NL2033030A - Preparation method of novel three-dimensional ferrite foam wave-absorbing material - Google Patents
Preparation method of novel three-dimensional ferrite foam wave-absorbing material Download PDFInfo
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Abstract
The invention. provides a preparation. method, of a novel three— dimensional ferrite foam wave—absorbing material, and relates to the technical field of inorganic wave—absorbing material preparation. The preparation method of the novel three—dimensional 5 ferrite foam wave—absorbing material comprises the following steps: Sl. Accurately weighing a certain amount of ferric nitrate, divalent transition metal nitrate and a certain amount of reducing agent, sequentially dissolving the ferric nitrate, the divalent transition metal nitrate and the reducing agent in deionized 10 water, and uniformly stirring to obtain binary metal mixed solution; SZ. Dripping ammonia water into the binary metal mixed solution in a stirring state, adjusting the pH value of the obtained solution to about 7, and continuously stirring to obtain uniform sol. According to the method, the three—dimensional l5 ferrite wave—absorbing material with the special curled two— dimensional porous surface is rapidly prepared by a sol—gel self— propagating combustion method. (+ Fig. l) 20
Description
P1590 /NLpd PREPARATION METHOD OF NOVEL THREE-DIMENSIONAL FERRITE FOAM WAVE-
ABSORBING MATERIAL Technical field The invention relates to the technical field of preparation of inorganic wave-absorbing materials, in particular to a prepara- tion method of a novel three-dimensional ferrite foam wave- absorbing material.
Background Technology With the progress of the times, wireless communication tech- nology plays a more and more important role in military and civil- ian use. In modern military warfare, the rapid transmission and accurate grasp of battlefield information is very important, and wireless communication can maintain confidentiality and real-time. In civil use, the popularity of electronic equipment also repre- sents the maturity of wireless communication technology. However, the problem of electromagnetic pollution is becoming more and more serious. The root cause of electromagnetic pollution is that elec- tronic equipment radiates electromagnetic waves of different fre- quency bands during operation. The human body is affected by high- intensity electromagnetic waves for a long time, which will cause certain damage to the body organs. In addition, electromagnetic waves will affect some valuable instruments with high precision, resulting in serious consequences. Therefore, it is imperative to develop a new type of electromagnetic wave absorption material with light weight, thin thickness, wide frequency band and strong absorption.
Ferrite is one of the earliest classical microwave absorbing materials, which has been widely used because of its good imped- ance matching, good stability and high magnetic loss. However, the microwave absorbing properties and applications of ferrite are greatly limited due to its disadvantages such as high density and easy magnetic agglomeration. Therefore, the existing work usually combines it with carbon materials to achieve the purpose of reduc- ing density and overcoming magnetic agglomeration, and the syner-
gistic effect of the two components can improve the absorbing properties of the materials. However, the preparation of composite materials mostly requires tedious operation steps, and the materi- al composite can not essentially solve the problems of high densi- ty and easy agglomeration of ferrite. In addition, most of the current synthesis methods of ferrite absorbing materials (hydro- thermal synthesis method, sclvothermal method, adsorption calcina- tion method) also have the disadvantages of complex operation, long experimental cycle and high energy consumption.
Aiming at the problems, the invention adopts a simple and en- ergy-saving sol-gel self-propagating combustion method to synthe- size the foamy ferrite. The three-dimensional foam structure re- duces the density of the ferrite on one hand, and overcomes the disadvantage of magnetic agglomeration of the material on the oth- er hand. The existence of a large number of pores improves the im- pedance matching characteristics of the material, thereby greatly improving the microwave absorption performance of the ferrite. Compared with the existing ferrite-based composite material, the composite material has the advantages of being lighter and wider in wave-absorbing frequency band, and the method is simple and easy to operate, short in preparation period and good in applica- tion prospect.
After searching, Existing patents (publication numbers: CN107365567A, CN109936974A, CN109233741A, CN1140445414, CN107010675A, CN102604395A, CN114560506A, CN105268997a and the like respectively disclose a preparation method of a ferrite-based composite wave-absorbing material. The disclosed method has the problems of complicated preparation process, long preparation pe- riod, high cost and the like, and the patents in the field of cheap pure ferrite wave-absorbing materials are relatively few. Therefore, those skilled in the art provide a preparation method of a novel three-dimensional ferrite foam wave-absorbing material to solve the problems raised in the background art.
Summary of the invention (=) Solved technical problems Aiming at the defects of the prior art, the invention pro- vides a preparation method of a novel three-dimensional ferrite foam wave-absorbing material; the method is simple in process, short in period, low in requirements on production equipment and easy for industrial production; and the prepared three-dimensional wave-absorbing material has the advantages of light weight, good wave-absorbing performance and the like. (Z) Technical proposal In order to realize the purpose, the invention is realized by the following technical scheme: The invention relates to a preparation method of a novel three-dimensional ferrite foam wave-absorbing material, which com- prises the following steps: S1. Accurately weighing a certain amount of ferric nitrate, divalent transition metal nitrate and a certain amount of reducing agent, sequentially dissolving the ferric nitrate, the divalent transition metal nitrate and the reducing agent in deionized wa- ter, and uniformly stirring to obtain binary metal mixed solution; S2. Dripping ammonia water into the binary metal mixed solu- tion in a stirring state, adjusting the pH value of the obtained solution to about 7, and continuously stirring to obtain uniform sol;
33. Putting the obtained sol into an oven, and drying to ob- tain xerogel; S4. And placing the obtained xerogel in a preheated muffle furnace to ignite, and naturally cooling to room temperature after combustion to obtain the three-dimensional ferrite wave-absorbing material.
