CN112341227A - High-temperature-resistant nano heat-insulating material and preparation method thereof - Google Patents
High-temperature-resistant nano heat-insulating material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-temperature-resistant nano heat-insulating material and a preparation method thereof, wherein the heat-insulating material comprises ceramic fibers, an opacifier and nano mullite, wherein the use temperature of the ceramic fibers is higher than 1400 ℃; the opacifier is selected from one or the combination of zirconium oxide or zirconium silicate, and the nano mullite is generated by the in-situ reaction of nano silicon oxide and nano aluminum oxide under a hot pressing environment; the mass ratio of the nano mullite to the opacifier to the ceramic fiber is 3.55 (0-1) to 0.03-0.35. The preparation method comprises the following steps: dispersing and mixing the raw materials according to the proportion to obtain composite powder; filling the composite powder into a forming die; and carrying out in-situ reaction in a hot-pressing environment to generate the fiber-reinforced mullite high-temperature-resistant nano heat-insulating material. The material has excellent heat insulating performance, and good overall strength and processability. Meanwhile, the preparation method has high forming precision on the external dimension, and is suitable for occasions with higher requirements on the dimensional precision of the heat-insulating material.
Description
Technical Field
The invention belongs to the technical field of heat insulation materials, and particularly relates to a 1400 ℃ high-temperature resistant nano heat insulation material and a preparation method thereof.
Background
The nano material has a pore structure and the size of solid phase particles is in the nano level, so that heat conduction and heat convection are effectively inhibited, the nano material has excellent heat insulation performance, and the nano material is applied to the fields of buildings, kilns, long-distance pipeline heat insulation and the like. The nano heat insulation material is also an ideal material for a thermal protection system of the hypersonic aircraft, and can block heat from being transferred to the cabin in a limited space.
SiO widely researched and applied at present2Aerogel material with long-term service temperature not higher than 650 deg.C and SiO2/Al2O3The use temperature of the composite nanometer heat-insulating material can be increased to 1100 ℃. With the increasing requirements of hypersonic aircrafts on flying speed, time and penetration capacity, the temperature of the outer surface of the aircraft is higher and higher, and higher requirements are provided for the use temperature of a thermal protection material. Therefore, the research and preparation of the nano heat-insulating material suitable for higher use temperature has very important significance.
Disclosure of Invention
In order to overcome the defects in the prior art, the inventor of the invention carries out intensive research and provides a high-temperature-resistant nano heat-insulating material and a preparation method thereof, the prepared nano heat-insulating material has the use temperature of more than 1400 ℃, and meanwhile, the preparation method ensures that the final product has high contour dimension forming precision and is suitable for occasions with higher requirements on the dimension precision of the heat-insulating material, thereby completing the invention.
The technical scheme provided by the invention is as follows:
in a first aspect, a high temperature resistant nano-insulation material comprises: ceramic fiber, opacifier and nano mullite, wherein the service temperature of the ceramic fiber is higher than 1400 ℃;
the opacifier is selected from one or the combination of zirconium oxide or zirconium silicate,
the nano mullite is generated by the in-situ reaction of nano silicon oxide and nano aluminum oxide in a hot-pressing environment;
the mass ratio of the nano mullite to the opacifier to the ceramic fiber is 3.55 (0-1) to 0.03-0.35.
In a second aspect, the high-temperature-resistant nano heat-insulating material is prepared from the following raw materials in parts by mass: 1 part of nano silicon oxide, 2.55 parts of nano aluminum oxide, 0-1 part of opacifier and 0.03-0.35 part of ceramic fiber.
In a third aspect, a method for preparing a high temperature resistant nano heat insulation material is used for preparing the high temperature resistant nano heat insulation material of the first aspect or the second aspect, and comprises the following steps:
step 1, dispersing and mixing nano silicon oxide, nano aluminum oxide, an opacifier and ceramic fibers to obtain composite powder;
step 2, filling the composite powder into a forming die;
step 3, placing the forming die filled with the composite powder in a hot pressing furnace, heating to a reaction temperature, keeping the temperature for a set time, pressurizing, and continuing to keep the temperature and pressure;
and 4, cooling to room temperature, taking out the mold, and demolding to obtain the fiber-reinforced mullite high-temperature-resistant nano heat-insulating material.
