CN111606727B - High-temperature wave-transparent heat-insulating integrated fiber-reinforced gamma- (Y)1-xHox)2Si2O7Porous solid solution and preparation method - Google Patents
High-temperature wave-transparent heat-insulating integrated fiber-reinforced gamma- (Y)1-xHox)2Si2O7Porous solid solution and preparation method Download PDFInfo
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- 239000006104 solid solution Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000835 fiber Substances 0.000 claims abstract description 53
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 239000000919 ceramic Substances 0.000 claims abstract description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000007710 freezing Methods 0.000 claims abstract description 8
- 230000008014 freezing Effects 0.000 claims abstract description 8
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- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001746 injection moulding Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 16
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 7
- 239000004088 foaming agent Substances 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 108010010803 Gelatin Proteins 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
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- 235000011852 gelatine desserts Nutrition 0.000 claims description 5
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- 239000000203 mixture Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
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- 239000011812 mixed powder Substances 0.000 claims description 2
- 230000003014 reinforcing effect Effects 0.000 claims description 2
- 230000004888 barrier function Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 28
- OWCYYNSBGXMRQN-UHFFFAOYSA-N holmium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ho+3].[Ho+3] OWCYYNSBGXMRQN-UHFFFAOYSA-N 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000011268 mixed slurry Substances 0.000 abstract description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 2
- 238000001291 vacuum drying Methods 0.000 abstract description 2
- 150000002466 imines Chemical class 0.000 abstract 1
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 23
- 238000000034 method Methods 0.000 description 7
- 230000002787 reinforcement Effects 0.000 description 7
- 238000009413 insulation Methods 0.000 description 6
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- 239000004642 Polyimide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002078 fully stabilized zirconia Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
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- 229920001721 polyimide Polymers 0.000 description 1
- 239000013354 porous framework Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- -1 rare earth silicate Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
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Abstract
The invention relates to the field of high-temperature wave-transmitting heat-insulating multifunctional integrated materials, in particular to a high-temperature wave-transmitting heat-insulating integrated fiber reinforced gamma- (Y)1‑xHox)2Si2O7Porous solid solution and preparation method thereof, wherein the value range of x is 0<x<1. The preparation method comprises the steps of taking yttrium oxide, holmium oxide, silicon oxide powder and YSZ fibers as raw materials, selecting polyacetyl imine, ammonium citrate or citric acid as a dispersing agent, preparing ceramic powder mixed slurry with uniformly dispersed YSZ fibers, then carrying out rapid mechanical stirring foaming on the slurry, then carrying out injection molding and low-temperature freezing to form a blank, then carrying out vacuum drying, demoulding the blank and drying in an oven. Finally, the fiber reinforced gamma- (Y) is prepared by high-temperature reaction sintering1‑xHox)2Si2O7A porous solid solution. The preparation process is simple and easy to operate, the cost is low, the synthesized wave-transparent heat-insulating multifunctional integrated material has the characteristics of ultrahigh porosity, low high-temperature dielectric constant, low dielectric loss, low high-temperature heat conductivity and excellent high-temperature heat stability, and the industrial production and application prospects are very wide.
Description
Technical Field
The invention relates to the field of high-temperature wave-transmitting heat-insulating multifunctional integrated materials, in particular to a novel high-temperature wave-transmitting heat-insulating integrated fiber-reinforced gamma- (Y) with ultrahigh porosity, low high-temperature dielectric constant, low dielectric loss, low high-temperature heat conductivity and excellent high-temperature heat stability1-xHox)2Si2O7Porous solid solutions and methods for their preparation.
Background
With the rapid development of the aerospace industry, high-speed aircrafts play an increasingly important role. As the flying speed of the aircraft is faster and faster, the pneumatic heating effect is very serious, so that the temperature of the surface of the aircraft is extremely high and can reach over 1200 ℃. In order to meet the requirements of extreme service environments, the surface layer material of the aircraft needs to have multiple functions, and the requirements of wave transmission, bearing and the like are met while good high-temperature heat insulation is achieved. Therefore, there is a need to develop a novel material integrating multiple functions of wave transmission, heat insulation, load bearing and the like, which is light, high in strength, low in thermal conductivity, low in dielectric constant and high-temperature resistant, so as to meet the urgent need of aerospace industry development.
