Integrated preparation method of gradient low dielectric high-temperature-resistant wave-transparent material

Abstract

The application relates to a gradient low-dielectric high-temperature-resistant wave-transparent material integrated preparation method, which comprises the following steps: preparing a porous quartz fiber ceramic blank; preparing a plurality of porous quartz fiber ceramic bases by using a plurality of silica sol solutions through the porous quartz fiber ceramic blank; the silica sol solutions comprise a first silica sol solution to an n-th silica sol solution; the porous quartz fiber ceramic bases comprise a first porous quartz fiber ceramic base to an n-th porous quartz fiber ceramic base; the first porous quartz fiber ceramic base to the n-th porous quartz fiber ceramic base are respectively processed according to corresponding preset sizes to obtain a first porous quartz fiber ceramic sub-piece to an n-th porous quartz fiber ceramic sub-piece; the first porous quartz fiber ceramic sub-piece to the n-th porous quartz fiber ceramic sub-piece are attached, fixed and sintered according to a preset order; and the gradient low-dielectric high-temperature-resistant wave-transparent material has high strength, low dielectric constant, low dielectric loss and wide-band wave-transparency.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of high-temperature-resistant wave-transparent materials, in particular to the technical field of a gradient low-dielectric high-temperature-resistant wave-transparent material integrated preparation method. BACKGROUND

[0002] High-temperature-resistant wave-transparent materials are widely used in the field of aerospace, and are used in a large number of key components of radar guidance systems such as radomes, which protect the internal seeker from external high-speed aerodynamic heat ablation and effectively transmit electromagnetic waves, and have the functions of heat protection, bearing and wave transmission in one. With the continuous improvement of combat requirements such as equipment flight speed, precision guidance and attack and defense confrontation, the development of ceramic radomes with high-temperature resistance and wide-band wave transmission performance has become one of the research hotspots at home and abroad.

[0003] The dielectric constant and dielectric loss of the conventional high-temperature-resistant wave-transparent material are mainly determined by the composition of the raw material, so it is difficult to make the dielectric constant and dielectric loss very low, and it is also impossible to achieve wide-band wave transmission.

[0004] Therefore, how to prepare a high-temperature-resistant wave-transparent material with high strength, low dielectric constant, low dielectric loss and wide-band wave transmission performance has become a difficult problem to be solved in the field. SUMMARY

[0005] In order to solve the above technical problems, the purpose of the present application is to provide a gradient low-dielectric high-temperature-resistant wave-transparent material integrated preparation method, which realizes high strength, low dielectric constant, low dielectric loss and wide-band wave transmission performance.

[0006] The present application provides a gradient low-dielectric high-temperature-resistant wave-transparent material integrated preparation method, comprising the following steps: preparing a porous quartz fiber ceramic body;

[0007] Preparation of a plurality of porous quartz fiber ceramic substrates by using a plurality of silica sol solutions on the porous quartz fiber ceramic body;

[0008] The silica sol solution includes a first silica sol solution to an n-th silica sol solution;

[0009] The porous quartz fiber ceramic substrate includes a first porous quartz fiber ceramic substrate to an n-th porous quartz fiber ceramic substrate;

[0010] The first porous quartz fiber ceramic substrate is prepared by impregnating, drying and sintering the porous quartz fiber ceramic body with the first silica sol solution;

[0011] The second porous quartz fiber ceramic substrate to the n-th porous quartz fiber ceramic substrate is prepared by respectively impregnating, drying and sintering the porous quartz fiber ceramic body with the second silica sol to the n-th silica sol;

[0012] The first porous quartz fiber ceramic base to the n-th porous quartz fiber ceramic base is respectively processed according to corresponding preset sizes, so that the first porous quartz fiber ceramic sub-piece to the n-th porous quartz fiber ceramic sub-piece is obtained;

[0013] The surfaces of the first porous quartz fiber ceramic sub-piece to the n-1-th porous quartz fiber ceramic sub-piece are attached with ceramic slurry; the ceramic slurry comprises quartz powder, a sintering aid and alcohol in a mass ratio of (9-11):(1-5):(95-105); the sintering aid comprises boron oxide;

[0014] The first porous quartz fiber ceramic sub-piece to the n-th porous quartz fiber ceramic sub-piece is attached, fixed and sintered according to a preset order, so that the gradient low-dielectric high-temperature-resistant wave-transparent material is obtained; the sintering temperature is 1000-1100 DEG C.

[0015] Compared with the prior art, the present application has the following beneficial effects: the porous quartz fiber ceramic base comprises the first porous quartz fiber ceramic base to the n-th porous quartz fiber ceramic base, so that porous quartz fiber ceramic bases with different porosities are prepared, the densities of the porous quartz fiber ceramic bases are different, and porous quartz fiber ceramic bases with different dielectric losses are prepared;

[0016] The silicon sol solution comprises the first silicon sol solution to the n-th silicon sol solution, so that silicon sols with different concentrations are prepared;

[0017] The first silicon sol to the n-th silicon sol is used for respectively impregnating, drying and sintering the porous quartz fiber ceramic base body, so that the second porous quartz fiber ceramic base body to the n-th porous quartz fiber ceramic base body is prepared, more kinds of porous quartz fiber ceramic sub-pieces with different dielectric constants are prepared, and the dielectric constants of the various porous quartz fiber ceramic sub-pieces are very low;