According to the high-temperature-resistant nano heat-insulating material and the preparation method thereof provided by the invention, the following beneficial effects are achieved:
(1) the fiber-reinforced mullite nano heat-insulating material is prepared by a hot-pressing method in-situ reaction, the use temperature can be higher than 1400 ℃ in an aerobic environment, and the applicable temperature range of the nano heat-insulating material is greatly improved;
(2) the fiber-reinforced mullite nano heat-insulating material contains uniformly dispersed opacifier, and the high-temperature heat-insulating property is obviously superior to that of fiber heat-insulating materials such as mullite felt and the like;
(3) the invention adopts a hot pressing method to generate the nano mullite by in-situ reaction, and the 'micro sintering' occurs among particles, so that the prepared fiber reinforced mullite nano heat-insulating material has higher strength and integrity;
(4) the invention designs the special mould for preparing the nano heat insulation material, the forming precision of the external dimension of the nano heat insulation material is high, meanwhile, the mould can be correspondingly designed according to the structural appearance of the nano heat insulation material, the preparation of the high temperature resistant nano heat insulation material with different structural appearances is realized, and the method has the advantages of wide application range, flexibility, variety and easy realization, and is simultaneously suitable for occasions with higher requirements on the dimensional precision of the heat insulation material.
Drawings
FIG. 1 is a schematic view of a forming mold used in the present invention, wherein FIG. 1a is a front view and FIG. 1b is a top view;
FIG. 2 is an XRD pattern of the nano-insulation material in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of the fiber-reinforced mullite nano refractory thermal insulation material in example 1 of the present invention.
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 a first aspect of the present invention, there is provided a high temperature resistant nano-insulation material comprising ceramic fibers, an opacifier and nano-mullite, wherein,
the ceramic fiber is used at a temperature higher than 1400 ℃, preferably selected from one of alumina fiber, silicon carbide fiber and mullite fiber or the combination thereof. The ceramic fibers have a diameter of 1 to 10 μm, a length of 0.5 to 10mm, preferably a length of 3 to 7mm, which are easy to disperse/mix and sufficient in reinforcing effect;
the opacifier is selected from one or the combination of zirconium oxide or zirconium silicate, and the zirconium oxide or the zirconium silicate is inert at high temperature and does not react with other raw material components. Furthermore, the particle diameter of the opacifier is 1-5 microns, and the particle diameter can better block infrared radiation heat transfer at 1400 ℃.
The nano mullite is generated by the in-situ reaction of nano silicon oxide and nano aluminum oxide in a hot-pressing environment. Wherein, the nano silicon oxide is selected from one or the combination of silicon oxide aerogel powder or gas-phase method silicon oxide powder.
The nano alumina is selected from one or a combination of alumina aerogel powder and gas phase method alumina powder.
The nano silicon oxide and the nano aluminum oxide can also be silicon oxide-aluminum oxide binary aerogel powder.
The mass ratio of the nano mullite to the opacifier to the ceramic fiber is 3.55 (0-1) to 0.03-0.35.
According to a second aspect of the invention, a high-temperature-resistant nano heat-insulating material is provided, which is prepared from the following raw materials in parts by mass: 1 part of nano silicon oxide, 2.55 parts of nano aluminum oxide, 0-1 part of opacifier and 0.03-0.35 part of ceramic fiber.
The ceramic fiber is used at a temperature higher than 1400 ℃, preferably selected from one of alumina fiber, silicon carbide fiber and mullite fiber or the combination thereof. The ceramic fiber has a diameter of 1 to 10 μm, a length of 0.5 to 10mm, and preferably a length of 3 to 7 mm.
The opacifier is selected from one or the combination of zirconium oxide or zirconium silicate, and the zirconium oxide or the zirconium silicate is inert at high temperature and does not react with other raw material components. Further, the particle diameter of the opacifier is 1-5 μm.
The nano silicon oxide is selected from one or the combination of silicon oxide aerogel powder or gas-phase silicon oxide powder.
The nano alumina is selected from one or a combination of alumina aerogel powder and gas phase method alumina powder.
The nano silicon oxide and the nano aluminum oxide can also be silicon oxide-aluminum oxide binary aerogel powder.
