CN115628646B - High-temperature-resistant radar wave-absorbing material, method for preparing wave-absorbing coating by using same and application of material - Google Patents
High-temperature-resistant radar wave-absorbing material, method for preparing wave-absorbing coating by using same and application of material Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 97
- 239000011248 coating agent Substances 0.000 title claims abstract description 94
- 239000000463 material Substances 0.000 title claims abstract description 50
- 239000011358 absorbing material Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000005507 spraying Methods 0.000 claims abstract description 83
- 229910004283 SiO 4 Inorganic materials 0.000 claims abstract description 55
- 239000000843 powder Substances 0.000 claims abstract description 55
- 238000007750 plasma spraying Methods 0.000 claims abstract description 35
- 238000005516 engineering process Methods 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 239000000956 alloy Substances 0.000 claims abstract description 19
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 19
- 229910052747 lanthanoid Inorganic materials 0.000 claims abstract description 4
- 150000002602 lanthanoids Chemical class 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
- 238000001354 calcination Methods 0.000 claims description 34
- 239000002002 slurry Substances 0.000 claims description 31
- 238000000498 ball milling Methods 0.000 claims description 29
- 229910052746 lanthanum Inorganic materials 0.000 claims description 25
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 25
- 229910052786 argon Inorganic materials 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 19
- 229910052710 silicon Inorganic materials 0.000 claims description 19
- 239000010703 silicon Substances 0.000 claims description 19
- 229910052712 strontium Inorganic materials 0.000 claims description 19
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 19
- 238000007873 sieving Methods 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 16
- 239000007921 spray Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- QSQXISIULMTHLV-UHFFFAOYSA-N strontium;dioxido(oxo)silane Chemical compound [Sr+2].[O-][Si]([O-])=O QSQXISIULMTHLV-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052917 strontium silicate Inorganic materials 0.000 abstract description 5
- 238000012795 verification Methods 0.000 abstract description 3
- 230000035939 shock Effects 0.000 abstract description 2
- 238000005336 cracking Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 14
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- 238000002310 reflectometry Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
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- 230000000694 effects Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 208000004232 Enteritis Diseases 0.000 description 1
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F41—WEAPONS
- F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
- F41H3/00—Camouflage, i.e. means or methods for concealment or disguise
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
Abstract
The invention discloses a high-temperature-resistant radar wave-absorbing material, a method for preparing a wave-absorbing coating by using the same and application thereof, wherein the molecular formula of the radar wave-absorbing material is Sr (2‑x) Ln x SiO 4 Wherein Ln is any lanthanoid element, and the doping amount x=0.6-1.0; the material takes strontium silicate with the thermal expansion coefficient close to that of an alloy base material used for a high-temperature part of weapon equipment as a base body phase, ln is used 3+ Substituted Sr 2 SiO 4 Part of Sr in material 2+ The formed powder material is then made into wave-absorbing coating by plasma spraying technology, and relevant parameters of spraying are strictly controlled. Compared with the traditional strontium silicate dielectric loss, the wave-absorbing coating prepared by the material has the advantages of good wave-absorbing performance at normal temperature and high temperature, good heat matching performance with a high-temperature alloy substrate, difficult falling and cracking at high temperature and good thermal shock resistance, and is particularly suitable for radar camouflage of weapon equipment through practical verification.
Description
Technical Field
The invention belongs to the technical field of wave-absorbing coating materials, and particularly relates to a high-temperature-resistant radar wave-absorbing material, a method for preparing a wave-absorbing coating by using the same and application of the material.
Background
As is well known, with the development and application of detection technologies such as infrared and radar, a serious threat is formed to the survival of modern weaponry in recent years, and in order to protect own weaponry and take the leading role in battlefield, development of stealth detection technologies is an important task in modern military. According to different combat conditions and detection means, stealth detection technologies can be classified into radar stealth, infrared stealth, sound wave stealth and the like, wherein the radar stealth technology mainly reduces radar echo intensity, namely reduces radar scattering cross section (Radar Cross Section, RCS for short) to weaken and inhibit target radar echo intensity, and further achieves the stealth purpose.
