Preparation method of multi-spectrum interference agent based on new electronic interference material

Abstract

The invention discloses a preparation method of a multi-spectrum interference agent based on a new electronic interference material, and relates to the technical field of photoelectric countermeasure and interference. The method mainly comprises the following steps: step 1, putting expanded graphite (with the length of 2-6 mm and the particle size of 300-500 microns) and short carbon fibers (with the length of 1-5 mm and the particle size of 2-8 microns) in a stirring container according to a mass ratio of 1: 1; step 2, taking a new electronic interference material with the same mass as the chopped carbon fiber and the expanded graphite, and putting the new electronic interference material into a stirring container; 3, stirring for 1-2 hours by using a direct-current stirrer until the materials in the stirring container are completely and uniformly mixed, putting into a vacuum drying box, and performing vacuum drying for 12-24 hours at the temperature of 60-80 DEG C, so as to obtain the multi-spectrum interference agent; and 4, placing the multi-spectrum interference agent in a sealing bag, and introducing nitrogen for storage so as to carry out subsequent electromagnetic shielding performance test on the multi-spectrum interference agent in the smoke box. The method has the advantages that the effect of multi-spectrum interference is high, pollution is avoided, and cost is reduced.

Description

Technical Field

[0001] The present invention relates to the field of photoelectric countermeasures and interference, and in particular to a method for preparing a multi-spectrum interference agent based on a new electronic interference material. Background Art

[0002] As an effective passive jamming method, smoke screens play a vital role in optoelectronic countermeasures and interference. Their basic principle is to exploit the material's reflection, absorption, scattering, and refraction properties to achieve electromagnetic wave attenuation. In modern warfare, the combination of guidance systems and the coordinated jamming of multiple modules are driving increasing demands for smoke screens with full-band jamming capabilities. Electromagnetic shielding materials such as expanded graphite and chopped carbon fiber are low-cost, industrially producible carbon materials and are widely used in smoke screens. However, these materials generally only provide millimeter-wave interference, resulting in poor results. Improvements to existing jamming materials are needed. Summary of the Invention

[0003] The purpose of the present invention is to integrate the new electronic jamming material developed by our company, which has good shielding performance for visible light and near, medium and far infrared light, with existing millimeter wave jamming carbon materials in different ways, to achieve the preparation of multi-spectrum jammers formed by mixing expanded graphite, chopped carbon fiber and the new electronic jamming material, and to use a smoke box to test the electromagnetic shielding performance of the multi-spectrum jammer, and finally select the best fusion scheme.

[0004] To achieve the above-mentioned purpose, the present invention adopts the following technical solution: The present invention provides a method for preparing a multi-spectrum interfering agent based on a new electronic interference material, comprising the following steps:

[0005] Step 1: Place expanded graphite (length 2-6 mm, particle size 300-500 μm) and chopped carbon fibers (length 1-5 mm, particle size 2-8 μm) in a stirring container at a mass ratio of 1:1;

[0006] Step 2: Take the same mass of new electronic interference material as expanded graphite and chopped carbon fiber and place it in a stirring container;

[0007] Step 3: Stirring the mixture using a DC stirrer for 1-2 hours until the materials in the stirring container are completely mixed, placing the mixture in a vacuum drying oven and vacuum drying the mixture at 60° C. to 80° C. for 12 to 24 hours to obtain a multi-spectrum interfering agent;

[0008] Step 4: Place the multi-spectrum jammer in a sealed bag and store it in nitrogen, pending subsequent electromagnetic shielding performance testing in a smoke box.

[0009] Preferably, anhydrous ethanol (concentration 99.5%) having the same volume as that of the three materials after mixing is added into the stirring container in step 2 as a dispersing solvent.

[0010] Preferably, after the materials are evenly mixed in step 3, the stirrer is placed in a forced air drying oven and the temperature is set at 60° C. to 80° C. to evaporate the ethanol to obtain a multi-spectrum interfering agent.