[0018] The porous quartz fiber ceramic base body is impregnated and dried by the silicon sol, and then sintered at a low sintering temperature, so that the glue is removed, the porous quartz fiber ceramic base has a certain strength, the porous quartz fiber ceramic sub-piece can be processed and prepared, the prepared porous quartz fiber ceramic sub-piece has high activity, the first porous quartz fiber ceramic sub-piece to the n-th porous quartz fiber ceramic sub-piece is attached, fixed and sintered according to a preset order, the bonding strength of the various porous quartz fiber ceramic sub-pieces is high, the gradient low-dielectric high-temperature-resistant wave-transparent material is integrally prepared, and the strength of the gradient low-dielectric high-temperature-resistant wave-transparent material is high;

[0019] Attaching ceramic slurry to the surface of the first porous quartz fiber ceramic sub-piece to the n-1 porous quartz fiber ceramic sub-piece; the ceramic slurry comprises quartz powder, sintering aid, alcohol in a mass ratio of (9-11):(1-5):(95-105); the sintering aid comprises boron oxide and the like, so as to realize chemical reaction between the ceramic slurry and the porous quartz fiber ceramic sub-piece in the subsequent sintering process, form boron-silicon compounds, and improve the high-temperature resistance and strength of the gradient low-dielectric high-temperature resistant wave-transparent material.

[0020] The prepared gradient low-dielectric high-temperature resistant wave-transparent material has high strength, low dielectric constant, low dielectric loss, and wide-band wave-transparent performance.

[0021] Further, when n=3, the silica sol solution comprises a first silica sol solution, a second silica sol solution, and a third silica sol solution.

[0022] The first silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, and the silica sol concentration of the first silica sol solution is 10-30% and the pH is 4-6.

[0023] The second silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, and the silica sol concentration of the second silica sol solution is 31-41% and the pH is 4-6.

[0024] The third silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, and the silica sol concentration of the third silica sol solution is 41-55% and the pH is 4-6.

[0025] The beneficial effects of the above step are that silica sols with different concentrations are prepared.

[0026] Further, the preparation process of the porous quartz fiber ceramic body comprises the following steps:

[0027] The quartz fiber and the alumina fiber are respectively sheared to obtain short fibers 1 and short fibers 2.

[0028] The short fibers 1, the short fibers 2, deionized water, and additives are mixed and stirred according to a proportion of (50-90):(10-40):(100-200):(10-15), and the stirring time is 60-120 min, to obtain a quartz fiber ceramic slurry.

[0029] The quartz fiber ceramic slurry is added to a forming mold, and then suction filtration is performed.

[0030] Then, after drying, high-temperature sintering is performed to obtain a porous quartz fiber ceramic body.

[0031] Further, the additive comprises boron oxide; the aspect ratio of the short fiber 1 is (100-1000):1, and the aspect ratio of the short fiber 2 is (100-500):1.

[0032] The beneficial effects of the above step are that, by the aspect ratio of the short fiber 1 being (100-1000):1, the aspect ratio of the short fiber 2 being (100-500):1, and the mixing of the short fiber 1 and the short fiber 2 in a ratio of (50-90):(10-40), a porous quartz fiber ceramic body with different porosities is obtained; by the mixing of the short fiber 1, the short fiber 2, the deionized water, and the additive in a ratio, and the additive comprising boron oxide, the boron-silicon compound is generated by the reaction of the boron oxide and the quartz fiber at the cross of the fibers in the porous quartz fiber ceramic body, so that the strength of the quartz fiber ceramic body after forming is high, and the problem of reducing the porosity by filling some materials into the porous quartz fiber ceramic body is avoided; so that the porosity in the porous quartz fiber ceramic body is mainly obtained by mixing the short fiber 1 and the short fiber 2 in a ratio of (50-90), so that the porosity in the porous quartz fiber ceramic body is controllable and adjustable.

[0033] Further, the porous quartz fiber ceramic matrix comprises a first porous quartz fiber ceramic matrix, a second porous quartz fiber ceramic matrix, and a third porous quartz fiber ceramic matrix.

[0034] The porous quartz fiber ceramic body is placed in a vacuum container for vacuum treatment, the first silica sol solution is siphoned into the vacuum container through the opening of the feeding port at the bottom of the vacuum container, and the vacuum treatment is continued for 30-60 min after the feeding port at the bottom of the vacuum container is closed; the porous quartz fiber ceramic body after immersion is heated together with the container and the first silica sol solution, and the first silica sol solution is gelled; the gelled porous quartz fiber ceramic body is dried at a drying temperature of (100-150) ℃, and then high-temperature calcination is performed at a calcination temperature of (600-800) ℃, to obtain the first porous quartz fiber ceramic matrix; the heating and gelling temperature of the first silica sol solution is (80-100) ℃;

[0035] The porous quartz fiber ceramic body is placed in a vacuum container for vacuum treatment, the second silica sol solution is siphoned into the vacuum container through the opening of the feeding port at the bottom of the vacuum container, and the vacuum treatment is continued for 30-60 min after the feeding port at the bottom of the vacuum container is closed; the porous quartz fiber ceramic body after immersion is heated together with the container and the second silica sol solution, and the second silica sol solution is gelled; the gelled porous quartz fiber ceramic body is dried at a drying temperature of (100-150) ℃, and then high-temperature calcination is performed at a calcination temperature of (600-800) ℃, to obtain the second porous quartz fiber ceramic matrix;

[0036] The second silica sol solution heating gel temperature is (80-100) °C;

[0037] The porous quartz fiber ceramic body is placed in a vacuum container for vacuum treatment, the third silica sol solution is siphoned into the vacuum container through the opening of the feeding port at the bottom of the vacuum container, and the feeding port at the bottom of the vacuum container is closed and the vacuum is maintained for 30-60 min. The impregnated porous quartz fiber ceramic body is heated together with the container and the third silica sol solution, and the third silica sol solution is gelled. The gelled porous quartz fiber ceramic body is dried at a drying temperature of (100-150) °C, and then high-temperature calcination is performed at a calcination temperature of (600-800) °C, to obtain a third porous quartz fiber ceramic matrix.