At present, the radar echo intensity is reduced by the following two means: firstly, designing the external shape of the combat weapon equipment so as to reduce radar signals reflected by the combat weapon equipment; secondly, radar wave absorbing materials are used on the surfaces of the weaponry to absorb, attenuate and convert electromagnetic waves, so that the radar scattering sectional area of the weaponry is reduced. The external shape design has higher transformation difficulty and higher cost, and the weight of the weapon equipment is easy to increase, so that the comprehensive performance of the weapon equipment is reduced, and the practical application has larger limit, and the radar wave-absorbing material just can make up for the defect, so that the radar wave-absorbing material becomes one of the important research points of various military countries, and particularly the wave-absorbing material applied to high-temperature parts of the weapon equipment.
The existing high-temperature wave absorbing materials which are more studied have C, siC, znO and the like, wherein C has the advantages of low density, high temperature resistance in inert atmosphere, adjustable electrical property, wide sources and the like, but has higher conductivity, serious impedance mismatch with free space, strong reflection on electromagnetic waves, poor wave absorbing performance, poor high-temperature oxidation resistance, oxidation reaction in an oxidizing atmosphere at 370 ℃ and incapability of serving at high temperature; the dielectric loss of pure SiC and pure ZnO is low, and the expected wave-absorbing effect is difficult to achieve at high temperature, so that a radar wave-absorbing material with good wave-absorbing performance at low temperature and high temperature is required to be researched.
In view of the above, the present inventors provide a high temperature resistant radar absorbing material, and a method and application for preparing a absorbing coating using the same, so as to overcome the defects of the prior art.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a high-temperature-resistant radar wave-absorbing material, a method for preparing a wave-absorbing coating by using the same and application thereof.
The aim of the invention is realized by the following technical scheme:
in a first aspect, the present invention provides a high temperature resistant radar absorbing material, where the molecular formula of the radar absorbing material is Sr (2-x) Ln x SiO 4 Wherein Ln is any lanthanoid element, and the doping amount x=0.4 to 1.0.
Further, the doping amount x=0.6 to 1.0.
In a second aspect, the present invention provides a method for preparing a wave-absorbing coating using the radar wave-absorbing material, the method comprising the steps of:
firstly, weighing a strontium source, a lanthanum source and a silicon source in set amounts in proportion, adding absolute ethyl alcohol, and ball-milling at the speed of 200-350 r/min for 10-14 h at room temperature to obtain slurry;
step two, standing the slurry obtained in the step one for 6 to 8 hours, and drying at 80 ℃ for 30 minutes to obtain a dried material;
calcining the dried material obtained in the step II at 1200-1350 ℃ for 3-6 h, cooling, grinding and sieving to obtain Sr after the calcining is finished (2-x) Ln x SiO 4 Powder, namely radar wave-absorbing material;
fourthly, using a plasma spraying technology to spray the Sr obtained in the third step (2-x) Ln x SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
and fifthly, placing the wave-absorbing coating subjected to the half-curing in the step four to be calcined for 4 to 6 hours at 900 to 1000 ℃ to obtain the cured wave-absorbing coating.
Further, the strontium source is SrCO 3 Or Sr (NO) 3 ) 2 Lanthanum source Ln 2 O 3 、Ln 2 (CO 3 ) 3 Or Ln (NO) 3 ) 3 The silicon source is SiO 2 。
Further, when Ln is used 2 O 3 Or Ln 2 (CO 3 ) 3 When the strontium source is used as the lanthanum source, the mole ratio of the strontium source, the lanthanum source and the silicon source is that: lanthanum source: silicon source= (2-x): x/2:1, a step of;
when Ln (NO) 3 ) 3 When the strontium source is used as the lanthanum source, the mole ratio of the strontium source, the lanthanum source and the silicon source is that: lanthanum source: silicon source= (2-x): x:1.
further, the Sr is obtained after sieving in the step three (2-x) Ln x SiO 4 The particle size of the powder is 40-90 μm for plasma spraying operation.