Preferably, the molar ratio of ferric nitrate to divalent transition metal nitrate in step S81 is 2:1.
Preferably, the ratio of the amount of the reducing agent to the amount of the ferric nitrate in step S1 is 0.3-1.5.
Preferably, the divalent transition metal nitrate in the step Sl includes cobalt nitrate, copper nitrate, nickel nitrate, zinc nitrate and the like.
Preferably, the reducing agent in step Sl comprises one or more of citric acid, glycine, urea and thiourea.
Preferably, the oven temperature in the step S3 does not ex- ceed 95 deg C.
Preferably, the ignition temperature of the combustion reac- tion in the muffle furnace in step S4 is 200-400 ° C.
Preferably, in the step S2, ammonia water is dripped into the solution with the assistance of a pH meter.
(ZE) Beneficial effect The invention provides a preparation method of a novel three- dimensional ferrite foam wave-absorbing material. Has the follow- ing beneficial effects:
1. The invention provides a method for preparing a novel three- dimensional ferrite foam wave-absorbing material.in the method, a three-dimensional ferrite wave-absorbing material with a special curly two-dimensional porous surface is quickly prepared by a sol- gel self-propagating combustion method; and the prepared ferrite wave-absorbing material is regular in appearance, overcomes the problem that the two-dimensional material is easy to agglomerate due to a three-dimensional structure, and is lighter.
2, The invention provides a preparation method of a novel three-dimensional ferrite foam wave-absorbing material; the mate- rial has the advantages of simple preparation process, cheap and easily available raw materials, short production period, low re- quirements on production equipment and easy industrial production; and the prepared three-dimensional ferrite wave-absorbing material has excellent wave-absorbing performance and good application pro- spect in the field of wave-absorbing materials.
3. The invention provides a method for preparing a novel three- dimensional ferrite foam wave-absorbing material.in the method, the shape of the wave-absorbing material is controlled by adjust- ing the proportion of a fuel to prepare the three-dimensional fer- rite wave-absorbing material with curled two-dimensional porous surfaces, The raw materials used are cheap and easy to obtain, and have the potential of industrialization.
Description of the drawings Fig. 1 is an X-ray diffraction pattern, a scanning electron micrograph, and a microwave absorbing performance graph of a sam- ple prepared in Example 1 of the present invention; Fig. 2 is an X-ray diffraction pattern, a scanning electron micrograph, and a microwave absorbing performance graph of a sam- ple prepared in Example 2 of the present invention; Fig. 3 is a scanning electron micrograph and a wave absorbing performance graph of a sample prepared in a third embodiment of 5 the present invention; Fig. 4 is a scanning electron micrograph and a wave absorbing performance graph of the sample prepared in Example 4 of the pre- sent invention.
Description of the invention In the following, the technical solutions of the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only a part of embodiments, but not all embodiments. Based on the embodiments of the present invention, all other embodiments ob- tained by those of ordinary skill in the art without creative work belong to the scope of protection of the present invention.
Example 1 As shown in Figure 1, the embodiment of the invention pro- vides a preparation method of a novel three-dimensional ferrite foam wave-absorbing material, which comprises the following steps: S1. 4.0402 G of Fe (NO(33. 9H:)0O and 1.4552 G of Co (NO:)). GH:0 were accurately weigh according to that stoichiometric ratio and adde to 50 mL of distilled water, Accurately weigh 1.0507 G of citric acid and add it to the above solution, and stir until it is completely dissolved; S2. Dripping ammonia water into the solution under the assis- tance of a pH meter, adjusting the pH value of the solution to about 7, and continuously stirring to obtain uniform sol; S3. The obtained sol was kept in an oven at 95 °C for 6 H, and dried to obtain xerogel.
S4. The dried gel is put into a muffle furnace which is pre- heated at the temperature of 200 deg C to be ignited, and the loose three-dimensional ferrite foam structure wave absorbing ma- terial is obtained after the combustion is finished.
Fig. 1 (a) shows the X-ray diffraction pattern of the pre- pared sample. All the diffraction peaks are sharp and consistent with the spinel structure CoFe204 (JCPDS No.22-1086}, indicating that CoFe204 has a complete crystal form and good crystallinity.
(B) is a scanning electron micrograph of the synthetic ab- sorbing material of this example. It can be seen from this figure that CoFe204 is a three-dimensional structure consisting of a curled two-dimensional porous surface.