[0038] The third silica sol solution heating gel temperature is (80-100) °C.

[0039] The above step has the beneficial effect of uniformly impregnating the silica sol solution inside the porous quartz fiber ceramic body, obtaining a porous quartz fiber ceramic matrix. By drying the gelled porous quartz fiber ceramic body at a drying temperature of (100-150) °C, and then high-temperature calcination at a calcination temperature of (600-800) °C, the porous quartz fiber ceramic matrix has a certain strength and can be cut, and the internal organic matter has been volatilized, but the internal chemical activity is beneficial to the subsequent overall sintering, and the adjacent porous quartz fiber ceramic sub-components have high assembly strength.

[0040] Further, the first porous quartz fiber ceramic matrix, the third porous quartz fiber ceramic matrix, and the third porous quartz fiber ceramic matrix are respectively machined according to the corresponding preset dimensions to obtain a first porous quartz fiber ceramic sub-component, a second porous quartz fiber ceramic sub-component, and a third porous quartz fiber ceramic sub-component.

[0041] The first porous quartz fiber ceramic sub-component has a thickness of 5-10 mm and a dielectric constant of 1.3-1.5; the second porous quartz fiber ceramic sub-component has a thickness of 30-40 mm and a dielectric constant of 1.5-1.6; and the third porous quartz fiber ceramic sub-component has a thickness of 10-20 mm and a dielectric constant of 1.8-1.9.

[0042] Preferably, the dielectric loss of the first porous quartz fiber ceramic sub-component, the second porous quartz fiber ceramic sub-component, and the third porous quartz fiber ceramic sub-component is (1-5) × 10 -3

[0043] Further, the porous quartz fiber ceramic body includes a first porous quartz fiber ceramic body, a second porous quartz fiber ceramic body, and a third porous quartz fiber ceramic body.

[0044] The ratio of short fiber 1, short fiber 2, deionized water, and additive in the first porous quartz fiber ceramic body is (70-90):(10-20):(100-200):(10-15);

[0045] The density of the first porous quartz fiber ceramic body is 0.297-0.505 g / cm 3 ;

[0046] The ratio of short fiber 1, short fiber 2, deionized water, and additive in the second porous quartz fiber ceramic body is (60-80):(20-30):(100-200):(10-15);

[0047] The density of the second porous quartz fiber ceramic body is 0.595-0.65 g / cm 3 ;

[0048] The ratio of short fiber 1, short fiber 2, deionized water, and additive in the third porous quartz fiber ceramic body is (50-70):(30-40):(100-200):(10-15);

[0049] The density of the third porous quartz fiber ceramic body is 0.81-0.95 g / cm 3 ;

[0050] Preferably, the dielectric loss of the first porous quartz fiber ceramic body, the second porous quartz fiber ceramic body, and the third porous quartz fiber ceramic body is (1-3)×10 -3 .

[0051] The beneficial effects of the above step are that by mixing short fiber 1 and short fiber 2 with different mass ratios and adding additives, a porous quartz fiber ceramic body with a preset porosity is prepared, thereby obtaining a preset dielectric constant, and by combining different dielectric constants and the thickness of the porous quartz fiber ceramic body with filling different concentrations of silica sol, a low dielectric loss of less than (1-5)×10 -3 is achieved, thereby realizing that the gradient low-dielectric high-temperature-resistant wave-transparent material has low dielectric constant, low dielectric loss, and wide-band wave-transparent performance.

[0052] Further, the first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece, and the third porous quartz fiber ceramic sub-piece are arranged horizontally, and then the third porous quartz fiber ceramic sub-piece, the first porous quartz fiber ceramic sub-piece, and the second porous quartz fiber ceramic sub-piece are sequentially attached, connected, and fixed, and then sintered to obtain the gradient low-dielectric high-temperature-resistant wave-transparent material.

[0053] The beneficial effect of the above step is that the porous quartz fiber ceramic subpieces are arranged horizontally, the dielectric constant of the first porous quartz fiber ceramic subpiece in the middle is the lowest, the dielectric constant of the second and third porous quartz fiber ceramic subpieces on the two sides is relatively high, and the thickness of the first porous quartz fiber ceramic subpiece is the lowest, thereby realizing wide-band wave transmission while having low dielectric loss.

[0054] Further, when n=4, the silica sol solution includes a first silica sol solution, a second silica sol solution, a third silica sol solution, and a fourth silica sol solution.

[0055] The first silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, the silica sol concentration of the first silica sol solution is 0-20%, and the pH is 4-6.

[0056] The second silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, the silica sol concentration of the second silica sol solution is 21-35%, and the pH is 4-6.

[0057] The third silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, the silica sol concentration of the third silica sol solution is 36-45%, and the pH is 4-6.

[0058] The fourth silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, the silica sol concentration of the fourth silica sol solution is 41-55%, and the pH is 4-6.

[0059] And / or

[0060] The porous quartz fiber ceramic body includes a first porous quartz fiber ceramic body, a second porous quartz fiber ceramic body, a third porous quartz fiber ceramic body, and a fourth porous quartz fiber ceramic body.

