CN112409653A - Wave absorbing agent, preparation method and application thereof - Google Patents
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Abstract
The invention provides a wave absorbing agent and a preparation method thereof, and the wave absorbing agent comprises the following steps of S1: carrying out hydroxylation treatment on a plurality of nano-silica with different particle sizes, wherein the particle size ratio of the large-particle size nano-silica to the small-particle size nano-silica is more than or equal to 5; s2: according to the preset formulaWeighing hydroxylated nano silicon dioxide, carbonyl iron powder, agate beads and absolute ethyl alcohol, and putting the materials into a ball milling tank; s3: the mixture is subjected to mechanochemical ball milling for a certain time, silicon dioxide gradation with different grain diameters is obtained after drying, large-grain-diameter grains are surrounded by small-grain-diameter grains, and SiO which is mainly distributed in a long chain shape is formed2The wave absorbing agent of the particle microcosmic filler network, and the interface of the nano silicon dioxide and the carbonyl iron powder generates-Si-O-Si-bond through chemical reaction for connection. The invention obtains the wave absorber with excellent processing performance and impedance matching performance through the grading of nano silicon dioxide with different particle sizes and a simple mechanochemical ball milling process.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of wave absorbers, in particular to a wave absorber, and a preparation method and application thereof.
[ background of the invention ]
The wave-absorbing material has very important and wide application in the fields of aerospace, electronic materials and the like, the currently used wave-absorbing material is mainly used for the working frequency X and Ku wave bands of radar, is limited by intrinsic electromagnetic parameters of the material, has limited absorption capacity for radar waves in low-frequency wave bands, gradually evolves the working frequency bands to low frequencies along with the continuous development of radar detection technology, and actively explores a new camouflage and stealth technology for the detection of low-frequency meter wave radar by various governments on the basis of the increasingly mature research on 4-20 GHz high-frequency wave-absorbing materials at home and abroad. However, most researches are focused on high-frequency wave-absorbing materials, and the researches on low-frequency L (1-2GHz) and S (2-4GHz) wave bands are not comprehensive.
Carbonyl iron powder is a metal micro-powder wave absorbing agent with excellent performance, and has magnetic loss and medium loss mechanisms, but the impedance matching of the carbonyl iron powder is poor, and the impedance matching of the carbonyl iron powder can be improved by coating a low dielectric layer on the surface of the carbonyl iron powder, but the prior art is complex, has the problems of large environmental pollution and incapability of being suitable for batch production, and the interface connecting force of a coating layer and the carbonyl iron powder is weak, so that the coating structure of the carbonyl iron powder is easily damaged in the processing process, and the processing performance is poor.
[ summary of the invention ]
In order to solve the above technical problem, the present invention provides a method for preparing a wave absorbing agent, comprising the following steps of S1: carrying out the preparation of nano silicon dioxide with various particle sizesHydroxylation treatment, wherein the particle diameter ratio of the large-particle-size nano silicon dioxide to the small-particle-size nano silicon dioxide is more than or equal to 5; s2: weighing hydroxylated nano silicon dioxide, carbonyl iron powder, agate beads and absolute ethyl alcohol according to a preset ratio, and putting the materials into a ball milling tank; s3: the mixture is subjected to mechanochemical ball milling for a certain time, silicon dioxide gradation with different grain diameters is obtained after drying, large-grain-diameter grains are surrounded by small-grain-diameter grains, and SiO which is mainly distributed in a long chain shape is formed2The wave absorbing agent of the particle microcosmic filler network is a wave absorbing agent with silicon dioxide coated on the edge and/or the surface of flaky carbonyl iron powder, and the interface of the nano silicon dioxide and the carbonyl iron powder is connected by generating a-Si-O-Si-bond through chemical reaction. According to the invention, carbonyl iron powder is flaked by a simple mechanochemical ball milling process, silicon dioxide networks with different grain size gradations are coated on the edge and/or the surface of the flaky carbonyl iron powder, and the interface of nano silicon dioxide and the carbonyl iron powder is connected by a-Si-O-Si-bond generated by chemical reaction, so that the wave absorbing agent with better processing performance and impedance matching performance is obtained. The wave absorbing agent has good binding property with the rubber elastic matrix, and a ternary interface non-uniform composite material can be obtained, so that a low-frequency rubber wave absorbing product with excellent service performance is prepared, and the low-frequency rubber wave absorbing product has a good low-frequency application prospect.