The traditional heat insulating material usually meets the service requirement of simple functions, and in order to simultaneously meet the multifunctional targets of wave transmission, heat insulation and bearing, a novel wave transmission and heat insulation integrated material needs to be developed. The rare earth silicate is an excellent candidate material for the high-temperature wave-transparent and heat-insulating integrated material due to the advantages of high melting point, low dielectric constant and low thermal conductivity.
Disclosure of Invention
The invention aims to provide a high-temperature wave-transmitting heat-insulating integrated fiber-reinforced gamma- (Y) with ultrahigh porosity, low high-temperature dielectric constant and dielectric loss, extremely low high-temperature heat conductivity and excellent thermal stability1-xHox)2Si2O7The porous solid solution and the preparation method thereof meet the requirements of high-temperature wave-transmitting and heat-insulating comprehensive properties.
The technical scheme of the invention is as follows:
high-temperature wave-transparent and heat-insulating integrated fiber-reinforced gamma- (Y)1-xHox)2Si2O7Porous solid solution in fiber reinforcement of gamma- (Y)1-xHox)2Si2O7In the porous solid solution finished product, the reinforcing phase YSZ fiber accounts for 5-50 wt%, and the rest is matrix gamma- (Y)1- xHox)2Si2O7The technical indexes are as follows: a porosity of 80-96%, a high-temperature dielectric constant of 1.2-2.5 at 1000 ℃ and a dielectric loss of 1.0X 10-3~7.5×10-2The high-temperature thermal conductivity at 600-1200 ℃ is 0.1-0.5W/(m.K), and the high-temperature thermal cycle shrinkage at 25-1550 ℃ is less than 1%.
The high-temperature wave-transparent heat-insulating integrated fiber-reinforced gamma- (Y)1-xHox)2Si2O7Porous solid solution in fiber reinforcement of gamma- (Y)1-xHox)2Si2O7In the final porous solid solution product, the porous composition comprises: the size distribution of macropores is 35-450 mu m, and the volume proportion of the macropores is 70-95%; the size of the small holes is 0.5-7.5 mu m, and the volume proportion of the small holes in the porous material is 30-5%.
The high-temperature wave-transparent heat-insulating integrated fiber-reinforced gamma- (Y)1-xHox)2Si2O7Porous solid solutions, preferably in fibre-reinforced gamma- (Y)1-xHox)2Si2O7In the porous solid solution finished product, the YSZ fiber accounts for 10-25 wt%.
The high-temperature wave-transparent heat-insulating integrated fiber-reinforced gamma- (Y)1-xHox)2Si2O7A preparation method of the porous solid solution, wherein the value range of x is 0<x<1, the added fiber is a zirconia fiber with yttria fully stabilized, and the specific steps are as follows:
1) preparing slurry: in parts by mass, as Y2O3、Ho2O3And SiO2Molar ratio (1-x): x: 2, taking 35-60 parts of mixed powder, 1-20 parts of YSZ fiber, 0.5-3 parts of dispersing agent and 60-80 parts of deionized water as raw materials, mixing and stirring for 2-4 hours to form slurry with uniformly dispersed fiber and ceramic powder;
2) foaming-pouring coagulation: heating the slurry to 35-50 ℃, adding 1-6 parts of foaming agent by weight, quickly and mechanically stirring for foaming for 10-25 minutes, adding 3-9 parts of gelatin as a gelling agent and 1-5 parts of polyethylene glycol as a surfactant, continuously and quickly and mechanically stirring for 15-50 minutes, and then injecting into a mold;
3) freeze drying-oven drying: placing the mold and a sample obtained by injection molding in a freezer at-20 to-50 ℃ for freezing for 5-24 hours, then vacuumizing for 12-36 hours until the vacuum degree is 1-20 Pa, then demolding and drying in an oven at 60-90 ℃ for 5-24 hours;
4) and (3) high-temperature sintering: high-temperature reaction sintering is carried out for 1-3 hours at 1450-1600 ℃ in the air, and the fiber reinforced gamma- (Y) is prepared1-xHox)2Si2O7A porous solid solution.