According to a third aspect of the present invention, a method for preparing a high temperature resistant nano heat insulating material is provided, which is used for preparing the high temperature resistant nano heat insulating material of the first aspect or the second aspect, and comprises the following steps:
step 1, dispersing and mixing nano silicon oxide, nano aluminum oxide, an opacifier and ceramic fibers to obtain composite powder;
step 2, filling the composite powder into a forming die;
step 3, placing the forming die filled with the composite powder in a hot pressing furnace, heating to a reaction temperature, keeping the temperature for a set time, pressurizing, and continuing to keep the temperature and pressure;
and 4, cooling to room temperature, taking out the mold, and demolding to obtain the fiber-reinforced mullite high-temperature-resistant nano heat-insulating material.
In the present invention, the nano-silica, the nano-alumina, the opacifier and the ceramic fiber are the same as the corresponding raw materials in the first aspect or the second aspect, and the detailed description is omitted.
In the invention, in step 1, the mass ratio of the nano silicon oxide to the nano aluminum oxide to the opacifier to the ceramic fiber is as follows: 1:2.55 (0-1) and (0.03-0.35).
In the invention, in the step 2, the forming die comprises a female die, a male die and a side die, wherein the side die is sleeved on the peripheries of the female die and the male die, and the molded surface formed by the female die, the male die and the side die is consistent with the molded surface of the nano heat-insulating material to be processed.
In the invention, in the step 3, the reaction temperature is 1000-1400 ℃, the heat preservation time is 1-3 h, the pressure is 0.3-4 MPa, and the heat preservation and pressure maintaining time is 1-5 h.
Through a large number of experiments, the inventor finds that nano mullite cannot be generated if the reaction temperature is lower than 1000 ℃, and nano particles are seriously sintered if the reaction temperature is higher than 1400 ℃; if the pressure is lower than 0.3MPa, the obtained material has lower strength, and if the pressure is higher than 4MPa, the material has too high density and poor heat insulation performance.
In the process of the step 3, the nano-silicon oxide and the nano-aluminum oxide react in situ to generate the nano-mullite, so that the use temperature of the final nano-thermal insulation material in an aerobic environment can be higher than 1400 ℃. Meanwhile, micro sintering occurs among the nano mullite particles, and the overall strength and the processability are good.
Examples
Example 1
The fiber reinforced mullite high temperature resistant nano heat insulating material prepared in this example is a partial cylindrical structure, as shown in fig. 1.
In the embodiment, the nano silicon oxide is A380 type gas phase method silicon oxide, the nano aluminum oxide is AluC type gas phase method aluminum oxide, and the ceramic fiber is mullite fiber (the length is 0.5-10 mm, and the diameter is 1-10 μm); the mass ratio of the gas-phase method silicon oxide to the gas-phase method aluminum oxide to the mullite fiber is 1:2.55: 0.05.
In this embodiment, the molding die is designed in a partial cylindrical structure and is obtained by processing graphite. The forming die consists of a female die, a male die and a side die, wherein the male die is of a convex surface structure matched with the cylindrical concave surface, the female die is of a concave surface structure matched with the cylindrical convex surface, and the side die is cylindrical.
The preparation method of the fiber reinforced mullite high temperature resistant nano heat insulation material in the embodiment comprises the following steps:
(1) putting the raw materials weighed in proportion into a high-speed dispersion machine for dispersion and mixing to obtain composite powder;
(2) sleeving a side die into the female die to form a cavity, filling the composite powder into the cavity, putting the male die into the side die, and putting the whole die into a hot pressing furnace;
(3) heating the autoclave to 1300 ℃, preserving heat for 2h, slowly pressurizing to 1.0MPa, preserving heat and maintaining pressure for 3 h;
(4) and cooling to room temperature, taking out the mold, and demolding to obtain the fiber-reinforced mullite high-temperature-resistant nano heat-insulating material.
An XRD (X-ray diffraction) pattern of mullite particles in the fiber-reinforced mullite high-temperature-resistant nano heat-insulating material prepared in the embodiment is shown in figure 2, a scanning electron microscope image is shown in figure 3, the heat conductivity of the material is 0.056W/m.K, the linear shrinkage rate of the material is less than or equal to 1.5% when the material is subjected to heat treatment at 1400 ℃ for 30min, and the compression strength of the material is 0.5 MPa.