[0061] The ratio of short fiber 1, short fiber 2, deionized water, and additive in the first porous quartz fiber ceramic body is (80-90):(10-15):(100-200):(10-15).

[0062] The density of the first porous quartz fiber ceramic body is 0.27-0.45 g / cm 3 ;

[0063] The ratio of short fiber 1, short fiber 2, deionized water, and additive in the second porous quartz fiber ceramic body is (70-80):(15-25):(100-200):(10-15).

[0064] The density of the second porous quartz fiber ceramic body is 0.45-0.65 g / cm 3;

[0065] The ratio of short fiber 1, short fiber 2, deionized water, and additive in the third porous quartz fiber ceramic body is (60-70):(20-30):(100-200):(10-15);

[0066] The density of the third porous quartz fiber ceramic body is 0.7-0.9g / cm 3 ;

[0067] The ratio of short fiber 1, short fiber 2, deionized water, and additive in the fourth porous quartz fiber ceramic body is (50-60):(30-40):(100-200):(10-15);

[0068] The density of the fourth porous quartz fiber ceramic body is 0.85-0.95g / cm 3 ;

[0069] Preferably, the dielectric loss of the first porous quartz fiber ceramic body, the second porous quartz fiber ceramic body, the third porous quartz fiber ceramic body, and the fourth porous quartz fiber ceramic body is (1-3) x 10 -3 ;

[0070] Preferably, the dielectric loss of the first porous quartz fiber ceramic body, the second porous quartz fiber ceramic body, the third porous quartz fiber ceramic body, and the fourth porous quartz fiber ceramic body is (1-5) x 10 -3 .

[0071] The beneficial effects of the above step are that four porous quartz fiber ceramic bodies with different densities are prepared according to a predetermined plan, so as to prepare porous quartz fiber ceramic bodies with different dielectric constants; and different thicknesses of porous quartz fiber ceramic bodies are impregnated with silicon sol solutions with different concentrations, so as to realize that the overall gradient low-dielectric high-temperature resistant wave-transparent material has wide-band wave transmission and reduced dielectric loss.

[0072] Further, the first porous quartz fiber ceramic body, the third porous quartz fiber ceramic body, the third porous quartz fiber ceramic body, and the fourth porous quartz fiber ceramic body are respectively processed according to corresponding predetermined sizes, to obtain the first porous quartz fiber ceramic part, the second porous quartz fiber ceramic part, the third porous quartz fiber ceramic part, and the fourth porous quartz fiber ceramic part;

[0073] The first porous quartz fiber ceramic sub-piece has a thickness of 45-50 mm and a dielectric constant of 1.3-1.4; the second porous quartz fiber ceramic sub-piece has a thickness of 35-40 mm and a dielectric constant of 1.5-1.6; the third porous quartz fiber ceramic sub-piece has a thickness of 25-30 mm and a dielectric constant of 1.7-1.8; and the fourth porous quartz fiber ceramic sub-piece has a thickness of 40-45 mm and a dielectric constant of 1.8-1.9.

[0074] The first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece and the third porous quartz fiber ceramic sub-piece are arranged in a curved manner, then the fourth porous quartz fiber ceramic sub-piece, the third porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece and the first porous quartz fiber ceramic sub-piece are sequentially connected and fixed, and then sintering is performed to obtain the gradient low-dielectric high-temperature-resistant wave-transparent material.

[0075] The beneficial effects of the above step are that the dielectric constants of the first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece, the third porous quartz fiber ceramic sub-piece and the fourth porous quartz fiber ceramic sub-piece connected in sequence decrease in turn, but the thickness decreases first and then decreases, which more effectively improves the wide-band wave-transparent performance of the gradient low-dielectric high-temperature-resistant wave-transparent material, and at the same time avoids the problem of rising dielectric loss caused by increasing the number of layers.

[0076] The first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece and the third porous quartz fiber ceramic sub-piece are arranged in a curved manner, which is further conducive to improving the wide-band wave-transparent performance and at the same time realizing effective wave focusing effect, thereby improving the wave-transparent intensity and avoiding the problem of reduced wave-transparent intensity caused by increasing the number of layers; and at the same time, the strength of the gradient low-dielectric high-temperature-resistant wave-transparent material is increased. DETAILED DESCRIPTION

[0077] In order to better understand the technical solutions of the present application, the present application will be further described below in combination with specific embodiments.

[0078] Embodiment one

[0079] The embodiment provides an integrated preparation method of a gradient low-dielectric high-temperature-resistant wave-transparent material, which comprises the following steps: preparing a porous quartz fiber ceramic body;

[0080] The preparation process of the porous quartz fiber ceramic body comprises the following steps:

[0081] The quartz fiber and the alumina fiber are respectively sheared to obtain short fibers 1 and short fibers 2;

[0082] Short fiber 1, short fiber 2, deionized water, additives are mixed, stirred and dispersed in proportion of 70:25:150:13, the stirring time is 90 min, and a quartz fiber ceramic slurry is obtained;

[0083] The quartz fiber ceramic slurry is added into a forming mold, and then suction filtration forming is performed; then, after drying, high-temperature sintering is performed, and a porous quartz fiber ceramic body is obtained.

[0084] The additives include boron oxide; the aspect ratio of the short fiber 1 is 550:1, and the aspect ratio of the short fiber 2 is 300:1.

[0085] The porous quartz fiber ceramic body includes a first porous quartz fiber ceramic body, a second porous quartz fiber ceramic body and a third porous quartz fiber ceramic body.