The high-temperature wave-transparent heat-insulating integrated fiber-reinforced gamma- (Y)1-xHox)2Si2O7The preparation method of the porous solid solution comprises the steps of using the dispersant as the polyacetimide, the ammonium citrate or the citric acid, and using the foaming agent as the sodium dodecyl sulfate or the sodium dodecyl sulfate.
The high-temperature wave-transparent heat-insulating integrated fiber-reinforced gamma- (Y)1-xHox)2Si2O7In the preparation method of the porous solid solution, in the step 2), the rotating speed range of a stirrer for rapid mechanical stirring is 1000-2500 rpm.
The design idea of the invention is as follows:
in order to obtain a high-temperature wave-transparent and heat-insulating integrated material with excellent comprehensive performance, a matrix needs to have extremely high porosity so as to realize extremely low dielectric constant, thermal conductivity and density of the material. Thus: firstly, the invention adopts a novel in-situ foaming-injection condensing-freeze drying technology to realize ultrahigh porosity and ultralight weight of the material. However, since the higher the porosity of the porous material is, the lower the strength is, the more effective means must be taken to improve the mechanical properties of the ultrahigh-porosity porous ceramic. Secondly, the invention improves the strength of the material by fiber reinforcement and solid solution reinforcement, so that the material has high strength at ultrahigh porosity. Meanwhile, the thermal conductivity of the material can be further reduced by the fiber reinforcement and solid solution method. Aiming at the working environment of the multifunctional integrated material is high temperature, even ultrahigh temperature, so the performance of the material at high temperature is very important. Thirdly, the comprehensive performance from room temperature to high temperature of the wave-transparent and heat-insulating integrated material needs to be researched. In conclusion, the preparation of the wave-transmitting heat-insulating multifunctional integrated material with excellent high-temperature performance has very important significance.
The invention has the advantages and beneficial effects that:
1. the porous ceramic with extremely high porosity is prepared by a novel in-situ foaming-casting-freeze drying process, and the porosity is as high as 80-96%, so that the purposes of ultra-light weight and ultra-heat insulation are achieved. In addition, the low dielectric constant and dielectric loss can be obtained, and a good wave-transmitting function is realized.
2. According to the invention, the mechanical properties of a high-porosity sample are effectively improved through fiber reinforcement (adding YSZ fibers) and solid solution reinforcement (solid solution of Ho elements), and the high-temperature wave-transparent and heat-insulating integrated material with ultra-light weight, high porosity and high strength is prepared.
3. The method has the advantages of simple process, convenient operation and easy conversion into productivity.
4. The fiber reinforced gamma- (Y) prepared by the invention1-xHox)2Si2O7The porous solid solution has excellent high-temperature comprehensive performance, is expected to become an excellent high-temperature wave-transmitting and heat-insulating multifunctional integrated material, has attractive application prospect in the field of wave-transmitting materials and heat insulation for aerospace aircrafts, and meets important requirements for aerospace development.
Drawings
FIG. 1(a) to FIG. 1(b) show YSZ fiber-reinforced γ - (Y)0.25Ho0.75)2Si2O7Scanning electron micrographs of the porous ceramics. Wherein FIG. 1(a) is a macro-pore micro-topography and FIG. 1(b) is a micro-topography and fiber distribution map of the micro-pores.
FIG. 2 shows YSZ fiber-reinforced gamma- (Y)0.5Ho0.5)2Si2O7XRD energy spectrum of porous ceramic.
FIG. 3(a) -FIG. 3(b) are YSZ fiber reinforced gamma- (Y)0.8Ho0.2)2Si2O7Dielectric property and thermal conductivity of the porous ceramic. Fig. 3(a) is a graph showing the influence of temperature on dielectric properties, and fig. 3(b) is a graph showing the influence of temperature on thermal conductivity.