Further, in the plasma spraying in the fourth step, argon and nitrogen are used as working gases, and parameters are set as follows: argon flow is 30L/min-40L/min, nitrogen flow is 5L/min-10L/min, spraying voltage is 30V-32V, spraying current is 200A-240A, spraying distance is 80 mm-120 mm, air carrying capacity is 5L/min-8L/min, powder feeding rate is 50 g/min-100 g/min, and spraying angle is 90 degrees.
Further, the thickness of the wave-absorbing coating after curing in the step five is 1.10 mm-1.55 mm.
In a third aspect, the invention also provides an application of the radar wave-absorbing material, namely, the radar wave-absorbing material is used as a raw material of the stealth coating, and plasma spraying is carried out on the surface of the substrate to be stealth to form the wave-absorbing coating for radar camouflage.
Further, the base is a metal substrate, and before application, the metal substrate is subjected to sand blasting and cleaning.
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:
1. the radar wave-absorbing material provided by the invention uses strontium silicate as a matrix phase and Ln 3+ Enter itIs doped and subjected to a series of treatments, and the thermal expansion coefficient of the strontium silicate is 12 multiplied by 10 -6 ～13×10 -6 While the thermal expansion coefficient of the alloy base material used for the high-temperature component of the weapon equipment is generally 14×10 -6 ～15×10 -6 Namely, the thermal expansion coefficients of the two materials are relatively close, so that the wave-absorbing coating prepared from the radar wave-absorbing material has good thermal matching property with the base material, and the wave-absorbing coating is not easy to fall off or crack under the high temperature condition and has good thermal shock resistance through practical verification.
2. The invention uses Ln 3+ Substituted Sr 2 SiO 4 Part of Sr in material 2+ Redundant electrons are generated in the electromagnetic wave generating device, and weak current is generated under an external electric field, so that the loss of the electromagnetic wave is increased; while Ln 3+ Ion size of (a) is larger than Sr 2+ Small, replacing Sr with it 2+ Vacancies are generated, lattice contraction and lattice distortion are caused, and dielectric loss of the material is further increased, so that wave absorbing performance is improved, and reflection of electromagnetic waves is reduced.
3. The radar wave-absorbing material and the method for preparing the wave-absorbing coating by using the material provided by the invention can be used at room temperature, have higher dielectric loss and lower emissivity at high temperature, have wider application range and are particularly suitable for radar camouflage of weapon equipment.
Detailed Description
Exemplary embodiments will be described in detail herein. The implementations described in the following exemplary examples do not represent all implementations consistent with the invention. Rather, they are merely examples of certain aspects of the invention that are consistent with the details of the claims below.
The present invention will be described in further detail with reference to examples for better understanding of the technical aspects of the present invention by those skilled in the art.
In a first aspect, the present invention provides a high temperature resistant radar absorbing material, where the molecular formula of the radar absorbing material is Sr (2-x) Ln x SiO 4 Wherein Ln is any one of lanthanide elementsThe doping amount x=0.4 to 1.0. Preferably, the doping amount x=0.6 to 1.0, since Ln is smaller than 0.6 when the doping amount x is smaller than 0.6 3+ Substituted Sr 2+ After that, the generated free charge is less, the dielectric loss of electromagnetic waves is not greatly increased, and the wave absorbing performance of the wave absorbing material is not obviously improved; when the doping amount x is larger than 1.0, the lattice distortion seriously promotes the destruction of the crystal structure of the matrix phase (strontium silicate), and the wave absorbing performance is lowered.
In a second aspect, the present invention provides a method for preparing a wave-absorbing coating by using the radar wave-absorbing material, the preparation method comprising the following specific steps:
firstly, weighing a strontium source, a lanthanum source and a silicon source in set amounts in proportion, adding absolute ethyl alcohol, and ball-milling at the speed of 200-350 r/min for 10-14 h at room temperature to obtain slurry;
specifically, the strontium source adopted by the invention is SrCO 3 Or Sr (NO) 3 ) 2 Lanthanum source Ln 2 O 3 、Ln 2 (CO 3 ) 3 Or Ln (NO) 3 ) 3 The silicon source is SiO 2 The addition amount of the absolute ethyl alcohol just floods the strontium source, the lanthanum source and the silicon source, wherein when Ln is used 2 O 3 Or Ln 2 (CO 3 ) 3 When the strontium source is used as the lanthanum source, the mole ratio of the strontium source, the lanthanum source and the silicon source is that: lanthanum source: silicon source= (2-x): x/2:1, a step of; when Ln (NO) 3 ) 3 When the strontium source is used as the lanthanum source, the mole ratio of the strontium source, the lanthanum source and the silicon source is that: lanthanum source: silicon source= (2-x): x:1.