Example 2
The fiber reinforced mullite high temperature resistant nano heat insulating material prepared in the embodiment has a partial cylindrical structure.
In the embodiment, the nano-silica is silica aerogel, the nano-alumina is alumina aerogel, the opacifier is zirconium silicate (the diameter is 1-5 μm), and the ceramic fiber is alumina fiber (the length is 0.5-10 mm, the diameter is 1-10 μm); the mass ratio of the silica aerogel to the alumina aerogel to the zirconium silicate to the alumina fiber is 1:2.55:0.25: 0.04.
In this embodiment, the molding die is designed in a partial cylindrical structure and is obtained by processing graphite. The forming die consists of a female die, a male die and a side die, wherein the male die is of a convex surface structure matched with the cylindrical concave surface, the female die is of a concave surface structure matched with the cylindrical convex surface, and the side die is cylindrical.
The preparation method of the fiber reinforced mullite high temperature resistant nano heat insulation material in the embodiment comprises the following steps:
(1) putting the raw materials weighed in proportion into a high-speed dispersion machine for dispersion and mixing to obtain composite powder;
(2) sleeving a side die into the female die to form a cavity, filling the composite powder into the cavity, putting the male die into the side die, and putting the whole die into a hot pressing furnace;
(3) heating the autoclave to 1250 ℃, preserving heat for 1h, slowly pressurizing to 1.3MPa, preserving heat and maintaining pressure for 2 h;
(4) and cooling to room temperature, taking out the mold, and demolding to obtain the fiber-reinforced mullite high-temperature-resistant nano heat-insulating material.
The thermal conductivity of the fiber reinforced mullite high temperature resistant nano heat insulating material prepared by the embodiment is 0.051W/m.K, the linear shrinkage rate of the fiber reinforced mullite high temperature resistant nano heat insulating material is less than or equal to 1.9 percent after heat treatment at 1400 ℃ for 30min, and the compression strength is 0.4 MPa.
Example 3
The fiber reinforced mullite high temperature resistant nano heat insulating material prepared in the embodiment has a partial cylindrical structure.
In this embodiment, the nano-silica and nano-alumina are in molar ratio n (Al)2O3):n(SiO2) The silica-alumina binary aerogel prepared in a ratio of 3:2 is prepared, wherein the opacifier is zirconia (the diameter is 1-5 mu m), and the ceramic fiber is alumina fiber (the length is 0.5-10 mm, and the diameter is 1-10 mu m); silica-alumina binary aerogel, oxygenThe mass ratio of the zirconium oxide to the alumina fiber is 1:0.06: 0.05.
In this embodiment, the molding die is designed in a partial cylindrical structure and is obtained by processing graphite. The forming die consists of a female die, a male die and a side die, wherein the male die is of a convex surface structure matched with the cylindrical concave surface, the female die is of a concave surface structure matched with the cylindrical convex surface, and the side die is cylindrical.
The preparation method of the fiber reinforced mullite high temperature resistant nano heat insulation material in the embodiment comprises the following steps:
(1) putting the raw materials weighed in proportion into a high-speed dispersion machine for dispersion and mixing to obtain composite powder;
(2) sleeving a side die into the female die to form a cavity, filling the composite powder into the cavity, putting the male die into the side die, and putting the whole die into a hot pressing furnace;
(3) heating the autoclave to 1200 ℃, preserving heat for 2h, slowly pressurizing to 1.5MPa, preserving heat and maintaining pressure for 3 h;
(4) and cooling to room temperature, taking out the mold, and demolding to obtain the fiber reinforced mullite nano heat insulating material.
The thermal conductivity of the fiber-reinforced mullite high-temperature-resistant nano heat-insulating material prepared by the embodiment is 0.048W/m.K, the linear shrinkage rate of the fiber-reinforced mullite high-temperature-resistant nano heat-insulating material is less than or equal to 2.1 percent after heat treatment at 1400 ℃ for 30min, and the compressive strength of the fiber-reinforced mullite high-temperature-resistant nano heat-.
Example 4
In this embodiment, the fiber-reinforced mullite refractory nano-thermal insulation material has a flat structure (not shown in this embodiment).