[0011] Preferably, the method of adding the new electronic interference material in step 2 is adjusted, specifically comprising the following steps:

[0012] (1) adding copper salt and water into the stirring container, dissolving the copper salt in the water, and continuously stirring and mixing using a stirrer, wherein the stirring paddle is made of polytetrafluoroethylene;

[0013] (2) Nucleation process: adding sodium hydroxide solution to the copper salt solution doped with the mixed material, stirring at 0-80°C to obtain a mixed flocculent precipitate A; adding a green reducing agent solution to the mixed flocculent precipitate A to obtain a precipitate B;

[0014] (3) Sulfurization process: adding a sulfur source to the precipitate B and mechanically stirring at room temperature for 1 to 4 hours to obtain a mixed precipitate C;

[0015] (4) Oxidation process: adding a strong oxidant solution to the precipitate C and mechanically stirring for 2 to 8 hours to obtain a suspension; filtering the suspension to obtain a mixed precipitate D, which is a mixture of expanded graphite, chopped carbon fibers, and a new electronic interference material;

[0016] (5) The mixed precipitate D is washed and dried. The washing process is to alternately wash with ultrapure water and anhydrous ethanol for 1 to 10 times.

[0017] Compared with the prior art, the present invention has the following beneficial effects: (1) in the preparation method of the multi-spectrum interfering agent of the present invention, expanded graphite and chopped carbon fiber are both materials with millimeter wave interference performance, and can achieve the effect of multi-spectrum interference by homogeneously mixing with the new electronic interference material with good visible light and infrared shielding effects; (2) in the preparation method of the multi-spectrum interfering agent of the present invention, expanded graphite and chopped carbon fiber themselves have certain fluidity and air retention, and the multi-spectrum interfering agent does not need to be added with additional fluidity; (3) in the preparation method of the multi-spectrum interfering agent of the present invention, the prepared multi-spectrum interfering agent does not pollute the environment; (4) in the preparation method of the multi-spectrum interfering agent of the present invention, the mixing ratio of copper sulfide in the mixed multi-spectrum interfering agent is reduced, which can greatly reduce the cost; (5) the present invention intends to compare the electromagnetic shielding performance of the multi-spectrum interfering agent prepared by three schemes to select the best scheme, and conduct pilot test and subsequent scale-up production based on existing production conditions; (6) in the preparation method of the multi-spectrum interfering agent of the present invention, anhydrous ethanol as a good mixed dispersion system can be extended to the homogeneous mixing of more single-action photoelectric interference materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 Schematic diagram of the smoke box.

[0019] Figure 2 This is the smoke box test result of Scheme 1.

[0020] Figure 3 This is the smoke box test result of Scheme 2.

[0021] Figure 4 This is the smoke box test result of Scheme 3. DETAILED DESCRIPTION

[0022] In order to enable those skilled in the art to better understand the present invention, the following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts should fall within the scope of protection of this application.

[0023] A patent for new electronic interference materials (application number ZL2024102005041) has been applied for and is awaiting publication, disclosing the manufacturing method. Expanded graphite (length 2-6mm, particle size 300-500μm) and chopped carbon fiber (length 1-5mm, particle size 2-8μm) can be purchased from JD.com.

[0024] Example:

[0025] Option 1: The mixing container is selected with a volume of 1m 3 An industrial continuous mixer or an industrial-grade mixing tank is used to take expanded graphite, chopped carbon fiber and new electronic interference material in a mass ratio of 1:1:1 and place them in a stirring container. 10 kg of each material is taken and stirred for 1-2 hours using a stainless steel DC stirrer until the three materials are completely mixed (the speed is set to 50-150 rpm). The mixed material is placed in a vacuum drying oven and vacuum-dried at 60°C to 80°C for 12 to 24 hours to obtain a multi-spectrum interfering agent. The multi-spectrum interfering agent is taken out and poured into a sealed bag for storage under nitrogen, pending subsequent electromagnetic shielding performance testing of the multi-spectrum interfering agent in a smoke box.