In some embodiments of the present invention, the hydroxylating process in step S1 includes activating the nano-silica with a mixed solution of concentrated sulfuric acid and hydrogen peroxide, where the mass ratio of the concentrated sulfuric acid to the hydrogen peroxide is 70:30, the reaction temperature is 70-80 ℃, and the reaction time is 0.5-2 hours.
In some embodiments of the present invention, the particle size of the nano-silica in step S1 is 2nm to 100nm, wherein the nano-silica is a graded combination of two different particle sizes, and the particle size ratio of the large-particle size nano-silica to the small-particle size nano-silica is greater than or equal to 5.
In some embodiments of the present invention, the large-particle size nano-silica has a particle size of 50 to 100nm, and the small-particle size nano-silica has a particle size of 2 to 20 nm.
In some embodiments of the invention, the mass ratio of the large-particle size nanosilica to the small-particle size nanosilica is 2: 1.
In some embodiments of the invention, the carbonyl iron powder: nano silicon dioxide: agate: the absolute ethyl alcohol is 100 g: (2-5) g: (1000-2000) g (1-2.2) L.
In some embodiments of the present invention, 1 to 3g of ester compound may be further added in the step S2.
In some embodiments of the present invention, in the step S3, the ball milling speed is 250 to 450r/min, and the ball milling time is 24 to 48 hours.
The invention also discloses a wave absorbing agent obtained by the preparation method or the preparation method and application of the wave absorbing agent in wave absorbing materials.
The invention also discloses a preparation method of the low-frequency flexible rubber wave-absorbing material, which comprises the following steps of a, weighing the nitrile rubber, the wave-absorbing agent, the vulcanizing agent sulfur, the accelerator M, the activator zinc oxide and the plasticizer stearic acid according to a preset ratio, wherein the ratio by mass parts is 100: 700: 3:1:5: 2; b. mixing the raw materials on an open type double-roller open mill, performing triangular packaging and thin passing for a plurality of times, uniformly mixing, then discharging and cooling to obtain a rubber material; c. and (3) placing the rubber material at normal temperature for more than 24h, and then curing and forming to obtain the rubber wave-absorbing material. The wave absorbing agent has good associativity with the rubber elastic matrix, and a ternary interface non-uniform composite material can be obtained, so that a low-frequency rubber wave absorbing product with excellent service performance is prepared, and the low-frequency rubber wave absorbing product has a good low-frequency application prospect.
In some embodiments of the present invention, the temperature for curing and molding the rubber compound is 140-.
According to the invention, carbonyl iron powder is flaked by ball milling through a mechanochemical method, and a stronger anisotropic field can be obtained, so that the magnetic conductivity is improved, and the absorption attenuation of the carbonyl iron powder on electromagnetic waves is improved. The carbonyl iron powder after ball milling has a flat stacking structure, and the vacancy among the arrangement of the flaky particles can influence the continuity of the conductive network. In one aspect of the invention, SiO with different grain diameters is used2Grading to form long chains with large particle size particles surrounded by small particle size particlesPredominantly distributed SiO2The particle microcosmic filler network has enough path to reduce relaxation time, thus reducing dielectric constant and improving the impedance matching performance of the interface of electromagnetic wave and material. On the other hand, in the ball milling process, a large number of defects are generated at the edges of the flaky particles to form vacancies and dislocations, free hydroxyl groups generated by absolute ethyl alcohol can fill the vacancies, and the free hydroxyl groups and SiO with abundant hydroxyl groups on the surface2Reaction to form firm-Si-O-Si-bond, SiO2The wave-absorbing material is stably attached to the surface and/or the edge of flaky carbonyl iron powder and is bonded with a rubber matrix to prepare the wave-absorbing material, and the wave-absorbing material forms a ternary interface heterogeneous composite material which can cause various reflection and propagation paths to enhance the interface loss and scattering loss of electromagnetic wave incidence.
[ description of the drawings ]
FIG. 1 is a scanning electron microscope image of a mixture of nano-silica with different particle sizes and carbonyl iron powder in example 1 of the present invention before ball milling treatment;
FIG. 2 is a scanning electron micrograph of a wave absorber obtained in example 1 of the present invention.