In the embodiment, the nano-silica is A380 type gas phase method silica, the nano-alumina is AluC type gas phase method alumina, the opacifier is zirconium silicate (the diameter is 1-5 μm), the ceramic fiber is mullite fiber (the length is 0.5-10 mm, the diameter is 1-10 μm); the mass ratio of the gas-phase method silicon oxide to the gas-phase method aluminum oxide to the zirconium silicate to the mullite fiber is 1:2.55:0.15: 0.04.
The molding die in this example was designed to be flat and was machined from graphite. The forming die consists of a female die, a male die and a side die, wherein the male die and the female die are both flat plates, and the side die is cylindrical.
The preparation method of the fiber reinforced mullite high temperature resistant nano heat insulation material in the embodiment comprises the following steps:
(1) putting the raw materials weighed in proportion into a high-speed dispersion machine for dispersion and mixing to obtain composite powder;
(2) sleeving a side die into the female die to form a cavity, filling the composite powder into the cavity, putting the male die into the side die, and putting the whole die into a hot pressing furnace;
(3) heating the autoclave to 1350 ℃, preserving heat for 2h, slowly pressurizing to 0.6MPa, preserving heat and maintaining pressure for 3 h;
(4) and cooling to room temperature, taking out the mold, and demolding to obtain the fiber reinforced mullite nano heat insulating material.
The thermal conductivity of the fiber reinforced mullite high-temperature resistant nano heat-insulating material prepared by the embodiment is 0.050W/m.K, the linear shrinkage rate of the fiber reinforced mullite high-temperature resistant nano heat-insulating material is less than or equal to 1.5% after heat treatment at 1400 ℃ for 30min, and the compression strength is 0.3 MPa.
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 (10)
1. A high-temperature-resistant nano heat-insulating material is characterized by comprising ceramic fibers, an opacifier and nano mullite, wherein the use temperature of the ceramic fibers is higher than 1400 ℃;
the opacifier is selected from one or the combination of zirconium oxide or zirconium silicate,
the nano mullite is generated by the in-situ reaction of nano silicon oxide and nano aluminum oxide in a hot-pressing environment;
the mass ratio of the nano mullite to the opacifier to the ceramic fiber is 3.55 (0-1) to 0.03-0.35.
2. The nano heat insulation material of claim 1, wherein the ceramic fibers are selected from one or a combination of alumina fibers, silicon carbide fibers or mullite fibers, the length of the fibers is 0.5-10 mm, and the diameter of the fibers is 1-10 μm.
3. The nano heat insulating material of claim 1, wherein the particle diameter of the opacifier is 1 to 5 μm.
4. The nano-insulation material as claimed in claim 1, wherein the nano-silica is selected from one or a combination of silica aerogel powder and gas-phase silica powder, and the nano-alumina is selected from one or a combination of alumina aerogel powder and gas-phase alumina powder;
or the nano silicon oxide and the nano aluminum oxide are silicon oxide-aluminum oxide binary aerogel powder.
5. The high-temperature-resistant nano heat-insulating material is characterized by being prepared from the following raw materials in parts by mass: 1 part of nano silicon oxide, 2.55 parts of nano aluminum oxide, 0.14-1 part of opacifier and 0.03-0.35 part of ceramic fiber.
6. The nano-insulation material of claim 5, wherein the ceramic fibers should be used at a temperature higher than 1400 ℃;
the opacifier is selected from one or the combination of zirconium oxide or zirconium silicate;
the nano-silica is selected from one or the combination of silica aerogel powder or gas-phase method silica powder, and the nano-alumina is selected from one or the combination of alumina aerogel powder or gas-phase method alumina powder; or the nano silicon oxide and the nano aluminum oxide are silicon oxide-aluminum oxide binary aerogel powder.
7. The nano heat insulation material of claim 6, wherein the ceramic fiber is selected from one or a combination of alumina fiber, silicon carbide fiber or mullite fiber, the length of the fiber is 0.5-10 mm, and the diameter is 1-10 μm; and/or
The particle diameter of the opacifier is 1-5 mu m.
8. A method for preparing a high temperature resistant nano heat insulating material according to one of claims 1 to 4 or 5 to 7, comprising:
step 1, dispersing and mixing nano silicon oxide, nano aluminum oxide, an opacifier and ceramic fibers to obtain composite powder;
step 2, filling the composite powder into a forming die;
step 3, placing the forming die filled with the composite powder in a hot pressing furnace, heating to a reaction temperature, keeping the temperature for a set time, pressurizing, and continuing to keep the temperature and pressure;
and 4, cooling to room temperature, taking out the mold, and demolding to obtain the fiber-reinforced mullite high-temperature-resistant nano heat-insulating material.