[0026] Option 2:

[0027] The mixing container is selected with a volume of 1m 3An industrial continuous mixer or an industrial-grade mixing tank is used. Expanded graphite, chopped carbon fiber and new electronic interference materials in a mass ratio of 1:1:1 are placed in a stirring container. 10 kg of each are taken, and anhydrous ethanol (concentration 99.5%) with a volume of 500-800 L is added as a dispersing solvent. A stainless steel DC stirrer is used to stir for 1-2 hours until the three materials are completely mixed (the speed is set to 50-150 rpm). The mixed material in the stirring container is then placed in a blast drying oven and set at a temperature of 60°C to 80°C to evaporate the ethanol. The mixed material is placed in a vacuum drying oven and vacuum-dried at 60°C to 80°C for 12 to 24 hours to obtain a multi-spectrum interfering agent. The multi-spectrum interfering agent is taken out and poured into a sealed bag for storage with nitrogen, pending subsequent electromagnetic shielding performance testing of the multi-spectrum interfering agent in a smoke box.

[0028] Option 3:

[0029] (1) The mixing container is selected with a volume of 1m 3 An industrial continuous mixer or an industrial-grade mixing tank is used, specifically, copper salt and water are added to the inside of the stirring container, the copper salt is dissolved in water, and expanded graphite and chopped carbon fibers are added to the copper salt solution at a mass ratio of 1:1 and placed in the stirring container. The mass of the expanded graphite and the chopped carbon fibers are 10 kg respectively. The process requires continuous stirring with a stirrer (speed 50-150 rpm), and the stirring paddle is made of polytetrafluoroethylene;

[0030] (2) Nucleation process: adding sodium hydroxide solution to the copper salt solution doped with the mixed material, stirring at 0-80°C to obtain a mixed flocculent precipitate A; adding a green reducing agent solution to the mixed flocculent precipitate A to obtain a precipitate B;

[0031] The copper salts include Cu(NO3)2·3H2O, CuCl2·2H2O, Cu(CH3COO)2·H2O and CuSO4, the concentration of the copper salts is 0.01-5 mol / L, and the concentration of the sodium hydroxide solution is 2-8 mol / L; the green reducing agent solution includes glucose, ascorbic acid, hydrazine hydrate and sodium borohydride, and the concentration of the green reducing agent solution is 0.7-1.2 mol / L.

[0032] (3) Sulfurization process: adding a sulfur source to the precipitate B and mechanically stirring at room temperature for 1 to 4 hours to obtain a mixed precipitate C;

[0033] The sulfur source includes a mixture of one or more of sodium sulfide, sodium hydrosulfide, sodium thiosulfate, and thiourea solution, with a concentration of 0.1 to 0.5 mol / L.

[0034] (4) Oxidation process: adding a strong oxidant solution to the precipitate C and mechanically stirring for 2 to 8 hours to obtain a suspension; filtering the suspension to obtain a mixed precipitate D, which is a mixture of expanded graphite, chopped carbon fibers, and a new electronic interference material;

[0035] The strong oxidant solution is one or more combinations of sulfuric acid, hydrochloric acid, nitric acid, acetic acid, and hydrogen peroxide; the stirring speed is 50 to 150 revolutions per minute, the stirring time is 1 to 4 hours, and the filtration accuracy is 0.05 to 10 microns.

[0036] (5) The mixed precipitate D is washed and dried. The washing process is to alternately wash with ultrapure water and anhydrous ethanol for 1 to 10 times, and finally vacuum-dry for 12 to 24 hours. The temperature of the vacuum drying oven is set at 60°C to 80°C. The dried sample is ground into fine powder to obtain a multi-spectral interfering agent.