[ detailed description ] embodiments
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Preparation of wave absorber
S1, carrying out hydroxylation treatment on two kinds of nano-silica with different particle sizes, wherein the particle size of the large-particle size nano-silica is 50-100nm, the particle size of the small-particle size nano-silica is 2-20nm, the particle size ratio of the large-particle size nano-silica to the small-particle size nano-silica is 5, and the mass ratio of the large-particle size nano-silica to the small-particle size nano-silica is 2: 1; s2: weighing hydroxylated nano silicon dioxide, carbonyl iron powder, agate beads and absolute ethyl alcohol according to a preset ratio, and putting the materials into a ball milling tank, wherein the weight ratio of the carbonyl iron powder: nano silicon dioxide: agate: the absolute ethyl alcohol is 100 g: (2-5) g: (1000-2000) g (1.0-2.2) L; s3: the ball milling speed is 250-450 r/min, the ball milling time is 24-48 h, the wave absorbing agent with silicon dioxide coated on the edge and/or the surface of the flaky carbonyl iron powder is obtained after drying, and the interface of the nano silicon dioxide and the carbonyl iron powder is connected by generating-Si-O-Si-bonds through chemical reaction.
In other embodiments of the present invention, in step S2, materials such as glycerol methacrylate, acrylate, and methyl acetate may also be added, and a mechanochemical effect generated during the ball milling process may induce a chemical reaction with the silica, and under the action of a mechanical force, Si — O bonds of a portion of the silica particles are broken to generate free radicals, and ester bonds are broken to react with the free radicals — OH, so that the surface of the silica has chemically active organic groups, which may further increase the interfacial bonding force between the nano silica and the carbonyl iron powder, and enhance the compatibility between the functional nano silica and the organic rubber matrix.
In other embodiments of the present invention, the particle size of the nano-silica is 2nm to 100nm, and the nano-silica can be graded by 3 or more than 3 different particle sizes, wherein the particle size ratio of any large-particle size nano-silica to small-particle size nano-silica is not less than 5, which is beneficial to further improving the coating of the nano-silica on carbonyl iron powder and adjusting the impedance matching characteristic of the carbonyl iron powder.
In other embodiments of the present invention, the hydroxylation process in step S1 includes activating the nano-silica with a mixed solution of concentrated sulfuric acid and hydrogen peroxide, where the mass ratio of concentrated sulfuric acid to hydrogen peroxide is 70:30, the reaction temperature is 70-80 ℃, and the reaction time is 0.5-2 hours. The process can further increase the hydroxyl content of the hydroxylated nano-silica and can activate the hydroxyl on the surface of the silica.
In order to further verify the wave absorbing performance and the processing performance of the wave absorbing agent prepared in the invention, the prepared wave absorbing agent and rubber are blended to prepare the wave absorbing material, and the wave absorbing performance is evaluated and tested.
Example 1
Preparing a wave absorbing agent: s1, carrying out hydroxylation treatment on two kinds of nano-silica with different particle sizes, wherein the particle size of the large-particle size nano-silica is 50-100nm, the particle size of the small-particle size nano-silica is 2-20nm, the particle size ratio of the large-particle size nano-silica to the small-particle size nano-silica is 5, and the mass ratio of the large-particle size nano-silica to the small-particle size nano-silica is 2: 1; s2: putting the hydroxylated nano silicon dioxide, carbonyl iron powder, agate beads and absolute ethyl alcohol into a ball milling tank according to a preset ratio, wherein the carbonyl iron powder is spherical particles with the particle size of 3-10 um: nano silicon dioxide: agate: the absolute ethyl alcohol is 100 g:2 g: 1000g: 1L; s3: the ball milling speed is 250r/min, and the ball milling time is 24 h.
Preparing a wave-absorbing rubber material: a. weighing nitrile rubber, a wave absorbing agent, a vulcanizing agent sulfur, an accelerator M, an activator zinc oxide and a plasticizer stearic acid according to a preset ratio, wherein the ratio by mass phr is 100: 700: 3:1:3: 2; b. mixing the raw materials on an open type double-roller open mill, performing triangular packaging and thin passing for a plurality of times, uniformly mixing, then discharging and cooling to obtain a rubber material; c. and (3) placing the rubber material for more than 24h at normal temperature, then filling the rubber material into a forming die with the length, width and thickness of 300 x 300mm and the thickness of 2.0mm, curing at the temperature of 140-.