[0086] The proportion of the short fiber 1, the short fiber 2, deionized water and additives in the first porous quartz fiber ceramic body is 80:15:150:13.

[0087] The density of the first porous quartz fiber ceramic body is 0.4 g / cm 3 ;

[0088] The proportion of the short fiber 1, the short fiber 2, deionized water and additives in the second porous quartz fiber ceramic body is 70:25:150:13.

[0089] The density of the second porous quartz fiber ceramic body is 0.62 g / cm 3 ;

[0090] The proportion of the short fiber 1, the short fiber 2, deionized water and additives in the third porous quartz fiber ceramic body is 60:35:150:13.

[0091] The density of the third porous quartz fiber ceramic body is 0.88 g / cm 3 ;

[0092] Preferably, the dielectric loss of the first porous quartz fiber ceramic body, the second porous quartz fiber ceramic body and the third porous quartz fiber ceramic body is (1.8-2.2)×10 -3 ;

[0093] A plurality of porous quartz fiber ceramic bodies are prepared by using a plurality of silica sol solutions through the porous quartz fiber ceramic body.

[0094] The silica sol solutions include a first silica sol solution to a third silica sol solution.

[0095] The porous quartz fiber ceramic bodies include a first porous quartz fiber ceramic body to an n-th porous quartz fiber ceramic body.

[0096] The porous quartz fiber ceramic base body is impregnated with the first silica sol solution, dried, and sintered to prepare a first porous quartz fiber ceramic base body;

[0097] The porous quartz fiber ceramic base body is impregnated with the second silica sol to the third silica sol, dried, and sintered to prepare a second porous quartz fiber ceramic base body to a third porous quartz fiber ceramic base body;

[0098] The silica sol solution includes a first silica sol solution, a second silica sol solution, and a third silica sol solution;

[0099] The first silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, and the silica sol concentration of the first silica sol solution is 20% and the pH is 5;

[0100] The second silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, and the silica sol concentration of the second silica sol solution is 36% and the pH is 5;

[0101] The third silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, and the silica sol concentration of the third silica sol solution is 48% and the pH is 5;

[0102] The first porous quartz fiber ceramic base body to the third porous quartz fiber ceramic base body are processed according to corresponding preset sizes to obtain a first porous quartz fiber ceramic sub-piece to a third porous quartz fiber ceramic sub-piece;

[0103] The porous quartz fiber ceramic base body includes a first porous quartz fiber ceramic base body, a second porous quartz fiber ceramic base body, and a third porous quartz fiber ceramic base body;

[0104] The porous quartz fiber ceramic base body is placed in a vacuum container for vacuumizing treatment, the first silica sol solution is siphoned into the vacuum container through the inlet at the bottom of the vacuum container, and the inlet is closed after 45 minutes of vacuumizing; the impregnated porous quartz fiber ceramic base body is heated together with the container and the first silica sol solution, and the first silica sol solution is gelled; the gelled porous quartz fiber ceramic base body is dried at a temperature of 125°C, and then high-temperature calcined at a temperature of 700°C to obtain a first porous quartz fiber ceramic base body; the gelling temperature of the first silica sol solution is 90°C;

[0105] The porous quartz fiber ceramic body is placed in a vacuum container for vacuum treatment, the second silica sol solution is siphoned into the vacuum container by opening the feed port at the bottom of the vacuum container, and the vacuum is maintained for 45 minutes after the feed port at the bottom of the vacuum container is closed; the impregnated porous quartz fiber ceramic body is heated together with the container and the second silica sol solution, and the second silica sol solution is gelled; the gelled porous quartz fiber ceramic body is dried at a drying temperature of 125 DEG C, and then high-temperature calcination is carried out at a calcination temperature of 700 DEG C, and then high-temperature calcination is carried out, to obtain a second porous quartz fiber ceramic matrix;

[0106] The heating and gelling temperature of the second silica sol solution is 90 DEG C;

[0107] The porous quartz fiber ceramic body is placed in a vacuum container for vacuum treatment, the third silica sol solution is siphoned into the vacuum container by opening the feed port at the bottom of the vacuum container, and the vacuum is maintained for 45 minutes after the feed port at the bottom of the vacuum container is closed; the impregnated porous quartz fiber ceramic body is heated together with the container and the third silica sol solution, and the third silica sol solution is gelled; the gelled porous quartz fiber ceramic body is dried at a drying temperature of 125 DEG C, and then high-temperature calcination is carried out at a calcination temperature of 700 DEG C, and then high-temperature calcination is carried out, to obtain a third porous quartz fiber ceramic matrix;

[0108] The heating and gelling temperature of the third silica sol solution is 90 DEG C.

[0109] The first porous quartz fiber ceramic matrix, the third porous quartz fiber ceramic matrix, and the third porous quartz fiber ceramic matrix are respectively processed according to the corresponding preset size to obtain a first porous quartz fiber ceramic sub-piece, a second porous quartz fiber ceramic sub-piece, and a third porous quartz fiber ceramic sub-piece;

[0110] The thickness of the first porous quartz fiber ceramic sub-piece is 8 mm, and the dielectric constant is 1.4; the thickness of the second porous quartz fiber ceramic sub-piece is 35 mm, and the dielectric constant is 1.55; the thickness of the third porous quartz fiber ceramic sub-piece is 15 mm, and the dielectric constant is 1.85;

[0111] The dielectric loss of the first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece, and the third porous quartz fiber ceramic sub-piece is (2.8-3.2) x 10 -3 .