Detailed Description
In the specific implementation process, yttrium oxide, holmium oxide, silicon oxide powder and YSZ fiber (yttria fully stabilized zirconia fiber) are used as raw materials, firstly ceramic powder mixed slurry with uniformly dispersed YSZ fiber is prepared, and then the slurry is rapidly mixedMechanically stirring and foaming, then injection molding and low-temperature freezing to form a green body, then carrying out vacuum drying, demoulding and oven drying on the green body, and finally preparing the YSZ fiber reinforced gamma- (Y) through high-temperature reaction sintering1-xHox)2Si2O7Porous solid solution wave-transparent heat-insulating integrated material. The preparation process is simple and easy to operate, the cost is low, the synthesized composite material has the characteristics of ultrahigh porosity, low high-temperature dielectric constant, low dielectric loss, low high-temperature thermal conductivity and excellent high-temperature thermal stability, and the industrial production and application prospects are very wide.
The invention is described in further detail below with reference to the figures and examples.
Example 1
In this example, 5g of Y was weighed2O325.0g of Ho2O3And 10.7g of SiO2(molar ratio 0.25: 0.75: 2), and raw materials of 16.3g of YSZ fiber, 0.75g of ammonium citrate and 80g of deionized water, and mixing and stirring for 4 hours to form slurry with uniformly dispersed fiber and ceramic powder. Heating the slurry to 50 ℃, adding 5g of foaming agent sodium dodecyl sulfate according to parts by weight, rapidly and mechanically stirring at 1500rpm for foaming for 25 minutes, then adding 9g of gel gelatin and 1.2g of surfactant polyethylene glycol, continuously and mechanically stirring at 1500rpm for 50 minutes, and then injecting the mixture into a mold; then placing the mold and a sample obtained by injection molding in a freezer at-50 ℃ for freezing for 6 hours, vacuumizing for 36 hours until the vacuum degree is 5Pa, then demolding and drying in an oven at 90 ℃ for 5 hours; finally, high-temperature reaction sintering is carried out in the air at 1600 ℃ for 1 hour to prepare the fiber enhanced gamma- (Y) with excellent comprehensive performance0.25Ho0.75)2Si2O7Porous solid solution wave-transparent heat-insulating integrated material. The fiber reinforced gamma- (Y)1-xHox)2Si2O7In the porous solid solution finished product, the YSZ fiber accounts for 40 wt%.
In this example, YSZ fiber-reinforced γ - (Y)0.25Ho0.75)2Si2O7The porosity of the porous solid solution was 95.5%, the compressive strength was 0.27MPa,the dielectric constant at room temperature is 1.25 to 1.27 (frequency is 7 to 19.5GHz), and the thermal conductivity at room temperature is 0.069W/(m.K). Fiber reinforced gamma- (Y)0.25Ho0.75)2Si2O7The microscopic morphology of the porous solid solution is shown by the SEM photographs of fig. 1(a) and 1(b), and the pore structure of the sample includes: the size distribution of macropores is 35-450 mu m, and the volume proportion of the macropores is 93%; the size of the small holes is 0.5-7.5 mu m, and the small holes account for 7% of the volume of the porous material. It can also be seen that the YSZ fibers are uniformly dispersed and penetrate through the γ - (Y)0.25Ho0.75)2Si2O7The porous framework of the matrix can improve the mechanical property of the material through the bridging effect of the fibers.
Example 2
In this example, 15.0Y was weighed out separately2O325.1g of Ho2O3And 16.0g of SiO2(molar ratio is 0.5: 0.5: 2), and YSZ fiber 3g, polyimide 2.5g and deionized water 60g as raw materials, mixing and stirring for 2 hours to form slurry with uniformly dispersed fiber and ceramic powder. Heating the slurry to 35 ℃, adding 2g of foaming agent sodium dodecyl sulfate according to parts by weight, rapidly and mechanically stirring at 1200rpm for foaming for 10 minutes, then adding 3.5g of gel gelatin and 3g of surfactant polyethylene glycol, continuously and mechanically stirring at 1200rpm for 50 minutes, and then injecting the mixture into a mold; then placing the mould and a sample obtained by injection molding in a freezing box at-20 ℃ for freezing for 24 hours, vacuumizing for 12 hours until the vacuum degree is 10Pa, then demolding and drying in an oven at 60 ℃ for 24 hours; finally, high-temperature reaction sintering is carried out in the air at 1500 ℃ for 3 hours to prepare the fiber enhanced gamma- (Y) with excellent comprehensive performance0.5Ho0.5)2Si2O7Porous solid solution wave-transparent heat-insulating integrated material. The fiber reinforced gamma- (Y)1-xHox)2Si2O7In the porous solid solution finished product, the YSZ fiber accounts for 5 wt%.