Referring to fig. 1 and fig. 2, it can be seen from fig. 1 that nano-silica and carbonyl iron powder particles in a spherical shape are changed into a flaked microstructure shown in fig. 2 after being processed by the mechanochemical method of the present invention, and the flaked edges show a distinct interface polarization structure state. At the mark of fig. 2, a SiO2 particle microcollection network is formed, in which large-particle-size particles are surrounded by small-particle-size particles and are mainly distributed in a long chain shape, and the flaky carbonyl iron powder surface and the surface connection thereof have rough and cohesive nano-shaped substances, but no void structure exists in which the nano-shaped substances exist alone, which indicates that the microcollection structure with tightly-connected-Si-O-Si-bonds is generated at the interface of the nano-silica and the carbonyl iron powder through chemical reaction.
Example 2
Preparing a wave absorbing agent: s1, carrying out hydroxylation treatment on two kinds of nano-silica with different particle sizes, wherein the particle size of the large-particle size nano-silica is 50-100nm, the particle size of the small-particle size nano-silica is 2-10nm, the particle size ratio of the large-particle size nano-silica to the small-particle size nano-silica is 8, and the mass ratio of the large-particle size nano-silica to the small-particle size nano-silica is 2: 1; s2: putting the hydroxylated nano silicon dioxide, carbonyl iron powder, agate beads and absolute ethyl alcohol into a ball milling tank according to a preset ratio, wherein the carbonyl iron powder is spherical particles with the particle size of 3-10 um: nano silicon dioxide: agate: the absolute ethyl alcohol is 100 g: 3 g: 1500g, 2L; s3: the ball milling speed is 300r/min, and the ball milling time is 30 h.
Preparing a wave-absorbing material: a. weighing nitrile rubber, a wave absorbing agent, a vulcanizing agent sulfur, an accelerator M, an activator zinc oxide and a plasticizer stearic acid according to a preset ratio, wherein the ratio by mass phr is 100: 700: 3:1:3: 2; b. mixing the raw materials on an open type double-roller open mill, performing triangular packaging and thin passing for a plurality of times, uniformly mixing, then discharging and cooling to obtain a rubber material; c. and (3) placing the rubber material for more than 24h at normal temperature, then filling the rubber material into a forming die with the length, width and thickness of 300 x 300mm and the thickness of 2.0mm, curing at the temperature of 140-.
Example 3
Preparing a wave absorbing agent: s1: according to the scheme, hydroxylation treatment is carried out on two kinds of nano-silica with different particle sizes, wherein the particle size of the large-particle-size nano-silica is 50-100nm, the particle size of the small-particle-size nano-silica is 2-10nm, the particle size ratio of the large-particle-size nano-silica to the small-particle-size nano-silica is 8, and the mass ratio of the large-particle-size nano-silica to the small-particle-size nano-silica is 2: 1; s2: putting the hydroxylated nano silicon dioxide, carbonyl iron powder, agate beads and absolute ethyl alcohol into a ball milling tank according to a preset ratio, wherein the carbonyl iron powder is spherical particles with the particle size of 3-10 um: nano silicon dioxide: glycerol methacrylate: agate: the absolute ethyl alcohol is 100 g: 3 g:1.5 g: 1500g, 2L; s3: the ball milling speed is 400r/min, and the ball milling time is 48 h.