(C) shows that a vector network analyzer (VNA, Agilent N5230a, USA) was used to test the absorbing properties of the ab- sorbing material prepared according to the present invention. The peak value of reflection loss is -23.6 dB in the range of 2-18 GHz. When the thickness is 2.1 mm, the effective bandwidth of RL < -10 dB is 7.28 GHz (10.72-18 GHz), which can effectively absorb electromagnetic waves in this band.
Example 2 As shown in fig. 2, the embodiment of the present invention provides a method for preparing a novel three-dimensional ferrite foam wave-absorbing material, which comprises the following steps: S1. 4.0402 G of Fe (NO(33: 9H:))0 and 1.2080 G of Cu (NO:))).)O - 3H;)0) were accurately weighed stoichiometrically and added to 50 mL of distilled water. Accurately weigh 0.0634 G of citric acid and add it into the above solution, and stir until it is complete- ly dissolved; S2. Dripping ammonia water into the solution under the assis- tance of a pH meter, adjusting the pH value of the solution to about 7, and continuously stirring to obtain uniform sol; S3. The obtained sol was kept in an oven at 95 °C for 6 H, and dried to obtain xerogel.
S4. The dried gel is put into a preheated muffle furnace at the temperature of 300 deg C to be ignited, and after the combus- tion is finished, the loose three-dimensional ferrite foam struc- ture wave absorbing material is obtained.
Fig. 2 {a) shows the X-ray diffraction pattern of the pre- pared sample. All the diffraction peaks are sharp and consistent with the spinel structure CuFe,0,JCPDS No.25-0283), indicating that CuFe;0 has a complete crystal form and good crystallinity.
(B) is a scanning electron micrograph of the synthetic ab- sorbing material of this example. It can be seen from this figure that CuFe,0,is a three-dimensional structure composed of a curled two-dimensional porous surface.
(C) Absorbing property. The peak value of reflection loss is -48.8 dB in the range of 2-18 GHz. When the thickness is 1. 7 mm, the effective bandwidth of RL < -10 dB is 6. 32 GHz (10. 00-16. 32 GHz), which can effectively absorb electromagnetic waves in this band.
Example 3 As shown in fig. 3, the embodiment of the present invention provides a method for preparing a novel three-dimensional ferrite foam wave-absorbing material, which comprises the following steps: S1. 4.0402 G of Fe (NO(33;.%9HO and 1.4540 G of Ni (NO52)).6H53) O were accurately weighed stoichiometrically and added to 50 mL of deionized water. Accurately weigh 1.1261 G of glycine and add it into the above solution, and stir it until it is completely dis- solved; S2. Dripping ammonia water into the solution under the assis- tance of a pH meter, adjusting the pH value of the solution to about 7, and continuously stirring to obtain uniform sol; S3. The obtained sol was kept in an oven at 95 °C for 6 H to obtain a xerogel.
S4. The dried gel is put into a preheated muffle furnace at the temperature of 400 deg C to be ignited, and after the combus- tion is finished, the loose three-dimensional ferrite foam struc- ture wave absorbing material is obtained.
Fig. 3 (a) is a scanning electron micrograph of the prepared sample. It can be seen from this figure that NiFe204 is a three- dimensional structure consisting of a curled two-dimensional po- rous surface.
(B) Absorbing property. In the range of 2-18 GHz, the peak value of reflection loss is -47.1 dB. When the thickness is 2. 9 mm, the effective bandwidth of RL < -10 dB is 4. 02 GHz (9. 10-13. 12 GHz), which can effectively absorb electromagnetic waves in this band.
Example 4 As shown in fig. 4, the embodiment of the present invention provides a method for preparing a novel three-dimensional ferrite foam wave-absorbing material, which comprises the following steps: S1. 4.0402g of Fe (NO(»:;.9HO and 1.4875g of Zn (NO52)).6H53) O were accurately weighed stoichiometrically and added to 50mL of deionized water. Accurately weigh 0.7612g of thiourea and adding that thiourea into the solution, and stir until the thiourea is completely dissolved; S2. Dripping ammonia water into the solution under the assis- tance of a pH meter, adjusting the pH value of the solution to about 7, and continuously stirring to obtain uniform sol; S3. The obtained sol was kept in an oven at 95 °C for 6 H to obtain a xerogel.
S4. The xerogel is put into a muffle furnace which is pre- heated at the temperature of 200 deg C to be ignited, and the wave-absorbing material with a loose foam structure is obtained after the combustion is finished.
Fig. 4 (a) is a scanning electron micrograph of the prepared sample. It can be seen from this figure that ZnFe,0;is a three- dimensional structure composed of a curled two-dimensional porous surface.
(B) Absorbing property. The peak value of reflection loss is -52.0 dB in the range of 2-18 GHz. When the thickness is 2.1 mm, the effective bandwidth of RL < -10 dB is 6.10 GHz (11.90-18.00 GHz), which can effectively absorb electromagnetic waves in this frequency band.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made herein without departing from the principles and spir- it of the invention, the scope of which is defined in the appended claims and their equivalents.
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