9. The preparation method according to claim 8, wherein in the step 2, the forming mold comprises a female mold, a male mold and a side mold, the side mold is sleeved on the periphery of the female mold and the male mold, and the molded surface formed by the female mold, the male mold and the side mold is in accordance with the molded surface of the nano heat-insulating material to be processed.
10. The preparation method according to claim 8, wherein in the step 3, the reaction temperature is 1000 to 1400 ℃, the holding time is 1 to 3 hours, the pressure is 0.3 to 4MPa, and the holding time is 1 to 5 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115700234A (en) * | 2022-10-27 | 2023-02-07 | 广州世陶新材料有限公司 | Fiber-reinforced low-density porous heat-insulating material and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4590132A (en) * | 1984-10-25 | 1986-05-20 | Toyota Jidosha Kabushiki Kaisha | Composite material reinforced with alumina-silica fibers including mullite crystalline form |
| CN104210151A (en) * | 2014-08-22 | 2014-12-17 | 航天材料及工艺研究所 | Surface-reinforced high-temperature-resistant nanometer thermal insulation material and preparation method thereof |
| CN105036785A (en) * | 2015-07-13 | 2015-11-11 | 上海柯瑞冶金炉料有限公司 | Composition and manufacturing method for high-temperature type non-burning nanometer microporous heat-insulating material |
| CN105967728A (en) * | 2016-05-10 | 2016-09-28 | 航天材料及工艺研究所 | Fiber-enhanced Al2O3-SiO2 aerogel efficient heat isolation composite material and preparation method thereof |
| CN108046739A (en) * | 2017-12-06 | 2018-05-18 | 航天材料及工艺研究所 | A kind of fiber preform enhancing aerogel heat-proof composite material and preparation method thereof |
| CN108439964A (en) * | 2018-02-05 | 2018-08-24 | 响水华夏特材科技发展有限公司 | A kind of nano-pore ceramics thermal insulation coiled material and preparation method thereof |
| CN110194649A (en) * | 2019-06-24 | 2019-09-03 | 广州晖能环保材料有限公司 | Aluminium oxide nano heat-barrier material and preparation method thereof |
-
2020
- 2020-10-23 CN CN202011150112.7A patent/CN112341227A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4590132A (en) * | 1984-10-25 | 1986-05-20 | Toyota Jidosha Kabushiki Kaisha | Composite material reinforced with alumina-silica fibers including mullite crystalline form |
| CN104210151A (en) * | 2014-08-22 | 2014-12-17 | 航天材料及工艺研究所 | Surface-reinforced high-temperature-resistant nanometer thermal insulation material and preparation method thereof |
| CN105036785A (en) * | 2015-07-13 | 2015-11-11 | 上海柯瑞冶金炉料有限公司 | Composition and manufacturing method for high-temperature type non-burning nanometer microporous heat-insulating material |
| CN105967728A (en) * | 2016-05-10 | 2016-09-28 | 航天材料及工艺研究所 | Fiber-enhanced Al2O3-SiO2 aerogel efficient heat isolation composite material and preparation method thereof |
| CN108046739A (en) * | 2017-12-06 | 2018-05-18 | 航天材料及工艺研究所 | A kind of fiber preform enhancing aerogel heat-proof composite material and preparation method thereof |
| CN108439964A (en) * | 2018-02-05 | 2018-08-24 | 响水华夏特材科技发展有限公司 | A kind of nano-pore ceramics thermal insulation coiled material and preparation method thereof |
| CN110194649A (en) * | 2019-06-24 | 2019-09-03 | 广州晖能环保材料有限公司 | Aluminium oxide nano heat-barrier material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115700234A (en) * | 2022-10-27 | 2023-02-07 | 广州世陶新材料有限公司 | Fiber-reinforced low-density porous heat-insulating material and preparation method thereof |
| CN115700234B (en) * | 2022-10-27 | 2023-11-10 | 广州世陶新材料有限公司 | Fiber-reinforced low-density porous heat insulation material and preparation method thereof |
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