Preparing a wave-absorbing material: a. weighing nitrile rubber, a wave absorbing agent, a vulcanizing agent sulfur, an accelerator M, an activator zinc oxide and a plasticizer stearic acid according to a preset ratio, wherein the ratio by mass phr is 100: 700: 3:1:4: 3; b. mixing the raw materials on an open type double-roller open mill, performing triangular packaging and thin passing for a plurality of times, uniformly mixing, then discharging and cooling to obtain a rubber material; c. placing the rubber material at normal temperature for more than 24h, filling the rubber material into a forming die with the length, width and thickness of 300 x 300mm and the thickness of 2.0mm, curing at the temperature of 140-
Comparative example 4
Preparing a wave absorbing agent: s1, carrying out hydroxylation treatment on two kinds of nano-silica with different particle sizes, wherein the particle size of the large-particle size nano-silica is 50-100nm, the particle size of the small-particle size nano-silica is 2-20nm, the particle size ratio of the large-particle size nano-silica to the small-particle size nano-silica is 5, and the mass ratio of the large-particle size nano-silica to the small-particle size nano-silica is 2: 1; s2: putting carbonyl iron powder, agate beads and absolute ethyl alcohol into a ball milling tank according to a preset ratio, wherein the carbonyl iron powder is spherical particles with the particle size of 3-10um, and the carbonyl iron powder: agate: the absolute ethyl alcohol is 100 g:2 g: 1000g: 1L; s3: the ball milling rotation speed is 250r/min, the ball milling time is 24h, and carbonyl iron powder is subjected to flakiness ball milling treatment; s4: and physically blending the dried carbonyl iron powder and the graded silicon dioxide by a mixing stirrer to prepare the wave absorbing agent.
Preparing a wave-absorbing material: a. weighing nitrile rubber, a wave absorbing agent, a vulcanizing agent sulfur, an accelerator M, an activator zinc oxide and a plasticizer stearic acid according to a preset ratio, wherein the ratio by mass phr is 100: 700: 3:1:3: 2; b. mixing the raw materials on an open type double-roller open mill, performing triangular packaging and thin passing for a plurality of times, uniformly mixing, then discharging and cooling to obtain a rubber material; c. and (3) placing the rubber material for more than 24h at normal temperature, then filling the rubber material into a forming die with the length, width and thickness of 300 x 300mm and the thickness of 2.0mm, curing at the temperature of 140-.
Comparative example 5
Preparing a wave absorbing agent: s1: according to the scheme, nano silicon dioxide with the same particle size is added for hydroxylation treatment, wherein the particle size range of the nano silicon dioxide is 80-100 nm. S2: putting the hydroxylated nano silicon dioxide, carbonyl iron powder, agate beads and absolute ethyl alcohol into a ball milling tank according to a preset ratio, wherein the carbonyl iron powder is spherical particles with the particle size of 3-10 um: nano silicon dioxide: agate: the absolute ethyl alcohol is 100 g: 4 g: 1000g: 1.5L; s3: the ball milling speed is 250r/min, and the ball milling time is 36 h.
Preparing a wave-absorbing material: a. weighing nitrile rubber, a wave absorbing agent, a vulcanizing agent sulfur, an accelerator M, an activator zinc oxide and a plasticizer stearic acid according to a preset ratio, wherein the ratio by mass phr is 100: 700: 3:1:3: 2; b. mixing the raw materials on an open type double-roller open mill, performing triangular packaging and thin passing for a plurality of times, uniformly mixing, then discharging and cooling to obtain a rubber material; c. and (3) placing the rubber material for more than 24h at normal temperature, then filling the rubber material into a forming die with the length, width and thickness of 300 x 300mm and the thickness of 2.0mm, curing at the temperature of 140-.
Comparative example 6
Preparing a wave absorbing agent: s1: according to the scheme, nano silicon dioxide is not added, and carbonyl iron powder is simply mechanically ball-milled to prepare the wave absorbing agent. S2: putting carbonyl iron powder, agate beads and absolute ethyl alcohol into a ball milling tank according to a preset ratio, wherein the carbonyl iron powder is spherical particles with the particle size of 3-10um, and the carbonyl iron powder: agate: the absolute ethyl alcohol is 100 g: 1000g, 2L; s3: the ball milling speed is 300r/min, and the ball milling time is 36 h.
Preparing a wave-absorbing material: a. weighing nitrile rubber, a wave absorbing agent, a vulcanizing agent sulfur, an accelerator M, an activator zinc oxide and a plasticizer stearic acid according to a preset ratio, wherein the ratio by mass phr is 100: 700: 3:1:3: 2; b. mixing the raw materials on an open type double-roller open mill, performing triangular packaging and thin passing for a plurality of times, uniformly mixing, then discharging and cooling to obtain a rubber material; c. and (3) placing the rubber material for more than 24h at normal temperature, then filling the rubber material into a forming die with the length, width and thickness of 300 x 300mm and the thickness of 2.0mm, curing at the temperature of 140-.