step two, standing the slurry obtained in the step one for 6 to 8 hours, and drying at 80 ℃ for 30 minutes to obtain a dried material;
calcining the dried material obtained in the step II at 1200-1350 ℃ for 3-6 h, cooling, grinding and sieving to obtain Sr with the particle size of 40-90 μm after the calcining (2-x) Ln x SiO 4 Powder, namely radar wave-absorbing material;
fourthly, using a plasma spraying technology to spray the Sr obtained in the third step (2-x) Ln x SiO 4 Powder spraying on high-temperature alloy base materialForming a semi-cured wave-absorbing coating on the surface;
specifically, before spraying, the metal substrate is firstly subjected to sand blasting and cleaning treatment, and during spraying, argon and nitrogen are used as working gases, and related parameters are set as follows: argon flow is 30L/min-40L/min, nitrogen flow is 5L/min-10L/min, spraying voltage is 30V-32V, spraying current is 200A-240A, spraying distance is 80 mm-120 mm, air carrying capacity is 5L/min-8L/min, powder feeding rate is 50 g/min-100 g/min, and spraying angle is 90 degrees;
step five, finally placing the wave-absorbing coating which is half-cured in the step four at 900-1000 ℃ for calcination for 4-6 hours to obtain the cured wave-absorbing coating; the thickness of the cured wave-absorbing coating is generally set to be 1.10 mm-1.55 mm.
To illustrate the efficacy of the radar absorbing material of the present invention in a coating, the inventors have performed the following specific examples for verification:
example 1
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) La x SiO 4 The raw material SiO is weighed according to the mol ratio of 1:2 at room temperature, wherein x=0 2 And SrCO 3 Adding absolute ethyl alcohol, and ball-milling for 14 hours at the speed of 200r/min at room temperature to obtain slurry; standing the slurry for 6 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200 ℃ for 6 hours to obtain Sr 2 SiO 4 Cooling, grinding and sieving to obtain Sr 2 SiO 4 Powder of Sr 2 SiO 4 The particle size of the powder was 40. Mu.m.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 2 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
in particular, argon and nitrogen are used as working gases in the plasma spraying process to protect Sr 2 SiO 4 The powder will not oxidize and the coating will be produced with less impurities. The relevant parameters are set as follows: argon flow is 30L/min, nitrogen flow is 5L/min, and spraying is carried outThe voltage is 30V, the spraying current is 200A, the spraying distance is 80mm, the air carrying capacity is 5L/min, the powder feeding speed is 50g/min, and the spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 900 ℃ for 6 hours to obtain the cured wave-absorbing coating with the thickness of 1.55mm.
Example 2
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) La x SiO 4 X=0.2, and the raw material SiO was weighed at room temperature in a molar ratio of 10:18:1 2 、SrCO 3 And La (La) 2 O 3 Adding absolute ethyl alcohol, and ball-milling for 12 hours at the speed of 300r/min at room temperature to obtain slurry; standing the slurry for 7 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200deg.C for 6 hr, cooling, grinding, and sieving to obtain Sr with particle diameter of 50 μm 1.8 La 0.2 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 1.8 La 0.2 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: the argon flow is 35L/min, the nitrogen flow is 8L/min, the spraying voltage is 31V, the spraying current is 220A, the spraying distance is 100mm, the gas carrying capacity is 6L/min, the powder feeding rate is 80g/min, and the spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 950 ℃ for 5.5 hours to obtain the cured wave-absorbing coating with the thickness of 1.55mm.
