and surfactant.
2. The low cost non-ablative sandwich thermal barrier material of claim 1, wherein,
The spacer fabric is integrally woven by ceramic fiber bundles and filaments with the linear density of 75-390 tex; the ceramic fiber bundle filaments are one or more of high silica fibers, quartz fibers, aluminum silicate fibers and aluminum oxide fibers;
The spacer fabric comprises an upper layer (1), a lower layer (4) and a spacer space layer (3), wherein the fiber core column (2) in the spacer space layer (3) is connected with the upper layer (1) and the lower layer (4); the thickness of the upper layer (1) and the lower layer (4) is 1-2 mm, and the thickness of the interval space layer (3) is 10-40 mm;
the fiber core column (2) in the interval space layer (3) forms an angle of 45 degrees plus or minus 5 degrees with the upper layer (1) and the lower layer (4).
3. The low cost non-ablative sandwich thermal barrier material of claim 1, wherein,
The sol for impregnating the spacer fabric is silica sol and/or alumina sol with water as a solvent, wherein the particle size of the sol is 10-20 nm, and the solid content of the sol is 35-50 wt%;
The shaping treatment after sol impregnation comprises the following steps: and taking out the spacer fabric from the sol pool after sol impregnation, and airing at room temperature and carrying out high-temperature heat treatment to obtain the shaped sandwich structure framework, wherein the high-temperature heat treatment temperature is 600-1200 ℃, and the high-temperature treatment time is 0.5-2 h.
4. The low cost non-ablative sandwich thermal barrier material of claim 1, wherein,
The fiber powder is formed by crushing heat-insulating ceramic fibers with the diameter of 2-3 mu m, and the heat-insulating ceramic fibers are any one or more of titanium oxide, zirconium oxide and silicon carbide fibers; the length of the fiber powder is 50-100 μm.
5. The low cost non-ablative sandwich thermal barrier material of claim 1, wherein,
The heat insulation powder is aerogel powder formed by crushing hydrophobic aerogel blocks, wherein the hydrophobic aerogel blocks are hydrophobic silica aerogel and/or alumina aerogel blocks; the particle size of the heat insulation powder is 20-50 mu m.
6. The low cost non-ablative sandwich thermal barrier material of claim 1, wherein,
The cement powder is silicate cement and/or aluminate cement;
The surfactant is one or two of sodium dodecyl benzene sulfonate, alkyl glucoside, fatty glyceride, sucrose ester and fatty alcohol ester.
7. The low cost non-ablative sandwich thermal barrier material of claim 1, wherein,
The heat insulation medium comprises the following components: the heat-insulating powder comprises (by weight) 5-20 parts of a surfactant, (40-70 parts of) 10-25 parts of (0.3-1 parts of) and (the heat-insulating powder comprises (by weight) cement powder.
8. The method of preparing a low cost non-ablative sandwich heat resistant structural material according to any one of claims 1 to 7, comprising the steps of:
S1, performing sol dipping and shaping treatment on the spacer fabric to obtain a sandwich structure framework;
S2, preparing heat insulation slurry: the method comprises the steps of adopting a stirring device to fully mix heat-insulating powder, fiber powder and cement powder, and then adding a mixed solution of a surfactant and deionized water into the stirring device to continuously stir for 10-30 min to form heat-insulating slurry with low viscosity and good fluidity;
S3, vertically placing the sandwich structure skeleton obtained in the S1 into an impregnating tank, pouring the heat-insulating slurry obtained in the S2 into the impregnating tank, fixing the impregnating tank on a vibrating table, continuously vibrating at a preset vibration frequency, standing after the heat-insulating slurry is completely filled into a middle sandwich layer of the sandwich structure skeleton, and obtaining a sandwich structure/heat-insulating slurry complex after the heat-insulating slurry is solidified;
S4, drying at normal pressure: and (3) placing the sandwich structure/heat-insulating slurry composite obtained in the step (S3) into a blast drying box, drying at normal pressure at a preset temperature, and taking out after the moisture in the sandwich structure/heat-insulating slurry composite slurry is completely removed, thereby obtaining the low-cost non-ablative sandwich heat-insulating structure material.
9. The method for preparing the low-cost non-ablative sandwich heat-resistant structural material according to claim 8, wherein,
In the step S2:
the proportion of the surfactant and the deionized water is calculated according to mass fraction: (0.3-1 parts of (180-300 parts);
the time for fully mixing the heat-insulating powder with the fiber powder and the cement powder is 0.5-4 h;
In the step S3:
the vibration frequency of the vibration table is 60-120 Hz, the amplitude is 0.5-2 mm, and the vibration time is 10-30 min;
Standing for 0.5-2 h;
in the step S4: the drying temperature is 70-120 ℃, and the drying time is 2-24 hours.
CN202410352905.9A 2024-03-26 2024-03-26 Low-cost non-ablative sandwich heat-resistant structural material and preparation method thereof Pending CN117945711A (en)

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