In this example, YSZ fiber-reinforced γ - (Y)0.5Ho0.5)2Si2O7Porosity of the porous solid solution is 83.1%, compressive strength is 10.9MPa, high temperature thermal cycle: (25 to 1500 ℃ C.) shrinkage ratio<0.59 percent. YSZ fiber reinforced gamma- (Y)0.5Ho0.5)2Si2O7The phase composition of the porous solid solution is shown in the XRD spectrum of figure 2. from figure 2, it can be seen that the sample is composed of gamma- (Y)0.5Ho0.5)2Si2O7The phase and the two phases of yttria-stabilized zirconia are formed without other impurities, which indicates that the two phases can stably coexist.
Example 3
In this example, 21.6g of Y were weighed out separately2O39.0g of Ho2O3And 14.5g of SiO2(molar ratio 0.8: 0.2: 2), and YSZ fiber 6.7g, citric acid 2g, and deionized water 70g as raw materials, and mixing and stirring for 3 hours to form slurry with uniformly dispersed fiber and ceramic powder. Heating the slurry to 42 ℃, adding 3.5g of foaming agent sodium dodecyl sulfate according to parts by weight, rapidly and mechanically stirring at 2000rpm for foaming for 15 minutes, then adding 7g of gel gelatin and 5g of surfactant polyethylene glycol, continuously and mechanically stirring at 2000rpm for 40 minutes, and then injecting into a mold; then placing the mould and the sample obtained by injection molding in a freezer at-35 ℃ for freezing for 12 hours, vacuumizing for 24 hours until the vacuum degree is 15Pa, then demolding and drying in an oven at 75 ℃ for 12 hours; finally, high-temperature reaction sintering is carried out for 2 hours at 1550 ℃ in the air, and the fiber enhanced gamma- (Y) with excellent comprehensive performance is prepared0.8Ho0.2)2Si2O7Porous solid solution wave-transparent heat-insulating integrated material. The fiber reinforced gamma- (Y)1- xHox)2Si2O7In the porous solid solution finished product, the YSZ fiber accounts for 15 wt%.
In this example, YSZ fiber reinforced gamma- (Y)0.8Ho0.2)2Si2O7The porous solid solution had a porosity of 93.1%, a compressive strength of 1.23MPa, and a density of 0.32g/cm3A room temperature dielectric constant of 1.30 to 1.32 and a room temperature dielectric loss of (1.2 to 1.9) × 10-3(frequency 7-19.5 GHz) and room-temperature thermal conductivity of 0.079W/(m.K). However, the high temperature performance of the material is more important, from the high temperature dielectric constant of FIG. 3(a)In the graph, it can be seen that the dielectric constant increases from 1.30 to 1.39 at room temperature and the dielectric loss increases from 1.20X 10 at room temperature to 1000 deg.C-3Increased to 3.5 × 10-2(frequency 7-19.5 GHz). Meanwhile, from the high temperature thermal conductivity graph of fig. 3(b), it can be seen that the composite material still maintains very low thermal conductivity at high temperature: it is only 0.209W/(mK) at 1200 ℃. And also has excellent high-temperature thermal stability and high-temperature thermal cycle (25-1550 ℃) shrinkage<0.7%。
The results of the examples show that the YSZ fiber enhanced gamma- (Y) with ultrahigh porosity, high strength, low high-temperature dielectric constant, low dielectric loss, low high-temperature thermal conductivity and excellent high-temperature thermal stability is prepared by adopting a novel foaming-injecting-condensing-freeze drying process1-xHox)2Si2O7Porous solid solution wave-transparent heat-insulating integrated material. The preparation process is simple, the operation is convenient, the cost is low, and the production and application prospects are very wide.