Example 3
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) La x SiO 4 X=0.4 in (a), and the raw material SiO is weighed according to the mol ratio of 10:16:2 at room temperature 2 、SrCO 3 And La (La) 2 O 3 Adding absolute ethyl alcohol, ball milling for 10h at the speed of 350r/min at room temperature to obtain slurryMaterial preparation; standing the slurry for 8 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200deg.C for 6 hr, cooling, grinding, and sieving to obtain Sr with particle diameter of 60 μm 1.6 La 0.4 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 1.6 La 0.4 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: argon flow is 40L/min, nitrogen flow is 10L/min, spraying voltage is 32V, spraying current is 240A, spraying distance is 120mm, air carrying capacity is 8L/min, powder feeding rate is 100g/min, and spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 1000 ℃ for 4 hours to obtain the cured wave-absorbing coating with the thickness of 1.55mm.
Example 4
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) La x SiO 4 X=0.6 in (a), and the raw material SiO is weighed according to the mol ratio of 10:14:3 at room temperature 2 、SrCO 3 And La (La) 2 O 3 Adding absolute ethyl alcohol, and ball-milling for 12 hours at the speed of 300r/min at room temperature to obtain slurry; standing the slurry for 7 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200deg.C for 6 hr, cooling, grinding, and sieving to obtain Sr with particle diameter of 70 μm 1.4 La 0.6 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 1.4 La 0.6 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: the argon flow is 36L/min, the nitrogen flow is 9L/min, the spraying voltage is 31V, the spraying current is 230A, the spraying distance is 110mm, the air carrying capacity is 7L/min, the powder feeding rate is 90g/min, and the spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 900 ℃ for 6 hours to obtain the cured wave-absorbing coating with the thickness of 1.55mm.
Example 5
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) La x SiO 4 X=0.8, and the raw material SiO was weighed at room temperature in a molar ratio of 10:12:4 2 、Sr(NO 3 ) 2 And La (La) 2 O 3 Adding absolute ethyl alcohol, and ball-milling for 14 hours at the speed of 250r/min at room temperature to obtain slurry; standing the slurry for 7 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1300deg.C for 5 hr, cooling, grinding, and sieving to obtain Sr with particle diameter of 80 μm 1.2 La 0.8 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 1.4 La 0.6 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: the argon flow is 35L/min, the nitrogen flow is 8L/min, the spraying voltage is 31V, the spraying current is 220A, the spraying distance is 100mm, the gas carrying capacity is 6L/min, the powder feeding rate is 80g/min, and the spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 900 ℃ for 6 hours to obtain the cured wave-absorbing coating with the thickness of 1.55mm.
Example 6
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) La x SiO 4 X=1.0 in (a), and the raw material SiO is weighed according to the molar ratio of 10:10:5 at room temperature 2 、Sr(NO 3 ) 2 And La (La) 2 O 3 Adding absolute ethyl alcohol, and ball-milling for 12 hours at the speed of 300r/min at room temperature to obtain slurry; after ball milling, the slurry is kept stand for 7 hours and then is placed at 80 DEG CDrying for 30min to obtain dried material; calcining the dried material at 1350 ℃ for 3 hours, cooling, grinding and sieving to obtain SrLaSiO with the grain diameter of 90 μm 4 And (3) powder.
2) Using plasma spraying technology to spray SrLaSiO obtained in the step 1) 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: argon flow is 30L/min, nitrogen flow is 5L/min, spraying voltage is 30V, spraying current is 200A, spraying distance is 80mm, gas carrying capacity is 5L/min, powder feeding rate is 50g/min, and spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 900 ℃ for 6 hours to obtain the cured wave-absorbing coating with the thickness of 1.55mm.
Example 7
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) La x SiO 4 X=1.2 in (a), and the raw material SiO is weighed according to the mol ratio of 10:8:6 at room temperature 2 、SrCO 3 And La (La) 2 O 3 Adding absolute ethyl alcohol, and ball-milling for 10 hours at the speed of 200r/min at room temperature to obtain slurry; standing the slurry for 8 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200deg.C for 6 hr, cooling, grinding, and sieving to obtain Sr with particle diameter of 60 μm 0.8 La 1.2 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 0.8 La 1.2 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: argon flow is 40L/min, nitrogen flow is 10L/min, spraying voltage is 32V, spraying current is 240A, spraying distance is 120mm, air carrying capacity is 8L/min, powder feeding rate is 100g/min, and spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 1000 ℃ for 4 hours to obtain the cured wave-absorbing coating with the thickness of 1.55mm.