[0112] The surfaces of the first porous quartz fiber ceramic sub-piece to the second porous quartz fiber ceramic sub-piece are attached with a ceramic slurry; the ceramic slurry comprises quartz powder, sintering aid, and alcohol in a mass ratio of 10:3:100; the sintering aid comprises boron oxide;

[0113] The first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece, and the third porous quartz fiber ceramic sub-piece are arranged horizontally, and then the third porous quartz fiber ceramic sub-piece, the first porous quartz fiber ceramic sub-piece, and the second porous quartz fiber ceramic sub-piece are sequentially connected and fixed, and then sintering is performed to obtain the gradient low-dielectric high-temperature-resistant wave-transparent material.

[0114] The first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece, and the third porous quartz fiber ceramic sub-piece are arranged horizontally, and then the third porous quartz fiber ceramic sub-piece, the first porous quartz fiber ceramic sub-piece, and the second porous quartz fiber ceramic sub-piece are sequentially connected and fixed, and then sintering is performed to obtain the gradient low-dielectric high-temperature-resistant wave-transparent material.

[0115] Embodiment Two

[0116] The same features of the embodiment as those of Embodiment One will not be described again. The embodiment provides a gradient low-dielectric high-temperature-resistant wave-transparent material integrated preparation method, which comprises the following steps: the silica sol solution comprises a first silica sol solution, a second silica sol solution, a third silica sol solution, and a fourth silica sol solution.

[0117] The first silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, the silica sol concentration of the first silica sol solution is 18%, and the pH is 5.8.

[0118] The second silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, the silica sol concentration of the second silica sol solution is 33%, and the pH is 5.8.

[0119] The third silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, the silica sol concentration of the third silica sol solution is 43%, and the pH is 5.8.

[0120] The fourth silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, the silica sol concentration of the third silica sol solution is 53%, and the pH is 4.8.

[0121] The porous quartz fiber ceramic body comprises a first porous quartz fiber ceramic body, a second porous quartz fiber ceramic body, a third porous quartz fiber ceramic body, and a fourth porous quartz fiber ceramic body.

[0122] The ratio of the short fiber 1, the short fiber 2, deionized water, and the additive in the first porous quartz fiber ceramic body is 88:13:180:14.

[0123] The density of the first porous quartz fiber ceramic body is 0.43 g / cm 3 ;

[0124] The ratio of short fiber 1, short fiber 2, deionized water, and additive in the second porous quartz fiber ceramic body is 73:23:180:13;

[0125] The density of the second porous quartz fiber ceramic body is 0.55g / cm 3 ;

[0126] The ratio of short fiber 1, short fiber 2, deionized water, and additive in the third porous quartz fiber ceramic body is 63:28:180:13;

[0127] The density of the third porous quartz fiber ceramic body is 0.8g / cm 3 ;

[0128] The ratio of short fiber 1, short fiber 2, deionized water, and additive in the fourth porous quartz fiber ceramic body is 53:38:180:13;

[0129] The density of the fourth porous quartz fiber ceramic body is 0.93g / cm 3 ;

[0130] The dielectric loss of the first porous quartz fiber ceramic body, the second porous quartz fiber ceramic body, the third porous quartz fiber ceramic body, and the fourth porous quartz fiber ceramic body is (1.8-2.2) x 10 -3 ;

[0131] The dielectric loss of the first porous quartz fiber ceramic body, the second porous quartz fiber ceramic body, the third porous quartz fiber ceramic body, and the fourth porous quartz fiber ceramic body is (1.8-2.2) x 10 -3 .

[0132] The first porous quartz fiber ceramic body, the third porous quartz fiber ceramic body, the third porous quartz fiber ceramic body, and the fourth porous quartz fiber ceramic body are respectively processed according to the corresponding preset size to obtain the first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece, the third porous quartz fiber ceramic sub-piece, and the fourth porous quartz fiber ceramic sub-piece;

[0133] The thickness of the first porous quartz fiber ceramic sub-piece is 46mm, and the dielectric constant is 1.32; the thickness of the second porous quartz fiber ceramic sub-piece is 36mm, and the dielectric constant is 1.52; the thickness of the third porous quartz fiber ceramic sub-piece is 26mm, and the dielectric constant is 1.72; the thickness of the fourth porous quartz fiber ceramic sub-piece is 41mm, and the dielectric constant is 1.82;

[0134] The first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece and the third porous quartz fiber ceramic sub-piece are arranged in a curved manner, then the fourth porous quartz fiber ceramic sub-piece, the third porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece and the first porous quartz fiber ceramic sub-piece are sequentially connected and fixed, and then sintering is performed to obtain the gradient low-dielectric high-temperature-resistant wave-transparent material.

[0135] The above description is merely preferred embodiments of the present application and a description of the technical principles of the application. It should be understood by those skilled in the art that the scope of the application disclosed in the present application is not limited to the technical solutions formed by the specific combinations of the above technical features, and should also cover other technical solutions formed by any combinations of the above technical features or equivalent features without departing from the inventive concept. For example, the above features are replaced with the technical features disclosed in the present application (but not limited to) having similar functions to form technical solutions.