Claims (5)
1. High-temperature wave-transmitting and heat-insulating integrated fiber-reinforced gamma- (Y) for aerospace aircraft1-xHox)2Si2O7Porous solid solution, characterized in that it is a fiber-reinforced gamma- (Y)1-xHox)2Si2O7In the porous solid solution finished product, the reinforcing phase YSZ fiber accounts for 5-50 wt%, and the matrix is gamma- (Y)1-xHox)2Si2O7The technical indexes are as follows: a porosity of 80-96%, a high-temperature dielectric constant of 1.2-2.5 at 1000 ℃ and a dielectric loss of 1.0X 10-3~7.5×10-2The high-temperature thermal conductivity at 600-1200 ℃ is 0.1-0.5W/(m.K), and the high-temperature thermal cycle shrinkage at 25-1550 ℃ is less than 1%;
the high-temperature wave-transparent heat-insulating integrated fiber-reinforced gamma- (Y)1-xHox)2Si2O7A preparation method of the porous solid solution, wherein the value range of x is 0<x<1, the added fiber is a zirconia fiber with yttria fully stabilized, and the specific steps are as follows:
1) preparing slurry: according to the qualityIn parts by weight, as Y2O3、Ho2O3And SiO2Molar ratio (1-x): x: 2, taking 35-60 parts of mixed powder, 1-20 parts of YSZ fiber, 0.5-3 parts of dispersing agent and 60-80 parts of deionized water as raw materials, mixing and stirring for 2-4 hours to form slurry with uniformly dispersed fiber and ceramic powder;
2) foaming-pouring coagulation: heating the slurry to 35-50 ℃, adding 1-6 parts of foaming agent by weight, quickly and mechanically stirring for foaming for 10-25 minutes, adding 3-9 parts of gelatin as a gelling agent and 1-5 parts of polyethylene glycol as a surfactant, continuously and quickly and mechanically stirring for 15-50 minutes, and then injecting into a mold;
3) freeze drying-oven drying: placing the mold and a sample obtained by injection molding in a freezer at-20 to-50 ℃ for freezing for 5-24 hours, then vacuumizing for 12-36 hours until the vacuum degree is 1-20 Pa, then demolding and drying in an oven at 60-90 ℃ for 5-24 hours;
4) and (3) high-temperature sintering: high-temperature reaction sintering is carried out for 1-3 hours at 1450-1600 ℃ in the air, and the fiber reinforced gamma- (Y) is prepared1-xHox)2Si2O7A porous solid solution.
2. The high temperature wave-transparent and heat-insulating integrated fiber-reinforced gamma- (Y) for aerospace and aviation aircraft according to claim 11- xHox)2Si2O7The porous solid solution is characterized in that the dispersant is polyacetimide, ammonium citrate or citric acid, and the foaming agent is sodium dodecyl sulfate or sodium dodecyl sulfate.
3. The high temperature wave-transparent and heat-insulating integrated fiber-reinforced gamma- (Y) for aerospace and aviation aircraft according to claim 11- xHox)2Si2O7The porous solid solution is characterized in that in the step 2), the rotating speed range of a stirrer for rapid mechanical stirring is 1000-2500 rpm.
4. The high temperature wave-transparent barrier for an aerospace vehicle according to claim 1Thermally integrated fiber reinforced gamma- (Y)1- xHox)2Si2O7Porous solid solution, characterized in that it is a fiber-reinforced gamma- (Y)1-xHox)2Si2O7In the final porous solid solution product, the porous composition comprises: the size distribution of macropores is 35-450 mu m, and the volume proportion of the macropores is 70-95%; the size of the small holes is 0.5-7.5 mu m, and the volume proportion of the small holes in the porous material is 30-5%.
5. The high temperature wave-transparent and heat-insulating integrated fiber-reinforced gamma- (Y) for aerospace and aviation aircraft according to claim 11- xHox)2Si2O7Porous solid solution, characterized in that it is a fiber-reinforced gamma- (Y)1-xHox)2Si2O7In the porous solid solution finished product, the YSZ fiber accounts for 10-25 wt%.
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