Example 8
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) La x SiO 4 X=1.4 in (a), and the raw material SiO was weighed at room temperature in a molar ratio of 10:6:7 2 、SrCO 3 And La (La) 2 O 3 Adding absolute ethyl alcohol, and ball-milling for 10 hours at the speed of 250r/min at room temperature to obtain slurry; standing the slurry for 8 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200deg.C for 6 hr, cooling, grinding, and sieving to obtain Sr with particle diameter of 60 μm 0.6 La 1.4 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 0.6 La 1.4 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: argon flow is 40L/min, nitrogen flow is 10L/min, spraying voltage is 32V, spraying current is 240A, spraying distance is 120mm, air carrying capacity is 8L/min, powder feeding rate is 100g/min, and spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 1000 ℃ for 4 hours to obtain the cured wave-absorbing coating with the thickness of 1.55mm.
Example 9
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) Dy x SiO 4 X=0.8, and the raw material SiO was weighed at room temperature in a molar ratio of 10:12:4 2 、Sr(NO 3 ) 2 And Dy 2 (CO 3 ) 3 Adding absolute ethyl alcohol, and ball-milling for 12 hours at the speed of 300r/min at room temperature to obtain slurry; standing the slurry for 7 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200 ℃ for 6 hours, and cooling,Grinding and sieving to obtain Sr with particle diameter of 80 μm 1.2 Dy 0.8 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 1.2 Dy 0.8 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: the argon flow is 35L/min, the nitrogen flow is 8L/min, the spraying voltage is 31V, the spraying current is 220A, the spraying distance is 100mm, the gas carrying capacity is 6L/min, the powder feeding rate is 80g/min, and the spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 900 ℃ for 6 hours to obtain the cured wave-absorbing coating with the thickness of 1.10 mm.
Example 10
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) Ce x SiO 4 X=0.8, and the raw material SiO was weighed at room temperature in a molar ratio of 10:12:4 2 、Sr(NO 3 ) 2 And Ce (Ce) 2 (CO 3 ) 3 Adding absolute ethyl alcohol, and ball-milling for 12 hours at the speed of 300r/min at room temperature to obtain slurry; standing the slurry for 7 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200deg.C for 6 hr, cooling, grinding, and sieving to obtain Sr with particle diameter of 80 μm 1.2 Ce 0.8 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 1.2 Ce 0.8 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: the argon flow is 35L/min, the nitrogen flow is 8L/min, the spraying voltage is 31V, the spraying current is 220A, the spraying distance is 100mm, the gas carrying capacity is 6L/min, the powder feeding rate is 80g/min, and the spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 900 ℃ for 6 hours to obtain the cured wave-absorbing coating with the thickness of 1.20 mm.
Example 11
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) Pr x SiO 4 X=0.8, and the raw material SiO was weighed at room temperature in a molar ratio of 10:12:8 2 、Sr(NO 3 ) 2 And Pr (NO) 3 ) 3 Adding absolute ethyl alcohol, and ball-milling for 12 hours at the speed of 350r/min at room temperature to obtain slurry; standing the slurry for 7 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200deg.C for 6 hr, cooling, grinding, and sieving to obtain Sr with particle diameter of 80 μm 1.2 Pr 0.8 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 1.2 Pr 0.8 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: the argon flow is 35L/min, the nitrogen flow is 8L/min, the spraying voltage is 31V, the spraying current is 220A, the spraying distance is 100mm, the gas carrying capacity is 6L/min, the powder feeding rate is 80g/min, and the spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 900 ℃ for 6 hours to obtain the cured wave-absorbing coating with the thickness of 1.30 mm.