[0037] The specific steps for testing visible light, infrared, and millimeter wave interference in a smoke box (3m×7m×3m) are as follows:

[0038] S1: Turn on the constant temperature and humidity air conditioner to keep the smoke box space at a constant temperature and humidity;

[0039] S2: Turn on the light source, blackbody, spectrometer, and infrared thermal imager, wait for the data to stabilize, and record the target and background grayscale values of each detector before the smoke screen is released;

[0040] S3: Turn on the smoke spraying equipment, spray the smoke screen into the smoke box and turn on the stirring fan at the same time. After the spraying is completed, let the fan run for 10 seconds and then turn off the stirring fan.

[0041] S4: Turn on the air concentration sampler to take samples and record the changes in the grayscale value of each detector after spraying the smoke screen.

[0042] like Figure 2 As shown, the multi-spectrum jammer prepared by Scheme 1 has an attenuation value of -12.58dB and -10.34dB at 3mm and 8mm waves.

[0043] like Figure 3 As shown, the attenuation values at 3mm and 8mm waves can reach -14.24dB and -11.28dB.

[0044] like Figure 4 As shown, the attenuation values at 3mm and 8mm waves can reach -11.38dB and -9.12dB.

[0045] From the above, it can be seen that the performance of the multi-spectrum interfering agent prepared by Scheme 2 is optimal, and a specific scheme can also be selected according to actual needs.

[0046] Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for preparing a multi-spectrum interfering agent based on a new electronic interference material, characterized in that: The following steps are involved: Step 1: Place expanded graphite (length 2-6 mm, particle size 300-500 μm) and chopped carbon fiber (length 1-5 mm, particle size 2-8 μm) in a stirring container at a mass ratio of 1:1; Step 2: Take the same mass of new electronic interference material as chopped carbon fiber and expanded graphite into a stirring container; Step 3: Stirring the mixture using a DC stirrer for 1-2 hours until the materials in the stirring container are completely mixed, and then placing the mixture in a vacuum drying oven at 60° C. to 80° C. for 12 to 24 hours to obtain a multi-spectrum interfering agent; Step 4: Place the mixed multi-spectrum interfering agent in a sealed bag and store it in nitrogen gas, pending subsequent electromagnetic shielding performance testing of the multi-spectrum interfering agent in a smoke box.

2. The method for preparing a multi-spectrum interfering agent based on a new electronic interference material according to claim 1, characterized in that: Anhydrous ethanol (99.5% concentration) having the same volume as that of the three materials after mixing was added into the stirring container in step 2 as a dispersing solvent.

3. The method for preparing a multi-spectrum interfering agent based on a new electronic interference material according to claim 2, characterized in that: After the materials are evenly mixed in step 3, the stirrer is placed in a forced air drying oven and the temperature is set at 60° C. to 80° C. to evaporate the ethanol and obtain a multi-spectrum interfering agent.

4. The method for preparing a multi-spectrum interfering agent based on a new electronic interference material according to claim 1, characterized in that: The method of adding the new electronic interference material in step 2 is adjusted, specifically comprising the following steps: (1) adding copper salt and water into the stirring container, dissolving the copper salt in the water, and continuously stirring and mixing using a stirrer, wherein the stirring paddle is made of polytetrafluoroethylene; (2) Nucleation process: adding sodium hydroxide solution to the copper salt solution doped with the mixed material, stirring at 0-80°C to obtain a mixed flocculent precipitate A; adding a green reducing agent solution to the mixed flocculent precipitate A to obtain a precipitate B; (3) Sulfurization process: adding a sulfur source to the precipitate B and mechanically stirring at room temperature for 1 to 4 hours to obtain a mixed precipitate C; (4) Oxidation process: adding a strong oxidant solution to the precipitate C and mechanically stirring for 2 to 8 hours to obtain a suspension; filtering the suspension to obtain a mixed precipitate D, which is a mixture of expanded graphite, chopped carbon fibers, and a new electronic interference material; (5) The mixed precipitate D is washed and dried. The washing process is to alternately wash with ultrapure water and anhydrous ethanol for 1 to 10 times.

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