Claims

1. A method for integrated preparation of a gradient low-dielectric high-temperature-resistant wave-transparent material, characterized in that, The method comprises the following steps: preparing a porous quartz fiber ceramic body; preparing a plurality of porous quartz fiber ceramic substrates through the porous quartz fiber ceramic body using a plurality of silica sol solutions; the silica sol solutions comprise a first silica sol solution to an n-th silica sol solution; the porous quartz fiber ceramic substrates comprise a first porous quartz fiber ceramic substrate to an n-th porous quartz fiber ceramic substrate; the first porous quartz fiber ceramic substrate is prepared by impregnating, drying and sintering the porous quartz fiber ceramic body using the first silica sol solution; the second porous quartz fiber ceramic substrate to the n-th porous quartz fiber ceramic substrate are respectively prepared by impregnating, drying and sintering the porous quartz fiber ceramic body using the second silica sol to the n-th silica sol; the first porous quartz fiber ceramic substrate to the n-th porous quartz fiber ceramic substrate are respectively processed according to corresponding preset sizes to obtain a first porous quartz fiber ceramic sub-piece to an n-th porous quartz fiber ceramic sub-piece; the surfaces of the first porous quartz fiber ceramic sub-piece to the n-1-th porous quartz fiber ceramic sub-piece are attached with ceramic slurry; the ceramic slurry comprises quartz powder, sintering aid and alcohol in a mass ratio of (9-11):(1-5):(95-105); the sintering aid comprises boron oxide; the first porous quartz fiber ceramic sub-piece to the n-th porous quartz fiber ceramic sub-piece are attached and fixed in a preset order, and then sintered to obtain the gradient low-dielectric high-temperature resistant wave-transparent material; the sintering temperature is 1000-1100 DEG C; the preparation process of the porous quartz fiber ceramic body comprises the following steps: the quartz fiber and the alumina fiber are respectively sheared to obtain short fiber 1 and short fiber 2; the short fiber 1, the short fiber 2, deionized water and an additive are mixed and stirred according to a proportion of (50-90):(10-40):(100-200):(10-15) to obtain a quartz fiber ceramic slurry; the stirring time is 60-120 min; the quartz fiber ceramic slurry is added into a forming mold, and then suction filtration forming is performed; then, drying and high-temperature sintering are performed to obtain the porous quartz fiber ceramic body; the additive comprises boron oxide; the long-diameter ratio of the short fiber 1 is (100-1000):1, and the long-diameter ratio of the short fiber 2 is (100-500):

1.

2. The integrated preparation method of the gradient low dielectric high-temperature-resistant wave-transparent material according to claim 1, characterized in that, when n=3, the silica sol solutions comprise a first silica sol solution, a second silica sol solution and a third silica sol solution; the first silica sol solution is obtained by adjusting the pH of silica sol with ammonia water; the silica sol concentration of the first silica sol solution is 10-30%, and the pH is 4-6; the second silica sol solution is obtained by adjusting the pH of silica sol with ammonia water; the silica sol concentration of the second silica sol solution is 31-41%, and the pH is 4-6; the third silica sol solution is obtained by adjusting the pH of silica sol with ammonia water; the silica sol concentration of the third silica sol solution is 41-55%, and the pH is 4-6. 3.The method of claim 1, wherein the method further comprises: mixing the low dielectric material, the high-temperature resistant material, and the wave-transparent material to form a mixture; and heating the mixture to form the gradient low dielectric high-temperature resistant wave-transparent material. the porous quartz fiber ceramic substrates comprise a first porous quartz fiber ceramic substrate, a second porous quartz fiber ceramic substrate and a third porous quartz fiber ceramic substrate; The porous quartz fiber ceramic body is placed in a vacuum container for vacuum treatment, a first silica sol solution is siphoned into the vacuum container through an inlet at the bottom of the vacuum container, and the inlet is closed and vacuum is maintained for 30-60 min; the impregnated porous quartz fiber ceramic body is heated together with the container and the first silica sol solution, and the first silica sol solution is gelled; the gelled porous quartz fiber ceramic body is dried at a temperature of (100-150) DEG C, and then high-temperature calcination is performed at a temperature of (600-800) DEG C, to obtain a first porous quartz fiber ceramic matrix; the gelling temperature of the first silica sol solution is (80-100) DEG C; The porous quartz fiber ceramic body is placed in a vacuum container for vacuum treatment, a second silica sol solution is siphoned into the vacuum container through an inlet at the bottom of the vacuum container, and the inlet is closed and vacuum is maintained for 30-60 min; the impregnated porous quartz fiber ceramic body is heated together with the container and the second silica sol solution, and the second silica sol solution is gelled; the gelled porous quartz fiber ceramic body is dried at a temperature of (100-150) DEG C, and then high-temperature calcination is performed at a temperature of (600-800) DEG C, to obtain a second porous quartz fiber ceramic matrix; The gelling temperature of the second silica sol solution is (80-100) DEG C; The porous quartz fiber ceramic body is placed in a vacuum container for vacuum treatment, a third silica sol solution is siphoned into the vacuum container through an inlet at the bottom of the vacuum container, and the inlet is closed and vacuum is maintained for 30-60 min; the impregnated porous quartz fiber ceramic body is heated together with the container and the third silica sol solution, and the third silica sol solution is gelled; the gelled porous quartz fiber ceramic body is dried at a temperature of (100-150) DEG C, and then high-temperature calcination is performed at a temperature of (600-800) DEG C, to obtain a third porous quartz fiber ceramic matrix; The gelling temperature of the third silica sol solution is (80-100) DEG C.