Example 12
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) Sm x SiO 4 X=0.8, and the raw material SiO was weighed at room temperature in a molar ratio of 10:12:8 2 、SrCO 3 And Sm (NO) 3 ) 3 Adding absolute ethyl alcohol, and ball-milling for 12 hours at the speed of 300r/min at room temperature to obtain slurry; standing the slurry for 7 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200deg.C for 6 hr, cooling, grinding, and sieving to obtain powder with particle diameter of 80 μmm Sr 1.2 Sm 0.8 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 1.2 Sm 0.8 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: the argon flow is 35L/min, the nitrogen flow is 8L/min, the spraying voltage is 31V, the spraying current is 220A, the spraying distance is 100mm, the gas carrying capacity is 6L/min, the powder feeding rate is 80g/min, and the spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 900 ℃ for 6 hours to obtain the cured wave-absorbing coating with the thickness of 1.30 mm.
Example 13
The modified strontium silicate wave-absorbing coating is prepared according to the following steps
1) Let molecular formula Sr (2-x) Nd x SiO 4 X=0.8, and the raw material SiO was weighed at room temperature in a molar ratio of 10:12:8 2 、SrCO 3 And Nd (NO) 3 ) 3 Adding absolute ethyl alcohol, and ball-milling for 12 hours at the speed of 300r/min at room temperature to obtain slurry; standing the slurry for 7 hours after ball milling, and drying at 80 ℃ for 30 minutes to obtain a dried material; calcining the dried material at 1200deg.C for 6 hr, cooling, grinding, and sieving to obtain Sr with particle diameter of 80 μm 1.2 Nd 0.8 SiO 4 And (3) powder.
2) Using plasma spraying technology to spray the Sr obtained in the step 1) 1.2 Nd 0.8 SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
the relevant parameters used in the plasma spraying process are set as follows: the argon flow is 35L/min, the nitrogen flow is 8L/min, the spraying voltage is 31V, the spraying current is 220A, the spraying distance is 100mm, the gas carrying capacity is 6L/min, the powder feeding rate is 80g/min, and the spraying angle is 90 degrees.
3) And (3) calcining the semi-cured wave-absorbing coating obtained in the step (2) at 900 ℃ for 6 hours to obtain the cured wave-absorbing coating with the thickness of 1.30 mm.
Further, the inventors tested electromagnetic parameters of the wave-absorbing coatings prepared in examples 1 to 8 by a waveguide method, the used instrument model was Agilent Technologies E8362B vector network analyzer, the test frequency band range was 8GHz to 12GHz, the test temperature was room temperature and 900 ℃, and the test data are shown in table 1 below:
TABLE 1 Complex dielectric constant of each coating at room temperature and 900℃
In addition, the emissivity of the wave-absorbing coatings of examples 1 to 8 was tested by an arch method, the test frequency range was 8GHz to 12GHz, the test temperature was room temperature and 900 ℃, and the reflectivity of the test results was expressed in decibels (dB) as shown in the following Table 2:
TABLE 2 reflectivity of coatings at room temperature and 900℃
As can be seen from the data in tables 1 and 2 and the test experiments described above, the La-like effect 3+ The invention uses Sr to increase the doping amount (2-x) La x SiO 4 The imaginary part epsilon' of the complex dielectric constant of the coating formed by the powder material is gradually increased, and the radar reflectivity of the coating is gradually improved; but when La 3+ After the doping amount of the coating is increased to a certain value, the imaginary part of the complex dielectric constant of the coating becomes smaller along with the increase of the doping amount, and the radar reflectivity of the coating becomes worse; therefore La 3+ The doping amount of the material should be maintained within a certain range, and the excessive and the insufficient doping ratio can affect the wave absorbing performance of the material.
The foregoing is only a specific embodiment of the invention to enable those skilled in the art to understand or practice the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention.