The wave absorbing agent prepared in cases 1 to 6 and paraffin are heated in a high-temperature furnace at 50-60 ℃ according to the mass ratio of 80:20, then the wave absorbing agent and the paraffin are quickly taken out, mixed and stirred uniformly, the obtained viscous solid is filled into a coaxial ring mold (the outer diameter of the mold is 7mm, the inner diameter of the mold is 3.04mm), samples with the thickness of 1-2mm are respectively prepared, and then a network vector analyzer is adopted to respectively measure the complex dielectric constant and the complex permeability.
The wave absorbing agents prepared in cases 1 to 6 were mixed with the nitrile rubber material to prepare wave absorbing materials, and the reflectivity and mechanical properties of the rubber wave absorbing materials were tested according to GJB2038A-2011 and GBT528-2009, with the results shown in table 1.
Table 1 results of testing reflectivity and mechanical property of wave-absorbing material in different embodiments
In the above embodiments, the present invention has been described only by way of example, but various modifications may be made by those skilled in the art without departing from the spirit and scope of the invention after reading the present patent application.
Claims (10)
1. The preparation method of the wave absorbing agent is characterized by comprising the following steps:
s1: carrying out hydroxylation treatment on a plurality of nano-silica with different particle sizes, wherein the particle size ratio of the large-particle size nano-silica to the small-particle size nano-silica is more than or equal to 5;
s2: weighing hydroxylated nano silicon dioxide, carbonyl iron powder, agate beads and absolute ethyl alcohol according to a preset ratio, and putting the materials into a ball milling tank;
s3: the mixture is subjected to mechanochemical ball milling for a certain time, silicon dioxide gradation with different grain diameters is obtained after drying, large-grain-diameter grains are surrounded by small-grain-diameter grains, and SiO which is mainly distributed in a long chain shape is formed2The wave absorbing agent of the particle microcosmic filler network, and the interface of the nano silicon dioxide and the carbonyl iron powder generates-Si-O-Si-bond through chemical reaction for connection.
2. The preparation method of claim 1, wherein the hydroxylation treatment process in the step S1 includes activating the nano-silica with a mixed solution of concentrated sulfuric acid and hydrogen peroxide, wherein the mass ratio of concentrated sulfuric acid to hydrogen peroxide is 70:30, the reaction temperature is 70-80 ℃, and the reaction time is 0.5-2 hours.
3. The method according to claim 1, wherein the nano-silica in step S1 has a particle size of 2nm to 100nm, wherein the nano-silica is a graded combination of two different particle sizes, and the ratio of the particle size of the large-particle size nano-silica to the particle size of the small-particle size nano-silica is 5 to 10.
4. The method according to claim 3, wherein the large-particle size nanosilicon dioxide has a particle size of 50 to 100nm and the small-particle size nanosilicon dioxide has a particle size of 2 to 20 nm.
5. The method according to claim 3, wherein the mass ratio of the large-particle size nano silica to the small-particle size nano silica is 2: 1.
6. The method of claim 1, wherein the carbonyl iron powder in step S2: nano silicon dioxide: agate beads: the absolute ethyl alcohol is 100 g: (2-5) g: (1000-2000) g (1-2.2) L.
7. The method of claim 6, wherein 1-3g of ester compound is further added in step S2.
8. A wave absorbing agent obtained by the production method according to any one of claims 1 to 7.
9. A preparation method of a low-frequency flexible rubber wave-absorbing material is characterized by comprising the following steps of a, weighing nitrile rubber, a wave-absorbing agent, a vulcanizing agent, an accelerator, an activator and a plasticizer according to a preset ratio, wherein the ratio by mass parts phr is 100: 700: 3-4:1-2:3-5:2-4, wherein the wave absorber is obtained by the preparation method of any one of claims 1-7;
b. mixing the raw materials on an open type double-roller open mill, performing triangular packaging and thin passing for a plurality of times, mixing for 20-30 min, and then performing sheet-feeding cooling to obtain a rubber material;
c. and (3) placing the rubber material at normal temperature for more than 24h, and then curing and forming to obtain the rubber wave-absorbing material.
10. The method according to claim 9, wherein the temperature for curing and molding the rubber compound is 140-150 ℃, the curing pressure is 14-16MPa, and the curing time is 10-12 min.
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