4. The integrated preparation method of the gradient low dielectric high-temperature-resistant wave-transparent material according to claim 2, characterized in that, The first porous quartz fiber ceramic matrix, the second porous quartz fiber ceramic matrix, and the third porous quartz fiber ceramic matrix are respectively machined according to corresponding preset sizes, to obtain a first porous quartz fiber ceramic sub-piece, a second porous quartz fiber ceramic sub-piece, and a third porous quartz fiber ceramic sub-piece; The first porous quartz fiber ceramic sub-piece has a thickness of 5-10 mm and a dielectric constant of 1.3-1.5; the second porous quartz fiber ceramic sub-piece has a thickness of 30-40 mm and a dielectric constant of 1.5-1.6; and the third porous quartz fiber ceramic sub-piece has a thickness of 10-20 mm and a dielectric constant of 1.8-1.

9.

5. The integrated preparation method of the gradient low dielectric high-temperature-resistant wave-transparent material according to claim 3, characterized in that, The porous quartz fiber ceramic body includes a first porous quartz fiber ceramic body, a second porous quartz fiber ceramic body, and a third porous quartz fiber ceramic body; The ratio of short fiber 1, short fiber 2, deionized water and additive in the first porous quartz fiber ceramic body is (70-90):(10-20):(100-200):(10-15); The first porous quartz fiber ceramic body has a density of 0.297-0.505 g / cm 3 ; The ratio of short fiber 1, short fiber 2, deionized water and additive in the second porous quartz fiber ceramic body is (60-80):(20-30):(100-200):(10-15); The second porous quartz fiber ceramic body has a density of 0.595-0.65 g / cm 3 ; The ratio of short fiber 1, short fiber 2, deionized water and additive in the third porous quartz fiber ceramic body is (50-70):(30-40):(100-200):(10-15); The third porous quartz fiber ceramic body has a density of 0.81-0.95 g / cm 3 .

6. The integrated preparation method of the gradient low dielectric high temperature resistant wave-transparent material according to claim 4, characterized in that, The first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece and the third porous quartz fiber ceramic sub-piece are arranged horizontally, then the third porous quartz fiber ceramic sub-piece, the first porous quartz fiber ceramic sub-piece and the second porous quartz fiber ceramic sub-piece are sequentially connected and fixed, and then sintering is performed to obtain the gradient low-dielectric high-temperature-resistant wave-transparent material.

7. The integrated preparation method of the gradient low-dielectric high-temperature-resistant wave-transparent material according to claim 1, characterized in that, When n=4, the silica sol solution comprises a first silica sol solution, a second silica sol solution, a third silica sol solution and a fourth silica sol solution; The first silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, and the silica sol concentration of the first silica sol solution is 0-20% and the pH is 4-6; The second silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, and the silica sol concentration of the second silica sol solution is 21-35% and the pH is 4-6; The third silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, and the silica sol concentration of the third silica sol solution is 36-45% and the pH is 4-6; The fourth silica sol solution is obtained by adjusting the pH of silica sol with ammonia water, and the silica sol concentration of the fourth silica sol solution is 41-55% and the pH is 4-6; And / or The porous quartz fiber ceramic body comprises a first porous quartz fiber ceramic body, a second porous quartz fiber ceramic body, a third porous quartz fiber ceramic body and a fourth porous quartz fiber ceramic body; The ratio of short fiber 1, short fiber 2, deionized water and additive in the first porous quartz fiber ceramic body is (80-90):(10-15):(100-200):(10-15); The first porous quartz fiber ceramic body has a density of 0.27-0.45 g / cm 3 ; The ratio of short fiber 1, short fiber 2, deionized water and additive in the second porous quartz fiber ceramic body is (70-80):(15-25):(100-200):(10-15); The second porous quartz fiber ceramic body has a density of 0.45-0.65 g / cm 3 ; The ratio of short fiber 1, short fiber 2, deionized water and additive in the third porous quartz fiber ceramic body is (60-70):(20-30):(100-200):(10-15); The third porous quartz fiber ceramic body has a density of 0.7-0.9 g / cm 3 ; The ratio of short fiber 1, short fiber 2, deionized water and additive in the fourth porous quartz fiber ceramic body is (50-60):(30-40):(100-200):(10-15); The fourth porous quartz fiber ceramic body has a density of 0.85-0.95 g / cm 3 . 8.The method of claim 7, wherein the method further comprises the step of: The first porous quartz fiber ceramic matrix, the second porous quartz fiber ceramic matrix, the third porous quartz fiber ceramic matrix, and the fourth porous quartz fiber ceramic matrix are respectively machined according to corresponding preset sizes to obtain a first porous quartz fiber ceramic sub-piece, a second porous quartz fiber ceramic sub-piece, a third porous quartz fiber ceramic sub-piece, and a fourth porous quartz fiber ceramic sub-piece; ​ The first porous quartz fiber ceramic sub-piece has a thickness of 45-50 mm and a dielectric constant of 1.3-1.4; the second porous quartz fiber ceramic sub-piece has a thickness of 35-40 mm and a dielectric constant of 1.5-1.6; the third porous quartz fiber ceramic sub-piece has a thickness of 25-30 mm and a dielectric constant of 1.7-1.8; and the fourth porous quartz fiber ceramic sub-piece has a thickness of 40-45 mm and a dielectric constant of 1.8-1.9; The first porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece, and the third porous quartz fiber ceramic sub-piece are all arranged in a curved manner, then the fourth porous quartz fiber ceramic sub-piece, the third porous quartz fiber ceramic sub-piece, the second porous quartz fiber ceramic sub-piece, and the first porous quartz fiber ceramic sub-piece are sequentially attached, fixed, and sintered to obtain the gradient low-dielectric high-temperature-resistant wave-transparent material.