It will be understood that the invention is not limited to what has been described above and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (6)
1. A method for preparing a wave-absorbing coating by using a radar wave-absorbing material, which comprises the following steps:
firstly, weighing a strontium source, a lanthanum source and a silicon source in set amounts in proportion, adding absolute ethyl alcohol, and ball-milling at the speed of 200-350 r/min for 10-14 h at room temperature to obtain slurry;
step two, standing the slurry obtained in the step one for 6 to 8 hours, and drying at 80 ℃ for 30 minutes to obtain a dried material;
calcining the dried material obtained in the step II at 1200-1350 ℃ for 3-6 h, cooling, grinding and sieving to obtain Sr after the calcining is finished (2-x) Ln x SiO 4 Powder, namely radar wave-absorbing material;
fourthly, using a plasma spraying technology to spray the Sr obtained in the third step （2-x） Ln x SiO 4 Powder spraying is carried out on the surface of the high-temperature alloy substrate to form a semi-cured wave-absorbing coating;
step five, finally placing the wave-absorbing coating which is half-cured in the step four at 900-1000 ℃ for calcination for 4-6 hours to obtain the cured wave-absorbing coating;
wherein the strontium source is SrCO 3 Or Sr (NO) 3 ) 2 Lanthanum source Ln 2 O 3 、Ln 2 (CO 3 ) 3 Or Ln (NO) 3 ) 3 The silicon source is SiO 2 ；
When Ln is used 2 O 3 Or Ln 2 (CO 3 ) 3 When used as lanthanum source, strontium source and lanthanum sourceAnd the molar ratio of the silicon source is that of the strontium source: lanthanum source: silicon source= (2-x): x/2:1, a step of;
when Ln (NO) 3 ) 3 When the strontium source is used as the lanthanum source, the mole ratio of the strontium source, the lanthanum source and the silicon source is that: lanthanum source: silicon source= (2-x): x:1, a step of;
the Sr is (2-x) Ln x SiO 4 Ln is any lanthanoid element, and the doping amount x=0.4 to 1.0.
2. The method for preparing a wave-absorbing coating using a radar absorbing material according to claim 1, wherein the doping amount x=0.6 to 1.0.
3. The method for preparing a wave-absorbing coating by using a radar wave-absorbing material according to claim 1, wherein the Sr is obtained after sieving in the third step (2-x) Ln x SiO 4 The particle size of the powder is 40-90 mu m so as to be used for plasma spraying operation.
4. The method for preparing a wave-absorbing coating by using a radar wave-absorbing material according to claim 1, wherein argon and nitrogen are used as working gases during the plasma spraying in the fourth step, and parameters are set as follows: argon flow is 30L/min-40L/min, nitrogen flow is 5L/min-10L/min, spraying voltage is 30V-32V, spraying current is 200A-240A, spraying distance is 80 mm-120 mm, air carrying capacity is 5L/min-8L/min, powder feeding rate is 50 g/min-100 g/min, and spraying angle is 90 degrees.
5. The method for preparing a wave-absorbing coating by using a radar absorbing material according to claim 1, wherein the thickness of the wave-absorbing coating after curing in the fifth step is 1.10 mm-1.55 mm.
6. Use of a method according to any one of claims 1 to 5, characterized in that the wave-absorbing coating obtained with the method is used for radar camouflage.
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| CN102105043A (en) * | 2010-12-15 | 2011-06-22 | 电子科技大学 | High temperature-resisting electromagnetic wave absorbing material and preparation method thereof |
| CN102718576A (en) * | 2012-06-28 | 2012-10-10 | 中国人民解放军国防科学技术大学 | Radar wave absorbing ceramic with capacitive cycle structure and preparation method thereof |
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| CN112680691A (en) * | 2020-12-24 | 2021-04-20 | 中国人民解放军国防科技大学 | High-temperature radar wave-absorbing coating based on disordered electromagnetic periodic structure and preparation method thereof |
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| CN102105043A (en) * | 2010-12-15 | 2011-06-22 | 电子科技大学 | High temperature-resisting electromagnetic wave absorbing material and preparation method thereof |
| CN102718576A (en) * | 2012-06-28 | 2012-10-10 | 中国人民解放军国防科学技术大学 | Radar wave absorbing ceramic with capacitive cycle structure and preparation method thereof |
| CN108060384A (en) * | 2017-12-12 | 2018-05-22 | 中国航发沈阳黎明航空发动机有限责任公司 | A kind of double ceramic layer thermal barrier coating systems and its composite-making process |
| CN112680691A (en) * | 2020-12-24 | 2021-04-20 | 中国人民解放军国防科技大学 | High-temperature radar wave-absorbing coating based on disordered electromagnetic periodic structure and preparation method thereof |
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